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<div origin="wiley" registered="yes" id="4" class="doi">10.1111/(ISSN)1551-2916</div>
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<div type="print" id="5" class="issn">0002-7820</div>
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<div type="electronic" id="6" class="issn">1551-2916</div>
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<div type="main" sort="JOURNAL OF THE AMERICAN CERAMIC SOCIETY" id="10" class="title">Journal of the American Ceramic Society</div>
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<div type="short" id="11" class="title">J Am Ceram Soc.</div>
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<div ownership="thirdParty" id="13" class="copyright">© 2025 The American Ceramic Society.</div>
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<div origin="wiley" id="15" class="doi">10.1111/jace.70435</div>
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<div type="articleCategory" id="22" class="title">RESEARCH ARTICLE</div>
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<div type="main" id="90" class="title">Quantifications of growth rate and particle size of magnesium silicate hydrate cement using small‐angle X‐ray scattering</div>
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<div type="shortAuthors" id="91" class="title"><span id="92" class="Dummy">NGUYEN </span><span id="93" class="sc">et al.</span></div><div iamnewxmlelement="true" mytype="articlenotegroup" id="254" class="noteGroup" xmlns="" iamrelocated="True"></div>
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<div id="94" class="creators">
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<span xmlid="jace70435-cr-0001" creatorRole="author" affiliationRef="#jace70435-aff-0001" id="95" class="creator" corresponding="no">
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<span id="96" class="personName"><span id="97" class="givenNames">Trinh Thao My</span><span id="98" class="familyName">Nguyen</span></span><span href="#jace70435-aff-0001" id="95-1" class="link" IamMadeFromParentAtt="AffiliationRef"><sup>1</sup></span></span>
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<span xmlid="jace70435-cr-0002" creatorRole="author" affiliationRef="#jace70435-aff-0002" id="99" class="creator" corresponding="no">
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<span id="100" class="personName"><span id="101" class="givenNames">Dylan</span><span id="102" class="familyName">Singh</span></span><span href="#jace70435-aff-0002" id="99-2" class="link" IamMadeFromParentAtt="AffiliationRef"><sup>2</sup></span></span>
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<span xmlid="jace70435-cr-0003" creatorRole="author" affiliationRef="#jace70435-aff-0003" id="103" class="creator" corresponding="no">
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<span id="104" class="personName"><span id="105" class="givenNames">Ivan</span><span id="106" class="familyName">Kuzmenko</span></span><span href="#jace70435-aff-0003" id="103-3" class="link" IamMadeFromParentAtt="AffiliationRef"><sup>3</sup></span></span>
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<span xmlid="jace70435-cr-0004" creatorRole="author" affiliationRef="#jace70435-aff-0004" id="107" class="creator" corresponding="no">
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<span id="108" class="personName"><span id="109" class="givenNames">Sang Soo</span><span id="110" class="familyName">Lee</span></span><span href="#jace70435-aff-0004" id="107-4" class="link" IamMadeFromParentAtt="AffiliationRef"><sup>4</sup></span></span>
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<span xmlid="jace70435-cr-0005" creatorRole="author" affiliationRef="#jace70435-aff-0001" corresponding="yes" id="111" class="creator">
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<span id="114" class="personName"><span id="115" class="givenNames">Erika</span><span id="116" class="familyName">La Plante</span></span><span href="#jace70435-aff-0001" id="111-1" class="link" IamMadeFromParentAtt="AffiliationRef"><sup>1</sup></span><span class="Starlink"><img class="ip - img - middle e - rte - image e - imginline" Iamnewelement="true" src="../assets/images/icons/envelope.png"></img></span><span id="112" class="contactDetails">
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<a id="113" class="email" href="mailto://eclaplante@ucdavis.edu">eclaplante@ucdavis.edu</a>
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</span></span>
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<div id="117" class="affiliationGroup">
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<div xmlid="jace70435-aff-0001" countryCode="US" id="118" class="affiliation">
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<span id="119" class="orgDiv">Materials Chemistry Laboratory</span>
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<span id="120" class="orgDiv">Department of Materials Science and Engineering</span>
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<span id="121" class="orgName">University of California, Davis</span>
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<span id="122" class="address">
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<span id="123" class="city">Davis</span>
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<span id="124" class="countryPart">California</span>
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<span id="125" class="country">USA</span>
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<div xmlid="jace70435-aff-0002" countryCode="US" id="126" class="affiliation">
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<span id="127" class="orgDiv">Department of Materials Science and Engineering</span>
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<span id="128" class="orgName">University of Texas at Arlington</span>
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<span id="129" class="address">
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<span id="130" class="city">Arlington</span>
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<span id="131" class="countryPart">Texas</span>
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<span id="132" class="country">USA</span>
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</span>
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</div>
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<div xmlid="jace70435-aff-0003" countryCode="US" id="133" class="affiliation">
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<span id="134" class="orgDiv">X‐ray Sciences Division</span>
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<span id="135" class="orgName">Argonne National Laboratory</span>
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<span id="136" class="address">
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<span id="137" class="city">Lemont</span>
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<span id="138" class="countryPart">Illinois</span>
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<span id="139" class="country">USA</span>
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</span>
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</div>
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<div xmlid="jace70435-aff-0004" countryCode="US" id="140" class="affiliation">
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<span id="141" class="orgDiv">Chemical Sciences and Engineering Division</span>
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<span id="142" class="orgName">Argonne National Laboratory</span>
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<span id="143" class="address">
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<span id="144" class="city">Lemont</span>
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<span id="145" class="countryPart">Illinois</span>
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<span id="146" class="country">USA</span>
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</div><div id="33" class="correspondenceTo"><div id="34" class="lineatedText"><div id="35" class="line"><b xmlns="http://www.wiley.com/namespaces/wiley">Correspondence</b></div><div id="36" class="line">Erika La Plante, Materials Chemistry Laboratory, Department of Materials Science and Engineering, University of California, Davis, CA 95616, USA.</div><span id="37" class="Dummy"> </span><div id="38" class="line"><span id="39" class="Dummy">Email: </span><a id="40" class="email" href="mailto://eclaplante@ucdavis.edu">eclaplante@ucdavis.edu</a></div></div></div>
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<div iamnewxmlelement="true" id="153" class="fundinginfogroup"><div class="title" iamnewelement="True">Funding Information</div><div id="154" class="fundingInfo" draggable="true" title="Click and drag it to desired location"><span iamnewelement="True" class="Query1"><span id="q1" class="Query" iamprocessedauthorquery="True">Aq1</span></span><span fundrefname="National Science Foundation" funderdoi="10.13039/100000001" id="155" class="fundingAgency">National Science Foundation</span><span class="fundingNumber old" isdeleteenable="true" emptyvalue="true" mytype="content" user="Erika La Plante" updatedon="09 Dec, 04:10 PM" id="156">#2342381</span><span class="fundingNumber new" isdeleteenable="true" mytype="content" user="Erika La Plante" updatedon="09 Dec, 04:11 PM" emptyvalue="true" id="79b2266b-b55e-4924-a69b-937418116df8">2342381</span></div></div>
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<div ownership="publisher" iamNewElement="True" Class="copyright1"> Copyright </div><div ownership="thirdParty" id="24" class="copyright">© 2025 The American Ceramic Society.</div><div id="25" class="eventGroup">
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<div type="manuscriptReceived" date="2025-06-18" id="26" class="event" MyValueIsMadeFromMyAttribute="date">2025-06-18</div>
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<div type="manuscriptRevised" date="2025-11-21" id="27" class="event" MyValueIsMadeFromMyAttribute="date">2025-11-21</div>
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<div type="manuscriptAccepted" date="2025-11-27" id="28" class="event" MyValueIsMadeFromMyAttribute="date">2025-11-27</div>
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<div type="xmlCreated" agent="Aptara" date="2025-12-05" id="29" class="event" MyValueIsMadeFromMyAttribute="date">2025-12-05</div>
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</div><div id="161" class="abstractGroup">
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<div type="main" xmllang="en" id="162" class="abstract" abstractHeading="true">
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<div type="main" id="163" class="title">Abstract</div>
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<p id="164" xmlns="http://www.wiley.com/namespaces/wiley"><span id="165" class="Dummy" xmlns="">The focus of recent research on cement binders has shifted to alternatives such as magnesium silicate hydrate (M‐S‐H) to mitigate the environmental impact of conventional concrete production. However, a detailed understanding of the morphology and growth rate of M‐S‐H, which informs its applicability as a cementing agent, is lacking. These properties are important as they influence cement hydration and consequently the development of macroscopic properties. In this study, the particle size distribution and growth rate of M‐S‐H synthesized by mixing aqueous stock solutions were analyzed using synchrotron‐based small‐angle X‐ray scattering. The reaction solutions contained dissolved magnesium and silicon with concentrations ranging from 2 to 500 mM, corresponding to saturation indices with respect to M‐S‐H endmembers, M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub>‐S‐H and M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H, between 5.8 and 10.3. The precipitation rates of M‐S‐H align with affinity‐based kinetic models and can be described by the following equations: For M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub>‐S‐H: </span><i iamnewelement="True" class="fa fa-eye" aria-hidden="true" xmlns=""></i><math xmlns="" display="inline" altimg="urn:x-wiley:00027820:media:jace70435:jace70435-math-0001" p7:location="equation/jace70435-math-0001.png" xmlns:p7="http://www.wiley.com/namespaces/wiley/wiley" math="" user="Erika La Plante" isdeleteenable="true" updatedon="09 Dec, 11:19 PM" emptyvalue="true" class="math updated-math" 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" mytype="equation" id="169"><mrow><msub><mi>r</mi><mrow><msub><mi mathvariant="normal">M</mi><mn>0.75</mn></msub><mo>-</mo><mi mathvariant="normal">S</mi><mo>-</mo><mi mathvariant="normal">H</mi></mrow></msub><mo>=</mo><msup><mn>10</mn><mrow><mo>−</mo><mn>9.54</mn><mo>±</mo><mn>0.70</mn></mrow></msup><mo stretchy="false">(</mo><msubsup><mi mathvariant="normal">Ω</mi><mrow><msub><mi mathvariant="normal">M</mi><mn>0.75</mn></msub><mi>SH</mi></mrow><mrow><mn>0.59</mn><mo>±</mo><mn>0.08</mn></mrow></msubsup><mo>−</mo><mn>1</mn><mo stretchy="false">)</mo></mrow></math><mathold style="display: none;" iamrelocated="True"><math xmlns="" display="inline" altimg="urn:x-wiley:00027820:media:jace70435:jace70435-math-0001" p7:location="equation/jace70435-math-0001.png" xmlns:p7="http://www.wiley.com/namespaces/wiley/wiley" class="math" mathid="169"><mrow><msub><mi>r</mi><mrow><msub><mi mathvariant="normal">M</mi><mn>0.75</mn></msub><mi>SH</mi></mrow></msub><mo>=</mo><msup><mn>10</mn><mrow><mo>−</mo><mn>9.54</mn><mo>±</mo><mn>0.70</mn></mrow></msup><mrow><mo stretchy="false">(</mo><mrow><msubsup><mi mathvariant="normal">Ω</mi><mrow><msub><mi mathvariant="normal">M</mi><mn>0.75</mn></msub><mi>SH</mi></mrow><mrow><mn>0.59</mn><mo>±</mo><mn>0.08</mn></mrow></msubsup><mo>−</mo><mn>1</mn></mrow><mo stretchy="false">)</mo></mrow></mrow></math></mathold><span id="205" class="Dummy" xmlns=""><ins user="Erika La Plante" title="Erika La Plante inserted content on: 09 Dec, 04:12 PM" class="new" updatedon="09 Dec, 04:12 PM" mytype="content" id="da40b8e7-ab91-49f9-83c4-65c95a7c96e0">, and</ins><del user="Erika La Plante" title="Erika La Plante deleted content on: 09 Dec, 04:12 PM" class="old" updatedon="09 Dec, 04:12 PM" mytype="content" id="46053cc7-1f69-4e56-8f9c-7b08de04b0f1">.</del> <ins user="Erika La Plante" title="Erika La Plante inserted content on: 09 Dec, 04:12 PM" class="new" updatedon="09 Dec, 04:12 PM" mytype="content" id="c1efb86a-5fc8-4fd2-bc02-f95256f2e02d">f</ins><del user="Erika La Plante" title="Erika La Plante deleted content on: 09 Dec, 04:12 PM" class="old" updatedon="09 Dec, 04:12 PM" mytype="content" id="443e9865-e42f-4ee7-84c3-c9fc56e673bf">F</del>or M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H: </span><i iamnewelement="True" class="fa fa-eye" aria-hidden="true" xmlns=""></i><math xmlns="" display="inline" altimg="urn:x-wiley:00027820:media:jace70435:jace70435-math-0002" p7:location="equation/jace70435-math-0002.png" xmlns:p7="http://www.wiley.com/namespaces/wiley/wiley" math="" user="Erika La Plante" isdeleteenable="true" updatedon="09 Dec, 11:20 PM" emptyvalue="true" class="math updated-math" 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mytype="equation" id="207"><mrow><msub><mi>r</mi><mrow><msub><mi mathvariant="normal">M</mi><mn>1.50</mn></msub><mo>-</mo><mi mathvariant="normal">S</mi><mo>-</mo><mi mathvariant="normal">H</mi></mrow></msub><mo>=</mo><msup><mn>10</mn><mrow><mo>−</mo><mn>7.56</mn><mo>±</mo><mn>0.37</mn></mrow></msup><mo stretchy="false">(</mo><msubsup><mi mathvariant="normal">Ω</mi><mrow><msub><mi mathvariant="normal">M</mi><mn>1.50</mn></msub><mi>SH</mi></mrow><mrow><mn>0.34</mn><mo>±</mo><mn>0.04</mn></mrow></msubsup><mo>−</mo><mn>1</mn><mo stretchy="false">)</mo></mrow></math><mathold style="display: none;" iamrelocated="True"><math xmlns="" display="inline" altimg="urn:x-wiley:00027820:media:jace70435:jace70435-math-0002" p7:location="equation/jace70435-math-0002.png" xmlns:p7="http://www.wiley.com/namespaces/wiley/wiley" class="math" mathid="207"><mrow><msub><mi>r</mi><mrow><msub><mi mathvariant="normal">M</mi><mn>1.50</mn></msub><mi>SH</mi></mrow></msub><mo>=</mo><msup><mn>10</mn><mrow><mo>−</mo><mn>7.56</mn><mo>±</mo><mn>0.37</mn></mrow></msup><mrow><mo stretchy="false">(</mo><mrow><msubsup><mi mathvariant="normal">Ω</mi><mrow><msub><mi mathvariant="normal">M</mi><mn>1.50</mn></msub><mi>SH</mi></mrow><mrow><mn>0.34</mn><mo>±</mo><mn>0.04</mn></mrow></msubsup><mo>−</mo><mn>1</mn></mrow><mo stretchy="false">)</mo></mrow></mrow></math></mathold><span id="243" class="Dummy" xmlns="">, where </span><i iamnewelement="True" class="fa fa-eye d-none" aria-hidden="true" xmlns=""></i><math xmlns="" display="inline" altimg="urn:x-wiley:00027820:media:jace70435:jace70435-math-0003" p7:location="equation/jace70435-math-0003.png" xmlns:p7="http://www.wiley.com/namespaces/wiley/wiley" class="math" id="244"><semantics xmlns=""><mi>r</mi><annotation encoding="application/x-tex">$r$</annotation></semantics></math><span id="248" class="Dummy" xmlns=""> is the rate in mol/L/s, and </span><i iamnewelement="True" class="fa fa-eye d-none" aria-hidden="true" xmlns=""></i><math xmlns="" display="inline" altimg="urn:x-wiley:00027820:media:jace70435:jace70435-math-0004" p7:location="equation/jace70435-math-0004.png" xmlns:p7="http://www.wiley.com/namespaces/wiley/wiley" class="math" id="249"><semantics xmlns=""><mi mathvariant="normal">Ω</mi><annotation encoding="application/x-tex">$\Omega $</annotation></semantics></math><span id="253" class="Dummy" xmlns=""> represents the saturation ratio with respect to M‐S‐H. Moreover, we observed that changing the [Mg]/[Si] ratio affects particle size, a trend that cannot be fully explained by changes in the saturation index alone. These insights are critical for improving the predictability and control of cementation in concrete that utilizes M‐S‐H‐based binders<ins user="Erika La Plante" title="Erika La Plante inserted content on: 09 Dec, 04:12 PM" class="new" updatedon="09 Dec, 04:12 PM" mytype="content" id="1666825c-a037-4116-b508-32c2ad083a7a">.</ins></span></p>
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</div>
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</div><div type="author" xmllang="en" id="147" class="keywordGroup">
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<span xmlid="jace70435-kwd-0001" id="148" class="keyword">cement binder</span>
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<span xmlid="jace70435-kwd-0002" id="149" class="keyword">empirical rate law</span>
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<span xmlid="jace70435-kwd-0003" id="150" class="keyword">M‐S‐H</span>
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<span xmlid="jace70435-kwd-0004" id="151" class="keyword">reaction rate</span>
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<span xmlid="jace70435-kwd-0005" id="152" class="keyword">X‐ray methods</span>
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</div>
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</div><span IamPlaceholderForId="254" xmlns=""></span>
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</header>
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<div sectionsNumbered="yes" id="255" class="body" xmlns="">
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<section xmlid="jace70435-sec-0010" id="256" xmlns="http://www.wiley.com/namespaces/wiley">
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<div type="main" id="257" class="title" xmlns="">INTRODUCTION</div>
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<p id="258"><span id="259" class="Dummy" xmlns="">The global construction industry heavily relies on ordinary Portland cement (OPC), which remains the most commonly used binder in concrete. However, cement production accounts for approximately 8% of global CO<sub xmlns="http://www.wiley.com/namespaces/wiley">2</sub> emissions, primarily from the calcination of CaCO<sub xmlns="http://www.wiley.com/namespaces/wiley">3</sub> and the energy‐intensive operations required for clinker production.<span href="#jace70435-bib-0001 #jace70435-bib-0002" id="262" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">1,2</sup></span> Previous studies have focused on calcium silicate hydrate (C‐S‐H), the cementitious hydration product in OPC.<span href="#jace70435-bib-0003 #jace70435-bib-0004 #jace70435-bib-0005" id="264" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">3–5</sup></span> The ability to control particle size during cement hydration, which involves complex chemical reactions that dictate the development of microstructure and, ultimately, the mechanical properties of the material, is beneficial.<span href="#jace70435-bib-0006 #jace70435-bib-0007" id="266" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">6,7</sup></span> For instance, reducing particle size increases the surface area available for water‐mediated reactions, which in turn accelerates <del user="Erika La Plante" title="Erika La Plante deleted content on: 09 Dec, 04:13 PM" class="old" updatedon="09 Dec, 04:13 PM" mytype="content" id="0315a23b-e9cf-4781-8b67-6b0c08430322">the</del> hydration<del user="Erika La Plante" title="Erika La Plante deleted content on: 09 Dec, 04:13 PM" class="old" updatedon="09 Dec, 04:13 PM" mytype="content" id="ddc3ce6a-869b-42ab-93cc-56fdcde9c5ce"> rate</del> and enhances early strength development.<span href="#jace70435-bib-0007 #jace70435-bib-0008 #jace70435-bib-0009 #jace70435-bib-0010 #jace70435-bib-0011 #jace70435-bib-0012" id="268" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">7–12</sup></span> Incorporating nano‐C‐S‐H particles or polymer‐stabilized nano‐C‐S‐H, up to a certain weight percentage, has been shown to boost early strength and speed up hydration.<span href="#jace70435-bib-0009 #jace70435-bib-0013" id="270" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">9,13</sup></span> This improvement is due to the increased reactive surface area and the higher number of nucleation sites these nanoparticles provide.<span href="#jace70435-bib-0009 #jace70435-bib-0013" id="272" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">9,13</sup></span> Similarly, additives <del user="Erika La Plante" title="Erika La Plante deleted content on: 09 Dec, 04:15 PM" class="old" updatedon="09 Dec, 04:15 PM" mytype="content" id="dc75404b-f2b4-453b-b84d-e1b0dc691058">like</del><ins user="Erika La Plante" title="Erika La Plante inserted content on: 09 Dec, 04:15 PM" class="new" updatedon="09 Dec, 04:15 PM" mytype="content" id="eed65321-fedc-4447-b499-16312532beee">such as</ins> nano‐silica (SiO<sub xmlns="http://www.wiley.com/namespaces/wiley">2</sub>) and nano‐calcium carbonate (CaCO<sub xmlns="http://www.wiley.com/namespaces/wiley">3</sub>) can act as nucleation agents or fillers between cement grains, promoting hydration, decreasing capillary porosity, and improving compressive strength.<span href="#jace70435-bib-0009 #jace70435-bib-0014 #jace70435-bib-0015 #jace70435-bib-0016 #jace70435-bib-0017" id="276" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">9,14–17</sup></span></span></p>
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<p id="277"><span id="278" class="Dummy" xmlns="">Magnesium silicate hydrate (M‐S‐H) has recently gained attention as a low‐pH binder alternative, offering a more sustainable option that can reduce the carbon footprint of construction.<span href="#jace70435-bib-0018 #jace70435-bib-0019 #jace70435-bib-0020" id="279" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">18–20</sup></span> M‐S‐H can be synthesized by combining silica fume, magnesium oxide/hydroxide (MgO/Mg(OH)<sub xmlns="http://www.wiley.com/namespaces/wiley">2</sub>), and water, or by using aqueous solutions containing dissolved silicon and magnesium salts.<span href="#jace70435-bib-0019 #jace70435-bib-0021 #jace70435-bib-0022 #jace70435-bib-0023 #jace70435-bib-0024 #jace70435-bib-0025" id="282" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">19,21–25</sup></span> Both methods have been utilized to synthesize M‐S‐H with similar chemical composition, structure, and crystallinity<ins user="Erika La Plante" title="Erika La Plante inserted content on: 09 Dec, 11:33 PM" class="new" updatedon="09 Dec, 11:33 PM" mytype="content" id="28ee30ba-1cc0-481d-abb4-ab3310c7aa95">, whereas t</ins><del user="Erika La Plante" title="Erika La Plante deleted content on: 09 Dec, 11:33 PM" class="old" updatedon="09 Dec, 11:33 PM" mytype="content" id="7da66e1f-b57b-4d7a-983e-150fe1750798">. T</del>he aqueous system is designed primarily to investigate the early nucleation mechanisms and growth rate of M‐S‐H. While this system provides valuable insights into particle formation and kinetics, it is not intended to directly replicate curing in concrete, which can be mimicked by the reaction of MgO with silica fume. This requires long curing times, and the reactivity of the solid precursors influences the kinetics of M‐S‐H formation. In the aqueous precipitation method, M‐S‐H nucleation occurs rapidly because Mg and Si ions are supplied from their soluble salts. Properties such as morphology, surface area, and mechanical strength can be controlled by the<ins user="Erika La Plante" title="Erika La Plante inserted content on: 09 Dec, 11:36 PM" class="new" updatedon="09 Dec, 11:36 PM" mytype="content" id="4e79ef5b-9c4a-4fc2-a7c7-32290d7690b6"> overall</ins> <del user="Erika La Plante" title="Erika La Plante deleted content on: 09 Dec, 11:35 PM" class="old" updatedon="09 Dec, 11:35 PM" mytype="content" id="99293af0-7e53-4700-a2da-65eafa43393e">[</del>Mg<del user="Erika La Plante" title="Erika La Plante deleted content on: 09 Dec, 11:35 PM" class="old" updatedon="09 Dec, 11:35 PM" mytype="content" id="4016dc78-31f2-412a-931d-72ef1cc1b74a">]</del>/<del user="Erika La Plante" title="Erika La Plante deleted content on: 09 Dec, 11:35 PM" class="old" updatedon="09 Dec, 11:35 PM" mytype="content" id="e6277a44-8dc7-45db-af9d-f6a33dee9fc0">[</del>Si<del user="Erika La Plante" title="Erika La Plante deleted content on: 09 Dec, 11:35 PM" class="old" updatedon="09 Dec, 11:35 PM" mytype="content" id="20eadcd8-21e3-4be0-a3c4-8cf498ac5d91">]</del> ratio<ins user="Erika La Plante" title="Erika La Plante inserted content on: 09 Dec, 11:36 PM" class="new" updatedon="09 Dec, 11:36 PM" mytype="content" id="1362f295-4cd8-4477-8cf8-99ea2cd3a51c"> of reactants</ins> in both methods. During synthesis, either transitional M‐S‐H phases gradually evolve into more polymerized structures, or Mg‐silicate complexes form M‐S‐H precursors that eventually transform into denser M‐S‐H frameworks.<span href="#jace70435-bib-0022 #jace70435-bib-0023" id="284" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">22,23</sup></span> Structurally, M‐S‐H features a layered silicate configuration, and its degree of polymerization can be tuned by adjusting the <ins user="Erika La Plante" title="Erika La Plante inserted content on: 09 Dec, 11:36 PM" class="new" updatedon="09 Dec, 11:36 PM" mytype="content" id="450cb345-0668-42b1-b041-7c53b3a3fbd6">aqueous </ins>magnesium‐to‐silicon ([Mg]/[Si]) ratio.<span href="#jace70435-bib-0018 #jace70435-bib-0026" id="286" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">18,26</sup></span> In contrast, C‐S‐H exhibits a lower degree of silicate tetrahedral polymerization, characterized by silicate chains separated by layers of calcium oxide and water, as studied using NMR.<span href="#jace70435-bib-0027 #jace70435-bib-0028" id="288" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">27,28</sup></span> The differences in basic building block structure are believed to influence the distinct morphologies of the two materials at the microscale. While not many studies have studied M‐S‐H, its building blocks have been described as spherical globules.<span href="#jace70435-bib-0025" id="290" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">25</sup></span> On the other hand, the unit structures of C‐S‐H have been widely studied and have been described as polydisperse multilayer disk‐like globules, nanosheets, fractal globules, nanoglobules, fine fibers, and thin sheets. These building units give C‐S‐H a wide range of morphologies, including globule‐like, foil‐like, fiber‐like, and microassembled structures ranging from a few nanometers to a thousand nanometers in <del user="Erika La Plante" title="Erika La Plante deleted content on: 09 Dec, 11:37 PM" class="old" updatedon="09 Dec, 11:37 PM" mytype="content" id="9b90a928-1a7b-49d8-9e6b-730f222de335">structure</del> size.<span href="#jace70435-bib-0028 #jace70435-bib-0029 #jace70435-bib-0030 #jace70435-bib-0031" id="292" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">28–31</sup></span> However, the nanoscale chemical mechanisms that govern the structural evolution of these <del user="Erika La Plante" title="Erika La Plante deleted content on: 09 Dec, 11:37 PM" class="old" updatedon="09 Dec, 11:37 PM" mytype="content" id="19b17f6e-fbab-4f03-91d1-9b4c9ac8f186">primary</del> binder phases remain poorly understood.</span></p>
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<p id="294"><span id="295" class="Dummy" xmlns="">To investigate the nanoscale structural evolution of particles, synchrotron‐based small‐angle X‐ray scattering (SAXS) is utilized. SAXS is a powerful technique that detects changes in particle size, shape, and aggregation during nucleation and growth, while simultaneously providing statistically robust results through the analysis of large particle populations.<span href="#jace70435-bib-0032" id="296" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">32</sup></span> For instance, SAXS has been shown to enable high‐resolution, in situ characterization of colloidal gold nanoparticles or the aggregation in silico‐alkaline solutions, implying its suitability for nondestructive probing of the poorly crystalline and complex microstructure of M‐S‐H, as well as its aggregation.<span href="#jace70435-bib-0033 #jace70435-bib-0034 #jace70435-bib-0035" id="298" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">33–35</sup></span> Indeed, SAXS has been used to quantify the size of M‐S‐H building blocks at the nanoscale.<span href="#jace70435-bib-0025" id="300" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">25</sup></span> In this work, we extend the application of SAXS to not only characterize particle sizes in M‐S‐H but also to systematically determine <del user="Erika La Plante" title="Erika La Plante deleted content on: 09 Dec, 11:38 PM" class="old" updatedon="09 Dec, 11:38 PM" mytype="content" id="756f1e27-165a-408c-a7b8-c4ecac281f94">the</del><ins user="Erika La Plante" title="Erika La Plante inserted content on: 09 Dec, 11:38 PM" class="new" updatedon="09 Dec, 11:38 PM" mytype="content" id="a6b37be3-1cf6-49b4-9534-7ed151fca48e">its</ins> growth rate for various solution conditions. By quantifying growth rates and complementing SAXS data with chemical characterization techniques such as Fourier‐transform infrared spectroscopy (FTIR), X‐ray diffraction (XRD), thermogravimetric analysis (TGA), and atomic force microscopy (AFM), this work aims to establish a precipitation rate law that can predict M‐S‐H formation under varying levels of supersaturation. As with C‐S‐H, the ability to control M‐S‐H precipitation offers a pathway to regulate the macroscopic properties of M‐S‐H‐based cementitious materials. Additionally, comparing the growth dynamics and structural evolution of M‐S‐H and C‐S‐H provides valuable insight into the fundamental mechanisms governing hydrated silicate binder formation and their influence on the resulting material properties.</span></p>
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</section>
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<section xmlid="jace70435-sec-0020" id="302" xmlns="http://www.wiley.com/namespaces/wiley">
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<div type="main" id="303" class="title" xmlns="">MATERIALS AND METHODS</div>
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<section xmlid="jace70435-sec-0030" id="304">
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<div type="main" id="305" class="title" xmlns="">Solution preparation and sample characterization</div>
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<p id="306" xmlns=""><span id="307" class="Dummy" xmlns="">Two equivalent sets of samples were prepared: one designated for SAXS analysis and the other for pH measurements and precipitate characterization. M‐S‐H samples were prepared by mixing stock solutions of magnesium nitrate hexahydrate (Mg(NO<sub xmlns="http://www.wiley.com/namespaces/wiley">3</sub>)<sub xmlns="http://www.wiley.com/namespaces/wiley">2</sub>·6H<sub xmlns="http://www.wiley.com/namespaces/wiley">2</sub>O) (Sigma Aldrich) and sodium metasilicate pentahydrate (Na<sub xmlns="http://www.wiley.com/namespaces/wiley">2</sub>SiO<sub xmlns="http://www.wiley.com/namespaces/wiley">3</sub>·5H<sub xmlns="http://www.wiley.com/namespaces/wiley">2</sub>O) (Sigma Aldrich) in ultrapure deionized (DI) water (Milli‐Q, >18.2 MΩ·cm) into a polypropylene centrifuge tube at various concentrations (and saturation indices) or [Mg]/[Si] molar ratios (Table <span href="#jace70435-tbl-0001" id="314" class="link">1</span>). Saturation index (SI), defined as the log<sub xmlns="http://www.wiley.com/namespaces/wiley">10</sub> of the saturation ratio, <span user="Erika La Plante" title="Erika La Plante inserted comments on: 09 Dec, 11:44 PM" class="reComment fas fa-comment" style="" updatedon="09 Dec, 11:44 PM" mytype="comment" id="8efaeaf2-9b5f-4247-9931-a152a98488c4"></span><i xmlns="http://www.wiley.com/namespaces/wiley">Ω</i>, was calculated using PHREEQC with the CEMDATA18 database.<span href="#jace70435-bib-0036 #jace70435-bib-0037" id="318" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">36,37</sup></span> Saturation ratio Ω is the ratio of the ion activity product (IAP) and the solubility product (<i xmlns="http://www.wiley.com/namespaces/wiley"><span id="320" class="Dummy" xmlns="">K</span><sub>sp</sub></i>) of a given phase. The equilibria that describe the dissolution and precipitation of M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub>‐S‐H or M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H are given by Equations (1) and (2)<span href="#jace70435-bib-0036 #jace70435-bib-0038" id="324" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">36,38</sup></span>:</span><span xmlid="jace70435-disp-0001" type="mathematics" id="326" class="displayedItem" xmlns=""><span iamnewelement="True"><i iamnewelement="True" class="fa fa-eye d-none" aria-hidden="true"></i><math xmlns="http://www.w3.org/1998/Math/MathML" display="block" altimg="urn:x-wiley:00027820:media:jace70435:jace70435-math-0005" p7:location="equation/jace70435-math-0005.png" xmlns:p7="http://www.wiley.com/namespaces/wiley/wiley" class="math" id="328"><semantics xmlns=""><mtable displaystyle="true"><mtr><mtd></mtd><mtd columnalign="left"><mrow><mi mathvariant="normal">M</mi><msub><mi mathvariant="normal">g</mi><mn>3</mn></msub><mi mathvariant="normal">S</mi><msub><mi mathvariant="normal">i</mi><mn>4</mn></msub><msub><mi mathvariant="normal">O</mi><mn>11</mn></msub><msub><mfenced separators="" open="(" close=")"><mrow><msub><mi mathvariant="normal">H</mi><mn>2</mn></msub><mi mathvariant="normal">O</mi></mrow></mfenced><mn>5</mn></msub></mrow></mtd></mtr><mtr><mtd></mtd><mtd columnalign="left"><mrow><mspace width="1em"></mspace><mo>↔</mo><mrow><mn>3</mn><mi mathvariant="normal">M</mi></mrow><msup><mi mathvariant="normal">g</mi><mrow><mn>2</mn><mo>+</mo></mrow></msup><mrow><mo linebreak="badbreak">+</mo><mn>4</mn><mi>Si</mi></mrow><msub><mi mathvariant="normal">O</mi><mn>2</mn></msub><mrow><mo linebreak="badbreak">+</mo><mn>6</mn><mi mathvariant="normal">O</mi></mrow><msup><mi mathvariant="normal">H</mi><mo>−</mo></msup><mrow><mo linebreak="badbreak">+</mo><mn>2</mn></mrow><msub><mi mathvariant="normal">H</mi><mn>2</mn></msub><mrow><mi mathvariant="normal">O</mi><mo>;</mo><mi>log</mi></mrow><mspace width="0.33em"></mspace><msub><mi>K</mi><mi>sp</mi></msub><mrow><mo linebreak="badbreak">=</mo><mo>−</mo><mn>57</mn></mrow><mrow><mo>.</mo><mn>6</mn></mrow></mrow></mtd></mtr></mtable><annotation encoding="application/x-tex">$$\begin{align}&{\mathrm{M}}{{\mathrm{g}}_{\mathrm{3}}}{\mathrm{S}}{{\mathrm{i}}_{\mathrm{4}}}{{\mathrm{O}}_{{\mathrm{11}}}}{\left( {{{\mathrm{H}}_{\mathrm{2}}}{\mathrm{O}}} \right)_{\mathrm{5}}} \nonumber\\ & \quad \leftrightarrow {\mathrm{3M}}{{\mathrm{g}}^{{\mathrm{2 + }}}}{\mathrm{ + 4Si}}{{\mathrm{O}}_{\mathrm{2}}}{\mathrm{ + 6O}}{{\mathrm{H}}^{\mathrm{-}}}{\mathrm{ + 2}}{{\mathrm{H}}_{\mathrm{2}}}{\mathrm{O; log}}\ {K_{{\mathrm{sp}}}}{\mathrm{ = -57}}{\mathrm{.6}}\end{align}$$</annotation></semantics></math><label id="327" xmlns="http://www.wiley.com/namespaces/wiley">1</label></span><span iamplaceholderforid="328"></span></span><span xmlid="jace70435-disp-0002" type="mathematics" id="404" class="displayedItem" xmlns=""><span iamnewelement="True"><i iamnewelement="True" class="fa fa-eye d-none" aria-hidden="true"></i><math xmlns="http://www.w3.org/1998/Math/MathML" display="block" altimg="urn:x-wiley:00027820:media:jace70435:jace70435-math-0006" p7:location="equation/jace70435-math-0006.png" xmlns:p7="http://www.wiley.com/namespaces/wiley/wiley" class="math" id="406"><semantics xmlns=""><mtable displaystyle="true"><mtr><mtd></mtd><mtd columnalign="left"><mrow><mi mathvariant="normal">M</mi><msub><mi mathvariant="normal">g</mi><mn>3</mn></msub><mi mathvariant="normal">S</mi><msub><mi mathvariant="normal">i</mi><mn>2</mn></msub><msub><mi mathvariant="normal">O</mi><mn>7</mn></msub><msub><mfenced separators="" open="(" close=")"><mrow><msub><mi mathvariant="normal">H</mi><mn>2</mn></msub><mi mathvariant="normal">O</mi></mrow></mfenced><mn>5</mn></msub></mrow></mtd></mtr><mtr><mtd></mtd><mtd columnalign="left"><mrow><mspace width="1em"></mspace><mo>↔</mo><mrow><mn>3</mn><mi mathvariant="normal">M</mi></mrow><msup><mi mathvariant="normal">g</mi><mrow><mn>2</mn><mo>+</mo></mrow></msup><mrow><mo linebreak="badbreak">+</mo><mn>2</mn><mi>Si</mi></mrow><msub><mi mathvariant="normal">O</mi><mn>2</mn></msub><mrow><mo linebreak="badbreak">+</mo><mn>6</mn><mi mathvariant="normal">O</mi></mrow><msup><mi mathvariant="normal">H</mi><mo>−</mo></msup><mrow><mo linebreak="badbreak">+</mo><mn>2</mn></mrow><msub><mi mathvariant="normal">H</mi><mn>2</mn></msub><mrow><mi mathvariant="normal">O</mi><mo>;</mo><mi>log</mi></mrow><mspace width="0.33em"></mspace><msub><mi>K</mi><mi>sp</mi></msub><mrow><mo linebreak="badbreak">=</mo><mo>−</mo><mn>47</mn></mrow><mrow><mo>.</mo><mn>1</mn></mrow></mrow></mtd></mtr></mtable><annotation encoding="application/x-tex">$$\begin{align}&{\mathrm{M}}{{\mathrm{g}}_{\mathrm{3}}}{\mathrm{S}}{{\mathrm{i}}_{\mathrm{2}}}{{\mathrm{O}}_{\mathrm{7}}}{\left( {{{\mathrm{H}}_{\mathrm{2}}}{\mathrm{O}}} \right)_{\mathrm{5}}} \nonumber\\ & \quad \leftrightarrow {\mathrm{3M}}{{\mathrm{g}}^{{\mathrm{2 + }}}}{\mathrm{ + 2Si}}{{\mathrm{O}}_{\mathrm{2}}}{\mathrm{ + 6O}}{{\mathrm{H}}^{\mathrm{-}}}{\mathrm{ + 2}}{{\mathrm{H}}_{\mathrm{2}}}{\mathrm{O; log}}\ {K_{{\mathrm{sp}}}}{\mathrm{ = -47}}{\mathrm{.1}}\end{align}$$</annotation></semantics></math><label id="405" xmlns="http://www.wiley.com/namespaces/wiley">2</label></span><span iamplaceholderforid="406"></span></span></p>
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<div xmlid="jace70435-tbl-0001" pRights="unknown" eRights="yes" copyright="John Wiley & Sons, Ltd." id="482" class="tabular" xmlns="">
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<span IamPlaceholderForId="483"></span>
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<div type="tabularName" id="485" class="title">TABLE<label id="483" xmlns="http://www.wiley.com/namespaces/wiley" iamrelocated="True">1</label><span type="main" id="486" class="title" iamrelocated="True"><span id="487" class="Dummy">Experimental details, showing Mg and Si concentrations, measured and calculated pH, and saturation indices with respect to brucite (Mg(OH)<sub xmlns="http://www.wiley.com/namespaces/wiley">2</sub>) and the two endmember M‐S‐H phases, M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub>‐S‐H or M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H.</span></span></div>
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</div>
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<span IamPlaceholderForId="698"></span>
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<div iamnewelement="True" class="TableOverFlow"><table frame="topbot" xmlns="http://www.wiley.com/namespaces/wiley">
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<tgroup cols="10">
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<colspec colnum="1" colname="col1" align="left" id="491" class="colspec" xmlns=""></colspec>
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<colspec colnum="2" colname="col2" align="left" id="492" class="colspec" xmlns=""></colspec>
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<colspec colnum="3" colname="col3" align="left" id="493" class="colspec" xmlns=""></colspec>
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<colspec colnum="4" colname="col4" align="left" id="494" class="colspec" xmlns=""></colspec>
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<colspec colnum="5" colname="col5" align="left" id="495" class="colspec" xmlns=""></colspec>
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<colspec colnum="6" colname="col6" align="left" id="496" class="colspec" xmlns=""></colspec>
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<colspec colnum="7" colname="col7" align="left" id="497" class="colspec" xmlns=""></colspec>
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<colspec colnum="8" colname="col8" align="left" id="498" class="colspec" xmlns=""></colspec>
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<colspec colnum="9" colname="col9" align="left" id="499" class="colspec" xmlns=""></colspec>
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<colspec colnum="10" colname="col10" align="left" id="500" class="colspec" xmlns=""></colspec>
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<thead>
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<tr id="501" xmlns="">
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<th colname="col1" id="502" class="thentry"></th>
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<th colname="col2" namest="col2" nameend="col3" rowsep="1" id="503" class="thentry" colspan="2">Concentration (mM)</th>
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<th colname="col4" id="504" class="thentry"></th>
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<th colname="col5" id="505" class="thentry"></th>
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<th colname="col6" namest="col6" nameend="col7" rowsep="1" id="506" class="thentry" colspan="2">pH</th>
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<th colname="col8" namest="col8" nameend="col10" rowsep="1" id="507" class="thentry" colspan="3">Saturation index, SI</th>
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</tr>
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<tr rowsep="1" id="508" xmlns="">
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<th colname="col1" id="509" class="thentry">Sample set</th>
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<th colname="col2" id="510" class="thentry">[Mg]</th>
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<th colname="col3" id="511" class="thentry">[Si]</th>
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<th colname="col4" id="512" class="thentry">[Mg]/[Si] ratio</th>
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<th colname="col5" id="513" class="thentry">Reaction time (min)</th>
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<th colname="col6" id="514" class="thentry">Measured</th>
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<th colname="col7" id="515" class="thentry">Calculated</th>
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<th colname="col8" id="516" class="thentry">Brucite</th>
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<th colname="col9" id="517" class="thentry"><span id="518" class="Dummy">M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub>‐S‐H</span></th>
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<th colname="col10" id="520" class="thentry"><span id="521" class="Dummy">M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H</span></th>
|
|
</tr>
|
|
</thead>
|
|
<tbody>
|
|
<tr id="523" xmlns="">
|
|
<td colname="col1" morerows="2" id="524" class="entry" rowspan="3">1 (Varying M‐S‐H SI at fixed brucite SI)</td>
|
|
<td colname="col2" id="525" class="entry">2</td>
|
|
<td colname="col3" id="526" class="entry">2</td>
|
|
<td colname="col4" id="527" class="entry">1.00</td>
|
|
<td colname="col5" id="528" class="entry">24</td>
|
|
<td colname="col6" id="529" class="entry">10.64</td>
|
|
<td colname="col7" id="530" class="entry">11.61</td>
|
|
<td colname="col8" id="531" class="entry">2.73</td>
|
|
<td colname="col9" id="532" class="entry">5.97</td>
|
|
<td colname="col10" id="533" class="entry">5.81</td>
|
|
</tr>
|
|
<tr id="534" xmlns="">
|
|
<td colname="col2" id="535" class="entry">2.6</td>
|
|
<td colname="col3" id="536" class="entry">4</td>
|
|
<td colname="col4" id="537" class="entry">0.65</td>
|
|
<td colname="col5" id="538" class="entry">24</td>
|
|
<td colname="col6" id="539" class="entry">10.87</td>
|
|
<td colname="col7" id="540" class="entry">11.79</td>
|
|
<td colname="col8" id="541" class="entry">2.73</td>
|
|
<td colname="col9" id="542" class="entry">6.41</td>
|
|
<td colname="col10" id="543" class="entry">6.03</td>
|
|
</tr>
|
|
<tr id="544" xmlns="">
|
|
<td colname="col2" id="545" class="entry">3.85</td>
|
|
<td colname="col3" id="546" class="entry">10</td>
|
|
<td colname="col4" id="547" class="entry">0.39</td>
|
|
<td colname="col5" id="548" class="entry">24</td>
|
|
<td colname="col6" id="549" class="entry">11.68</td>
|
|
<td colname="col7" id="550" class="entry">12.08</td>
|
|
<td colname="col8" id="551" class="entry">2.73</td>
|
|
<td colname="col9" id="552" class="entry">6.86</td>
|
|
<td colname="col10" id="553" class="entry">6.25</td>
|
|
</tr>
|
|
<tr id="554" xmlns="">
|
|
<td colname="col1" morerows="9" id="555" class="entry" rowspan="10">2 (Varying M‐S‐H SI)</td>
|
|
<td colname="col2" id="556" class="entry">2</td>
|
|
<td colname="col3" id="557" class="entry">2</td>
|
|
<td colname="col4" id="558" class="entry">1.00</td>
|
|
<td colname="col5" id="559" class="entry">61–123</td>
|
|
<td colname="col6" id="560" class="entry">10.64</td>
|
|
<td colname="col7" id="561" class="entry">11.60</td>
|
|
<td colname="col8" id="562" class="entry">2.73</td>
|
|
<td colname="col9" id="563" class="entry">5.97</td>
|
|
<td colname="col10" id="564" class="entry">5.81</td>
|
|
</tr>
|
|
<tr id="565" xmlns="">
|
|
<td colname="col2" id="566" class="entry">5</td>
|
|
<td colname="col3" id="567" class="entry">5</td>
|
|
<td colname="col4" id="568" class="entry">1.00</td>
|
|
<td colname="col5" id="569" class="entry">61–123</td>
|
|
<td colname="col6" id="570" class="entry">10.43</td>
|
|
<td colname="col7" id="571" class="entry">11.97</td>
|
|
<td colname="col8" id="572" class="entry">3.40</td>
|
|
<td colname="col9" id="573" class="entry">6.58</td>
|
|
<td colname="col10" id="574" class="entry">6.61</td>
|
|
</tr>
|
|
<tr id="575" xmlns="">
|
|
<td colname="col2" id="576" class="entry">10</td>
|
|
<td colname="col3" id="577" class="entry">10</td>
|
|
<td colname="col4" id="578" class="entry">1.00</td>
|
|
<td colname="col5" id="579" class="entry">61–123</td>
|
|
<td colname="col6" id="580" class="entry">10.32</td>
|
|
<td colname="col7" id="581" class="entry">12.25</td>
|
|
<td colname="col8" id="582" class="entry">3.89</td>
|
|
<td colname="col9" id="583" class="entry">7.00</td>
|
|
<td colname="col10" id="584" class="entry">7.19</td>
|
|
</tr>
|
|
<tr id="585" xmlns="">
|
|
<td colname="col2" id="586" class="entry">25</td>
|
|
<td colname="col3" id="587" class="entry">25</td>
|
|
<td colname="col4" id="588" class="entry">1.00</td>
|
|
<td colname="col5" id="589" class="entry">61–123</td>
|
|
<td colname="col6" id="590" class="entry">10.16</td>
|
|
<td colname="col7" id="591" class="entry">12.62</td>
|
|
<td colname="col8" id="592" class="entry">4.54</td>
|
|
<td colname="col9" id="593" class="entry">7.51</td>
|
|
<td colname="col10" id="594" class="entry">7.93</td>
|
|
</tr>
|
|
<tr id="595" xmlns="">
|
|
<td colname="col2" id="596" class="entry">50</td>
|
|
<td colname="col3" id="597" class="entry">50</td>
|
|
<td colname="col4" id="598" class="entry">1.00</td>
|
|
<td colname="col5" id="599" class="entry">61–123</td>
|
|
<td colname="col6" id="600" class="entry">10.40</td>
|
|
<td colname="col7" id="601" class="entry">12.91</td>
|
|
<td colname="col8" id="602" class="entry">5.04</td>
|
|
<td colname="col9" id="603" class="entry">7.88</td>
|
|
<td colname="col10" id="604" class="entry">8.49</td>
|
|
</tr>
|
|
<tr id="605" xmlns="">
|
|
<td colname="col2" id="606" class="entry">100</td>
|
|
<td colname="col3" id="607" class="entry">100</td>
|
|
<td colname="col4" id="608" class="entry">1.00</td>
|
|
<td colname="col5" id="609" class="entry">61–123</td>
|
|
<td colname="col6" id="610" class="entry">10.20</td>
|
|
<td colname="col7" id="611" class="entry">13.19</td>
|
|
<td colname="col8" id="612" class="entry">5.58</td>
|
|
<td colname="col9" id="613" class="entry">8.21</td>
|
|
<td colname="col10" id="614" class="entry">9.06</td>
|
|
</tr>
|
|
<tr id="615" xmlns="">
|
|
<td colname="col2" id="616" class="entry">200</td>
|
|
<td colname="col3" id="617" class="entry">200</td>
|
|
<td colname="col4" id="618" class="entry">1.00</td>
|
|
<td colname="col5" id="619" class="entry">61–123</td>
|
|
<td colname="col6" id="620" class="entry">11.72</td>
|
|
<td colname="col7" id="621" class="entry">13.46</td>
|
|
<td colname="col8" id="622" class="entry">6.14</td>
|
|
<td colname="col9" id="623" class="entry">8.52</td>
|
|
<td colname="col10" id="624" class="entry">9.63</td>
|
|
</tr>
|
|
<tr id="625" xmlns="">
|
|
<td colname="col2" id="626" class="entry">300</td>
|
|
<td colname="col3" id="627" class="entry">300</td>
|
|
<td colname="col4" id="628" class="entry">1.00</td>
|
|
<td colname="col5" id="629" class="entry">61–123</td>
|
|
<td colname="col6" id="630" class="entry">—</td>
|
|
<td colname="col7" id="631" class="entry">13.62</td>
|
|
<td colname="col8" id="632" class="entry">6.47</td>
|
|
<td colname="col9" id="633" class="entry">8.69</td>
|
|
<td colname="col10" id="634" class="entry">9.96</td>
|
|
</tr>
|
|
<tr id="635" xmlns="">
|
|
<td colname="col2" id="636" class="entry">400</td>
|
|
<td colname="col3" id="637" class="entry">400</td>
|
|
<td colname="col4" id="638" class="entry">1.00</td>
|
|
<td colname="col5" id="639" class="entry">61–123</td>
|
|
<td colname="col6" id="640" class="entry">—</td>
|
|
<td colname="col7" id="641" class="entry">13.71</td>
|
|
<td colname="col8" id="642" class="entry">6.68</td>
|
|
<td colname="col9" id="643" class="entry">8.82</td>
|
|
<td colname="col10" id="644" class="entry">10.19</td>
|
|
</tr>
|
|
<tr id="645" xmlns="">
|
|
<td colname="col2" id="646" class="entry">500</td>
|
|
<td colname="col3" id="647" class="entry">500</td>
|
|
<td colname="col4" id="648" class="entry">1.00</td>
|
|
<td colname="col5" id="649" class="entry">61–123</td>
|
|
<td colname="col6" id="650" class="entry">—</td>
|
|
<td colname="col7" id="651" class="entry">13.78</td>
|
|
<td colname="col8" id="652" class="entry">6.83</td>
|
|
<td colname="col9" id="653" class="entry">8.94</td>
|
|
<td colname="col10" id="654" class="entry">10.35</td>
|
|
</tr>
|
|
<tr id="655" xmlns="">
|
|
<td colname="col1" morerows="3" id="656" class="entry" rowspan="4"><span id="657" class="Dummy">3 (Varying [Mg]/[Si] ratio at fixed M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub>‐S‐H SI)</span></td>
|
|
<td colname="col2" id="659" class="entry">1.6</td>
|
|
<td colname="col3" id="660" class="entry">2.1</td>
|
|
<td colname="col4" id="661" class="entry">0.76</td>
|
|
<td colname="col5" id="662" class="entry">76</td>
|
|
<td colname="col6" id="663" class="entry">10.87</td>
|
|
<td colname="col7" id="664" class="entry">11.56</td>
|
|
<td colname="col8" id="665" class="entry">2.49</td>
|
|
<td colname="col9" id="666" class="entry">5.97</td>
|
|
<td colname="col10" id="667" class="entry">5.63</td>
|
|
</tr>
|
|
<tr id="668" xmlns="">
|
|
<td colname="col2" id="669" class="entry">2</td>
|
|
<td colname="col3" id="670" class="entry">2</td>
|
|
<td colname="col4" id="671" class="entry">1.00</td>
|
|
<td colname="col5" id="672" class="entry">76</td>
|
|
<td colname="col6" id="673" class="entry">10.69</td>
|
|
<td colname="col7" id="674" class="entry">11.60</td>
|
|
<td colname="col8" id="675" class="entry">2.73</td>
|
|
<td colname="col9" id="676" class="entry">5.97</td>
|
|
<td colname="col10" id="677" class="entry">5.81</td>
|
|
</tr>
|
|
<tr id="678" xmlns="">
|
|
<td colname="col2" id="679" class="entry">4.2</td>
|
|
<td colname="col3" id="680" class="entry">2.4</td>
|
|
<td colname="col4" id="681" class="entry">1.75</td>
|
|
<td colname="col5" id="682" class="entry">76</td>
|
|
<td colname="col6" id="683" class="entry">10.35</td>
|
|
<td colname="col7" id="684" class="entry">11.83</td>
|
|
<td colname="col8" id="685" class="entry">3.52</td>
|
|
<td colname="col9" id="686" class="entry">5.97</td>
|
|
<td colname="col10" id="687" class="entry">6.40</td>
|
|
</tr>
|
|
<tr id="688" xmlns="">
|
|
<td colname="col2" id="689" class="entry">275</td>
|
|
<td colname="col3" id="690" class="entry">18.33</td>
|
|
<td colname="col4" id="691" class="entry">15.00</td>
|
|
<td colname="col5" id="692" class="entry">76</td>
|
|
<td colname="col6" id="693" class="entry">9.33</td>
|
|
<td colname="col7" id="694" class="entry">13.40</td>
|
|
<td colname="col8" id="695" class="entry">7.25</td>
|
|
<td colname="col9" id="696" class="entry">5.97</td>
|
|
<td colname="col10" id="697" class="entry">9.19</td>
|
|
</tr>
|
|
</tbody>
|
|
</tgroup>
|
|
</table></div><div id="698" class="noteGroup">
|
|
<div xmlid="jace70435-tbl1-note-0001" numbered="no" id="699" class="note"><p id="700" xmlns="http://www.wiley.com/namespaces/wiley"><i>Note</i><span id="701" class="Dummy" xmlns="">: The discrepancy between measured and calculated pH can be explained by the immediate formation of M‐S‐H upon mixing of the Mg‐ and Si‐containing stock solutions. Unavailable pH values correspond to samples with a gel‐like consistency.</span></p></div>
|
|
</div></div>
|
|
<p id="702"><span id="703" class="Dummy" xmlns="">pH measurements were performed in triplicate within 10 s of mixing the stock solutions<del user="Erika La Plante" title="Erika La Plante deleted content on: 09 Dec, 11:45 PM" class="old" updatedon="09 Dec, 11:45 PM" mytype="content" id="731ced06-133e-4b6d-b39f-4bc60e446306">,</del> using a pH meter (Orion Versa Star Pro, Thermo Fisher Scientific) equipped with a pH/ATC Triode probe (Ross Ultra, Thermo Fisher Scientific)<ins user="Erika La Plante" title="Erika La Plante inserted content on: 09 Dec, 11:45 PM" class="new" updatedon="09 Dec, 11:45 PM" mytype="content" id="1923e452-94cb-44f6-b90a-b0980c21609c"> and</ins><del user="Erika La Plante" title="Erika La Plante deleted content on: 09 Dec, 11:45 PM" class="old" updatedon="09 Dec, 11:45 PM" mytype="content" id="6ea1910d-c322-400d-aefc-93ff205ac898">,</del> calibrated over the pH range of 4 to 12. After 3 h of reaction, the suspensions were centrifuged <del user="Erika La Plante" title="Erika La Plante deleted content on: 09 Dec, 11:46 PM" class="old" updatedon="09 Dec, 11:46 PM" mytype="content" id="1777ca9d-129e-4816-b630-1a3c2161a06d">at 2500 rpm </del><del user="Erika La Plante" title="Erika La Plante deleted content on: 09 Dec, 11:45 PM" class="old" updatedon="09 Dec, 11:45 PM" mytype="content" id="20310b77-d6ab-49b0-8dfb-1e4c1797ada5">using a centrifuge </del>(Horizon 24 Flex, Druker Diagnostics) <ins user="Erika La Plante" title="Erika La Plante inserted content on: 09 Dec, 11:46 PM" class="new" updatedon="09 Dec, 11:46 PM" mytype="content" id="f3b9b0cc-fb60-473d-bea8-3ab9e9126af5">at 2500 rpm </ins>to separate the supernatant. The supernatant was decanted and replaced with an approximately equal volume of ethanol to suppress further reactions. The samples were then centrifuged in ethanol for 15 min, after which the solid precipitates were collected and dried at ambient temperature and pressure. The dried solids were characterized using FTIR <del user="Erika La Plante" title="Erika La Plante deleted content on: 09 Dec, 11:46 PM" class="old" updatedon="09 Dec, 11:46 PM" mytype="content" id="c94b09a6-f98e-49cf-9f56-0947b0c5dd15">with a spectrometer </del>(Nicolet iS50, Thermo Fisher Scientific) over a wavenumber range of 600–4000 cm<sup xmlns="http://www.wiley.com/namespaces/wiley">−1</sup>. X‐ray diffraction patterns were collected using an X‐ray diffractometer (D‐500, Siemens) with Cu Kα radiation source (λ = 1.54 Å), over a 2θ range of 5° to 80°, with a step size of 0.02°, a dwell time of 0.5 s, and operating conditions of 30 mA current and 40 kV voltage. Thermogravimetric analysis was performed using an analyzer (SDT Q600, TA Instruments) under an ultrahigh‐purity (UHP) N<sub xmlns="http://www.wiley.com/namespaces/wiley">2</sub> flow of 20 mL/min, at a heating rate of 15°C/min, from ambient temperature to 1000°C. The sample for AFM imaging was prepared by immersing a freshly cleaved mica substrate (Ted Pella) in a growth solution containing [Mg] = [Si] = 50 mM for 30 min at ambient temperature. At the end of the reaction, the sample was blow‐dried using ultra‐high‐purity N<sub xmlns="http://www.wiley.com/namespaces/wiley">2</sub>. Imaging was performed using a Cypher ES atomic force microscope (Oxford Instruments Asylum Research) with a gold‐coated silicon probe.</span></p>
|
|
</section>
|
|
<section xmlid="jace70435-sec-0040" id="707">
|
|
<div type="main" id="708" class="title" xmlns="">SAXS data collection and analysis</div>
|
|
<p id="709"><span id="710" class="Dummy" xmlns="">SAXS measurements were conducted at beamline 12‐ID‐B of the Advanced Photon Source at Argonne National Laboratory. M‐S‐H samples were prepared following the procedure described in Section <span href="#jace70435-sec-0030" id="711" class="link">2.1</span>. Within 15 s of mixing the stock solutions, the reaction mixtures were loaded into quartz glass capillary tubes (2 mm inner diameter), which were then mounted horizontally in the sample holder. SAXS scans were performed across a 3 mm vertical range within each capillary, using a step size of 0.25 mm. Images collected outside the capillary were identified by the absence of characteristic scattering patterns, whereas those taken at the air‐capillary‐solution interface were distinguished by the presence of specular reflection from the capillary wall. Only images confirmed to be acquired from within the solution‐filled section of the capillary were included in the analys<ins user="Erika La Plante" title="Erika La Plante inserted content on: 09 Dec, 11:52 PM" class="new" updatedon="09 Dec, 11:52 PM" mytype="content" id="0bcdd2ac-3246-449f-b065-39156c6db317">e</ins><del user="Erika La Plante" title="Erika La Plante deleted content on: 09 Dec, 11:52 PM" class="old" updatedon="09 Dec, 11:52 PM" mytype="content" id="e346f7fd-c87b-467a-9fbc-f86e27b904e3">i</del>s.</span></p>
|
|
<p id="713"><span id="714" class="Dummy" xmlns="">Scattering intensities were recorded using a Pilatus 2M detector with an exposure time of 0.2 s. For each sample, three to five scattering patterns were averaged to produce representative profiles. SAXS data collection for each sample was completed within 2 to 3 h, with the exact time of data acquisition recorded as the corresponding reaction time (Table <span href="#jace70435-tbl-0001" id="715" class="link">1</span>).</span></p>
|
|
<p id="717"><span id="718" class="Dummy" xmlns="">Background subtraction was performed using appropriate controls: DI water for samples having Mg and Si concentrations less than 200 mM, and 1 M Mg(NO<sub xmlns="http://www.wiley.com/namespaces/wiley">3</sub>)<sub xmlns="http://www.wiley.com/namespaces/wiley">2</sub> for samples with higher concentrations. This correction accounted for the elevated ionic strength and corresponding variations in the electron density of the solution. Selected SAXS patterns were analyzed using the Irena package<span href="#jace70435-bib-0039" id="721" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">39</sup></span> implemented in Wavemetrics Igor Pro 9 to extract particle volume size distributions. These analyses assume dilute limit conditions, where particle–particle interactions are negligible. As such, there is no structure factor contribution, and only the form factor contributes to the measured intensity (Equation 3)<span href="#jace70435-bib-0040" id="723" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">40</sup></span>:
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</span><span xmlid="jace70435-disp-0003" type="mathematics" id="725" class="displayedItem" xmlns=""><span iamnewelement="True"><i IamNewElement="True" class="fa fa-eye d-none" aria-hidden="true"></i><math display="block" altimg="urn:x-wiley:00027820:media:jace70435:jace70435-math-0007" p7:location="equation/jace70435-math-0007.png" id="727" class="math" xmlns:p7="http://www.wiley.com/namespaces/wiley/wiley"><semantics id="728" xmlns=""><mtable displaystyle="true" id="729"><mtr id="730"><mtd id="731"></mtd><mtd columnalign="left" id="732"><mrow id="733"><mrow id="734"><mi id="735">Measured</mi><mspace width="0.33em" id="736"></mspace><mi id="737">intensity</mi></mrow><mspace width="0.33em" id="738"></mspace><mi id="739">I</mi><mfenced open="(" close=")" id="740"><mi id="741">Q</mi></mfenced></mrow></mtd></mtr><mtr id="742"><mtd id="743"></mtd><mtd columnalign="left" id="744"><mrow id="745"><mspace width="1em" id="746"></mspace><mo linebreak="badbreak" id="747">=</mo><msup id="748"><mfenced separators="" open="|" close="|" id="749"><mrow id="750"><mi mathvariant="normal" id="751">Δ</mi><mi id="752">ρ</mi></mrow></mfenced><mn id="753">2</mn></msup><mo id="754">∫</mo><msup id="755"><mfenced separators="" open="|" close="|" id="756"><mrow id="757"><mi id="758">F</mi><mfenced separators="" open="(" close=")" id="759"><mrow id="760"><mi id="761">Q</mi><mo id="762">,</mo><mi id="763">a</mi></mrow></mfenced></mrow></mfenced><mn id="764">2</mn></msup><msup id="765"><mfenced separators="" open="(" close=")" id="766"><mrow id="767"><mi id="768">V</mi><mfenced open="(" close=")" id="769"><mi id="770">a</mi></mfenced></mrow></mfenced><mn id="771">2</mn></msup><mi id="772">N</mi><mi id="773">P</mi><mfenced open="(" close=")" id="774"><mi id="775">a</mi></mfenced><mi id="776">d</mi><mi id="777">a</mi></mrow></mtd></mtr></mtable><annotation encoding="application/x-tex" id="778"><![CDATA[$$\begin{align}&{\mathrm{Measured\ intensity}}\ I\left( Q \right) \nonumber\\ & \quad= {\left| { \Delta \rho } \right|^2}\int {\left| { F\left( {Q,a} \right)} \right|^2}{\left( {V\left( a \right)} \right)^2}NP\left( a \right)da\end{align}$$]]></annotation></semantics></math><label id="726" xmlns="http://www.wiley.com/namespaces/wiley">3</label></span>
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<span IamPlaceholderForId="727"></span></span></p>
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<p id="779" xmlns=""><span id="780" class="Dummy" xmlns="">Here, <i xmlns="http://www.wiley.com/namespaces/wiley">Δρ</i> represents the electron‐density contrast, <i xmlns="http://www.wiley.com/namespaces/wiley">F(Q,a)</i> is the form factor, <i xmlns="http://www.wiley.com/namespaces/wiley">Q</i> is the momentum transfer, <i xmlns="http://www.wiley.com/namespaces/wiley">V(a)</i> denotes the particle volume, <i xmlns="http://www.wiley.com/namespaces/wiley">N</i> is the number of particles, and <i xmlns="http://www.wiley.com/namespaces/wiley">P(a)</i> is the probability of occurrence of scatterers of dimension <i xmlns="http://www.wiley.com/namespaces/wiley">a</i> (e.g., radius for spherical particles). The fitted parameters in the model include the volume, mean, and standard deviation of particle size distribution. Scattering contrast values of 124.6 × 10<sup xmlns="http://www.wiley.com/namespaces/wiley">20</sup> cm<sup xmlns="http://www.wiley.com/namespaces/wiley">−4</sup> for M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub><del user="Erika La Plante" title="Erika La Plante deleted content on: 09 Dec, 11:54 PM" class="old" updatedon="09 Dec, 11:54 PM" mytype="content" id="ebc66f05-3a9e-454c-89bc-dff9e84d74c0">S</del><ins user="Erika La Plante" title="Erika La Plante inserted content on: 09 Dec, 11:54 PM" class="new" updatedon="09 Dec, 11:54 PM" mytype="content" id="323f520e-c034-4b07-ab3f-9c11fc99c382">-</ins>S<ins user="Erika La Plante" title="Erika La Plante inserted content on: 09 Dec, 10:45 AM" class="new" updatedon="09 Dec, 10:45 AM" mytype="content" id="d5d2d213-eacd-469f-a0e6-f60718bf9d66">-</ins>H and 100.1 × 10<sup xmlns="http://www.wiley.com/namespaces/wiley">20</sup> cm<sup xmlns="http://www.wiley.com/namespaces/wiley">−4</sup> for M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub><del user="Erika La Plante" title="Erika La Plante deleted content on: 09 Dec, 11:54 PM" class="old" updatedon="09 Dec, 11:54 PM" mytype="content" id="3dfc091c-61f3-4b70-8d30-1a61fe0ee359">S</del><ins user="Erika La Plante" title="Erika La Plante inserted content on: 09 Dec, 11:54 PM" class="new" updatedon="09 Dec, 11:54 PM" mytype="content" id="a0e11dc4-0974-43d2-b39a-6d294254393e">-S</ins><ins user="Erika La Plante" title="Erika La Plante inserted content on: 09 Dec, 10:45 AM" class="new" updatedon="09 Dec, 10:45 AM" mytype="content" id="26c9cf9c-0b3e-4fad-8186-ef33612a2909">-</ins>H were used, calculated using the built‐in scattering contrast calculator in the Irena package, based on the densities and chemical compositions reported by Nied et al.<span href="#jace70435-bib-0021" id="794" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">21</sup></span> An aspect ratio of 1 was used, consistent with observations from independent atomic force microscopy (AFM) imaging.<span href="#jace70435-bib-0026" id="796" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">26</sup></span></span></p>
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</section>
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</section>
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<section xmlid="jace70435-sec-0050" id="797" xmlns="http://www.wiley.com/namespaces/wiley">
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<div type="main" id="798" class="title" xmlns="">RESULTS AND DISCUSSION</div>
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<section xmlid="jace70435-sec-0060" id="799">
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<div type="main" id="800" class="title" xmlns="">Geochemical modeling and phase assemblage characterization</div>
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<p id="801"><span id="802" class="Dummy" xmlns="">Three distinct sets of samples were prepared to examine (Set 1) the phase assemblage, (Set 2) the effect of saturation<del user="Erika La Plante" title="Erika La Plante deleted content on: 09 Dec, 11:55 PM" class="old" updatedon="09 Dec, 11:55 PM" mytype="content" id="6cd89623-0196-403d-b644-3ecbd4905e0a"> on the formation of M‐S‐H</del>, and (Set 3) the influence of the [Mg]/[Si] ratio<ins user="Erika La Plante" title="Erika La Plante inserted content on: 09 Dec, 11:55 PM" class="new" updatedon="09 Dec, 11:55 PM" mytype="content" id="c398a11f-4099-497e-aec9-53a075990593"> on the formation of M-S-H</ins>. Detailed experimental conditions are listed in Table <span href="#jace70435-tbl-0001" id="803" class="link">1</span>. Geochemical modeling of saturation indices using PHREEQC shows that under the experimental conditions, the solutions were supersaturated with respect to brucite (Mg(OH)<sub xmlns="http://www.wiley.com/namespaces/wiley">2</sub>), M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub>‐S‐H, and M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H. In <b xmlns="http://www.wiley.com/namespaces/wiley">Set 1</b>, where the saturation index (SI) of brucite was held constant, the SIs of both M‐S‐H phases increased while the [Mg]/[Si] ratio decreased. In Set 2, the [Mg]/[Si] ratio is fixed at 1, while the SI increased with rising concentrations of Mg and Si. Finally, in <b xmlns="http://www.wiley.com/namespaces/wiley">Set 3</b>, the SI of M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub>‐S‐H remained constant, while the SIs for both M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H and brucite increased, concurrent with increasing [Mg]/[Si] ratio.</span></p>
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<p id="812"><span id="813" class="Dummy" xmlns="">In contrast to previous studies where M‐S‐H was synthesized from the reaction of MgO or Mg(OH)<sub xmlns="http://www.wiley.com/namespaces/wiley">2</sub> with silica fume,<span href="#jace70435-bib-0019 #jace70435-bib-0021 #jace70435-bib-0022" id="815" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">19,21,22</sup></span> and wherein the rate‐limiting step is the dissolution of the precursor solids, solution‐based synthesis from soluble magnesium and silicon salts facilitates homogeneous nucleation of M‐S‐H.<span href="#jace70435-bib-0023 #jace70435-bib-0024 #jace70435-bib-0025" id="817" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">23–25</sup></span> Under supersaturated conditions, M‐S‐H has been shown to precipitate rapidly.<span href="#jace70435-bib-0023" id="819" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">23</sup></span> At high concentrations, Na<sup xmlns="http://www.wiley.com/namespaces/wiley">+</sup> and NO<sub xmlns="http://www.wiley.com/namespaces/wiley">3</sub><sup xmlns="http://www.wiley.com/namespaces/wiley">–</sup> ions can increase both solution pH and ionic strength (Table <span href="#jace70435-supinfo-0001" id="823" class="link">S1</span>). Moreover, previous SEM‐EDS analysis on M‐S‐H synthesized using the same aqueous precipitation method as in the present study has shown that the [Mg]/[Si] ratio in the solid was similar to the [Mg]/[Si] ratio in the growth solution, supporting the applicability of the synthesis method.<span href="#jace70435-bib-0026" id="825" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">26</sup></span> <b xmlns="http://www.wiley.com/namespaces/wiley">Set 1</b> experiments were designed to assess the relative proportions of M‐S‐H and brucite in the precipitated solids, as geochemical modeling predicted supersaturation with respect to both phases (Table <span href="#jace70435-tbl-0001" id="828" class="link">1</span>). Importantly, prior studies have shown that when solutions are supersaturated with respect to M‐S‐H, brucite does not form during early reaction times (<3 h).<span href="#jace70435-bib-0024 #jace70435-bib-0025" id="830" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">24,25</sup></span></span></p>
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<p id="831"><span id="832" class="Dummy" xmlns="">Consistent with these findings, <del user="Erika La Plante" title="Erika La Plante deleted content on: 10 Dec, 12:02 AM" class="old" updatedon="10 Dec, 12:02 AM" mytype="content" id="74026306-f308-4f72-9186-b8c66ade8237">our </del>FTIR data confirm the exclusive presence of M‐S‐H and the absence of brucite in all three samples (Figure <span href="#jace70435-fig-0001" id="833" class="link">1A</span>).<span href="#jace70435-bib-0018" id="835" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">18</sup></span> Furthermore, XRD analysis of precipitates formed from a solution containing [Mg] = [Si] = 5, 200, and 500 mM revealed only characteristic M‐S‐H peaks (Figure <span href="#jace70435-fig-0001" id="837" class="link">1B</span>). Brucite undergoes a major dehydroxylation between 300°C and 500°C,<span href="#jace70435-bib-0041" id="839" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">41</sup></span> which is absent in the TGA curve of synthesized M‐S‐H. The two gradual mass losses observed at around 400°C and 600°C are attributed to M‐S‐H.<span href="#jace70435-bib-0021" id="841" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">21</sup></span> Notably, a previous study has shown that the TGA detection limit for brucite is 0.3 wt.% for a heating rate of 10 K/min.<span href="#jace70435-bib-0042" id="843" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">42</sup></span> These observations suggest that brucite does not form under our experimental conditions and that the differences observed in the SAXS data (Section <span href="#jace70435-sec-0070" id="845" class="link">3.2</span>) can be attributed solely to M‐S‐H precipitation. If minor amounts of brucite are present, the precipitation rate would be slightly overestimated, given the smaller molar volume of brucite compared with M‐S‐H (Section <span href="#jace70435-sec-0080" id="847" class="link">3.2.1</span>).</span></p>
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<figure xmlid="jace70435-fig-0001"><div id="851" class="mediaResourceGroup" xmlns="" draggable="false"><span user="Erika La Plante" title="Erika La Plante inserted comments on: 10 Dec, 04:18 PM" class="reComment fas fa-comment" style="margin-top: 304px; margin-left: 100px; z-index: 1000000;" updatedon="10 Dec, 04:18 PM" mytype="comment" id="eb224081-d94e-46dc-8478-191532c53f41"></span><span user="Erika La Plante" title="Erika La Plante inserted comments on: 10 Dec, 04:17 PM" class="reComment fas fa-comment far" style="margin-top: 102px; margin-left: 261px; z-index: 1000000;" updatedon="10 Dec, 04:17 PM" mytype="comment" id="f042ea0e-4697-49bf-8844-f190d26abf0e"></span><img mimetype="image/png" rendition="webOriginal" alt="image" id="854" class="mediaResource e-rte-image e-imginline e-resize tooltipobj" originalsrc="image_n/jace70435-fig-0001.png" src="https://arpasset1.pubmate.in/JACE_EV_JACE70435_fcc841d596c24ac1aa3ecacc8800bb99/ProofLink/image_n/jace70435-fig-0001.png" srchires="https://arpasset1.pubmate.in/JACE_EV_JACE70435_fcc841d596c24ac1aa3ecacc8800bb99/ProofLink/image_m/jace70435-fig-0001-m.png" originalsrchires="image_m/jace70435-fig-0001-m.png" iamrelocated="True" style="" /></div>
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<div type="figureName" id="850" class="title" xmlns="">FIGURE<label id="849" iamrelocated="True" xmlns="http://www.wiley.com/namespaces/wiley">1</label><span id="856" class="caption" xmlns="" iamrelocated="True"><span id="857" class="Dummy">(A) Fourier‐transform infrared (FTIR) spectra of precipitates grown under constant brucite SI with varying M‐S‐H SI (Set 1, Table <span href="#jace70435-tbl-0001" id="858" class="link">1</span>), showing characteristic vibrational bands associated with M‐S‐H<span href="#jace70435-bib-0021 #jace70435-bib-0024 #jace70435-bib-0043 #jace70435-bib-0044 #jace70435-bib-0045" id="860" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">21,24,43–45</sup></span> (Note: <ins user="Erika La Plante" title="Erika La Plante inserted content on: 10 Dec, 04:18 PM" class="new" updatedon="10 Dec, 04:18 PM" mytype="content" id="4ba02f88-f296-4b47-9e44-ab0804fb3517">T</ins><del user="Erika La Plante" title="Erika La Plante deleted content on: 10 Dec, 04:18 PM" class="old" updatedon="10 Dec, 04:18 PM" mytype="content" id="6e140d3d-e82c-4ff0-b8fc-6dcac85330b5">t</del>he peak at ∼2400 cm<sup xmlns="http://www.wiley.com/namespaces/wiley">−1</sup> originates from atmospheric CO<sub xmlns="http://www.wiley.com/namespaces/wiley">2</sub>). In the Q<sup xmlns="http://www.wiley.com/namespaces/wiley">n</sup> notation, <i xmlns="http://www.wiley.com/namespaces/wiley">n</i> represents the number of bridging oxygen atoms, and the subscripts <i xmlns="http://www.wiley.com/namespaces/wiley">s</i> and <i xmlns="http://www.wiley.com/namespaces/wiley">b</i> refer to stretching and bending vibration modes. (B) X‐ray diffraction (XRD) pattern of precipitates grown from a solution containing [Mg] = [Si] = 5, 200, and 500 mM (Set 2, Table <span href="#jace70435-tbl-0001" id="868" class="link">1</span>), compared with reference brucite.<span href="#jace70435-bib-0046" id="870" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">46</sup></span> The absence of sharp brucite peaks and the presence of <del user="Erika La Plante" title="Erika La Plante deleted content on: 10 Dec, 04:19 PM" class="old" updatedon="10 Dec, 04:19 PM" mytype="content" id="f77ef72c-0525-498a-beca-98a1f47d1e7b">diffraction</del><ins user="Erika La Plante" title="Erika La Plante inserted content on: 10 Dec, 04:19 PM" class="new" updatedon="10 Dec, 04:19 PM" mytype="content" id="284b8d29-1c7e-4e6c-8b01-6d43b3a6df7a">broad</ins> peaks at 2θ = 25°, 35°, and 60° confirm the exclusive formation of M‐S‐H under these conditions.<span href="#jace70435-bib-0021 #jace70435-bib-0024 #jace70435-bib-0045 #jace70435-bib-0047" id="872" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">21,24,45,47</sup></span> (C) TGA profiles and differential curve for M‐S‐H precipitated from a growth solution containing [Mg] = [Si] = 200 mM at ambient temperature. (D) Representative AFM image of M‐S‐H precipitate grown for 30 min on a mica substrate by reaction with a solution containing [Mg] = [Si] = 50 mM at ambient temperature.</span></span></div>
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</figure></section>
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<section xmlid="jace70435-sec-0070" id="874" sectionno="3.2" class="Section subSection" xmlns=""><div type="main" id="875" class="title" xmlns="">Quantifications of M‐S‐H precipitation rates and size distribution</div><section xmlid="jace70435-sec-0080" id="876" xmlns=""><div type="main" id="877" class="title" xmlns="">Influence of the degree of supersaturation at constant [Mg]/[Si]</div><p id="878"><span id="879" class="Dummy" xmlns="">Figure <span href="#jace70435-fig-0002" id="880" class="link">2A</span> shows the SAXS intensity profiles of the M‐S‐H samples. The volume distributions were divided into two populations (Figure <span href="#jace70435-fig-0002" id="882" class="link">2B,C</span>) based on distinct changes in the slope of the SAXS curves. Population 1 (Figure <span href="#jace70435-fig-0002" id="884" class="link">2B</span>) was fitted over a Q range of 0.08–0.32 Å<sup xmlns="http://www.wiley.com/namespaces/wiley">−1</sup>, corresponding to probe lengths (2π/Q) between 20 and 79 Å. Population 2 (Figure <span href="#jace70435-fig-0002" id="887" class="link">2C</span>) was fitted over a lower Q range of 0.005–0.08 Å<sup xmlns="http://www.wiley.com/namespaces/wiley">−1</sup>, corresponding to probe lengths of 79 to 126 Å, consistent with the expected dimensions of M‐S‐H particles. For comparison, AFM images of M‐S‐H precipitates grown on mica substrates (Figure <span href="#jace70435-fig-0001" id="890" class="link">1D</span>) indicate that heterogeneously nucleated particles range in diameter from 300 to 1500 Å, representing the Population 2 particle size. The intensities from both Population 1 and 2 were used to calculate the precipitation rate.</span></p><figure xmlid="jace70435-fig-0002" draggable="false"><div id="894" class="mediaResourceGroup" xmlns="" draggable="false"><span user="Erika La Plante" title="Erika La Plante inserted comments on: 10 Dec, 04:25 PM" class="reComment fas fa-comment far" style="margin-top: 95px; margin-left: 118px; z-index: 1000000;" updatedon="10 Dec, 04:25 PM" mytype="comment" id="6b9b55e1-a1b6-404b-a0cd-3db728584ee4"></span><span user="Erika La Plante" title="Erika La Plante inserted comments on: 09 Dec, 10:42 AM" class="reComment fas fa-comment far" style="margin-top: 267px; margin-left: 113px; z-index: 1000000;" updatedon="09 Dec, 10:42 AM" mytype="comment" id="a04507b1-7c13-46ed-8e76-3e84f07204ed"></span><img mimetype="image/png" rendition="webOriginal" alt="image" id="897" class="mediaResource e-rte-image e-imginline e-resize tooltipobj" originalsrc="image_n/jace70435-fig-0002.png" src="https://arpasset1.pubmate.in/JACE_EV_JACE70435_fcc841d596c24ac1aa3ecacc8800bb99/ProofLink/image_n/jace70435-fig-0002.png" srchires="https://arpasset1.pubmate.in/JACE_EV_JACE70435_fcc841d596c24ac1aa3ecacc8800bb99/ProofLink/image_m/jace70435-fig-0002-m.png" originalsrchires="image_m/jace70435-fig-0002-m.png" iamrelocated="True" style="" /></div><div type="figureName" id="893" class="title" xmlns="">FIGURE<label id="892" iamrelocated="True" xmlns="http://www.wiley.com/namespaces/wiley">2</label><span id="899" class="caption" xmlns="" iamrelocated="True"><span id="900" class="Dummy">(A) SAXS patterns of Set 2 samples after 61 min of reaction, with corresponding volume fraction distributions shown in (B) and (C) for M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub>‐S‐H. (D) Volume fractions at various reaction times were used to calculate (E) precipitation rates for M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub>‐S‐H. Volume fraction distributions and volume fractions for M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H are given in Figure <span href="#jace70435-supinfo-0001" id="904" class="link">S1</span> in the Supporting Information. (F) Precipitation rate for M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H.</span></span></div></figure><p id="907"><span id="908" class="Dummy" xmlns="">We have also attempted to evaluate the contribution of larger secondary particles, representing M‐S‐H aggregates.<span href="#jace70435-bib-0026" id="909" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">26</sup></span> However, the SAXS fitting in this size range exhibited high uncertainty, as these dimensions fall beyond the range that is fully defined by the SAXS measurements. <del user="Erika La Plante" title="Erika La Plante deleted content on: 09 Dec, 10:48 AM" class="old" updatedon="09 Dec, 10:48 AM" mytype="content" id="6433bd54-fc88-41b8-8c04-00463cc3426a">The intensities from both Populations 1 and 2 were used to calculate the precipitation rate.</del></span></p><p id="911"><span id="912" class="Dummy" xmlns="">The volume fraction of M‐S‐H particles increased over time as a result of homogeneous nucleation (Figure <span href="#jace70435-fig-0002" id="913" class="link">2B,C</span>). The particle size distribution, expressed as </span><i iamnewelement="True" class="fa fa-eye d-none" aria-hidden="true" xmlns=""></i><math xmlns="" display="inline" altimg="urn:x-wiley:00027820:media:jace70435:jace70435-math-0008" p7:location="equation/jace70435-math-0008.png" xmlns:p7="http://www.wiley.com/namespaces/wiley/wiley" class="math" id="915"><semantics xmlns=""><mfrac><mrow><mi>d</mi><mi>V</mi></mrow><mrow><mi>d</mi><mi>r</mi></mrow></mfrac><annotation encoding="application/x-tex">$\frac{{dV}}{{dr}}$</annotation></semantics></math><span id="925" class="Dummy" xmlns=""> (the change in particle volume, <i xmlns="http://www.wiley.com/namespaces/wiley">V</i>, with respect to radius, <i xmlns="http://www.wiley.com/namespaces/wiley">r</i>) provides insight into dispersity, morphology, and the degree of aggregation within cementitious systems.<span href="#jace70435-bib-0007 #jace70435-bib-0008 #jace70435-bib-0010" id="928" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">7,8,10</sup></span> Accurately characterizing this distribution is critical for modeling and interpreting the material's mechanical properties.<span href="#jace70435-bib-0034" id="930" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">34</sup></span></span></p><p id="931"><span id="932" class="Dummy" xmlns="">The volume fraction, <i xmlns="http://www.wiley.com/namespaces/wiley">f</i>, is defined as the ratio of the precipitate volume (<i xmlns="http://www.wiley.com/namespaces/wiley"><span id="934" class="Dummy" xmlns="">V</span><sub>P</sub></i>) to the solution volume of solution (<i xmlns="http://www.wiley.com/namespaces/wiley"><span id="936" class="Dummy" xmlns="">V</span><sub>S</sub></i>), that is, <i xmlns="http://www.wiley.com/namespaces/wiley">f</i> = </span><i iamnewelement="True" class="fa fa-eye d-none" aria-hidden="true" xmlns=""></i><math xmlns="" display="inline" altimg="urn:x-wiley:00027820:media:jace70435:jace70435-math-0009" p7:location="equation/jace70435-math-0009.png" xmlns:p7="http://www.wiley.com/namespaces/wiley/wiley" class="math" id="939"><semantics xmlns=""><mfrac><msub><mi>V</mi><mi>P</mi></msub><msub><mi>V</mi><mi>S</mi></msub></mfrac><annotation encoding="application/x-tex">$\frac{{{V_P}}}{{{V_S}}}$</annotation></semantics></math><span id="949" class="Dummy" xmlns="">, and obtained by integrating the size distribution curve over the <i xmlns="http://www.wiley.com/namespaces/wiley">r</i> range. The molar volumes (<i xmlns="http://www.wiley.com/namespaces/wiley"><span id="951" class="Dummy" xmlns="">V</span><sub>M</sub></i>) of M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub>‐S‐H or M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H phases have been previously reported as 189.8 and 148.6 cm<sup xmlns="http://www.wiley.com/namespaces/wiley">3</sup>/mol. The molar volume (in cm<sup xmlns="http://www.wiley.com/namespaces/wiley">3</sup>/mol) is defined by Equation (4)<span href="#jace70435-bib-0021" id="957" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">21</sup></span>:</span><span xmlid="jace70435-disp-0004" type="mathematics" id="959" class="displayedItem" xmlns=""><span iamnewelement="True"><i iamnewelement="True" class="fa fa-eye d-none" aria-hidden="true"></i><math xmlns="http://www.w3.org/1998/Math/MathML" display="block" altimg="urn:x-wiley:00027820:media:jace70435:jace70435-math-0010" p8:location="equation/jace70435-math-0010.png" xmlns:p8="http://www.wiley.com/namespaces/wiley/wiley" class="math" id="961"><semantics xmlns=""><mtable displaystyle="true"><mtr><mtd columnalign="right"><mrow><msub><mi>V</mi><mi>M</mi></msub><mo linebreak="badbreak">=</mo><mfrac><msub><mi>V</mi><mi>P</mi></msub><mi>n</mi></mfrac><mo>,</mo></mrow></mtd></mtr></mtable><annotation encoding="application/x-tex">$$\begin{align}{V_M} = \frac{{{V_P}}}{n},\end{align}$$</annotation></semantics></math><label id="960" xmlns="http://www.wiley.com/namespaces/wiley">4</label></span><span iamplaceholderforid="961"></span></span><span id="978" class="Dummy" xmlns="">where <i xmlns="http://www.wiley.com/namespaces/wiley">n</i> is the number of moles.</span></p><p id="980"><span id="981" class="Dummy" xmlns="">Accordingly, the precipitation rate, <i xmlns="http://www.wiley.com/namespaces/wiley">r</i> (in mol/L/s), can be calculated using Equation (5):</span><span xmlid="jace70435-disp-0005" type="mathematics" id="983" class="displayedItem" xmlns=""><span iamnewelement="True"><i iamnewelement="True" class="fa fa-eye d-none" aria-hidden="true"></i><math xmlns="http://www.w3.org/1998/Math/MathML" display="block" altimg="urn:x-wiley:00027820:media:jace70435:jace70435-math-0011" p8:location="equation/jace70435-math-0011.png" xmlns:p8="http://www.wiley.com/namespaces/wiley/wiley" class="math" id="985"><semantics xmlns=""><mtable displaystyle="true"><mtr><mtd columnalign="right"><mrow><mi>r</mi><mo linebreak="badbreak">=</mo><mfrac><mi>n</mi><mrow><msub><mi>V</mi><mi>S</mi></msub><mspace width="0.33em"></mspace><mi>t</mi></mrow></mfrac><mo linebreak="goodbreak">=</mo><mfrac><msub><mi>V</mi><mi>P</mi></msub><mrow><msub><mi>V</mi><mrow><mi>M</mi><mo>·</mo></mrow></msub><msub><mi>V</mi><mi>S</mi></msub><mspace width="0.33em"></mspace><mi>t</mi></mrow></mfrac><mo linebreak="goodbreak">=</mo><mfrac><mi>f</mi><mrow><msub><mi>V</mi><mi>M</mi></msub><mspace width="0.33em"></mspace><mi>t</mi></mrow></mfrac><mo>,</mo></mrow></mtd></mtr></mtable><annotation encoding="application/x-tex">$$\begin{align}r = \frac{n}{{{V_{S}}\ t}} = \frac{{{V_P}}}{{{V_{M \cdot }} {V_{S}}\ t}} = \frac{f}{{{V_{M}}\ t}},\end{align}$$</annotation></semantics></math><label id="984" xmlns="http://www.wiley.com/namespaces/wiley">5</label></span><span iamplaceholderforid="985"></span></span><span id="1028" class="Dummy" xmlns="">where <i xmlns="http://www.wiley.com/namespaces/wiley">t</i> is the reaction time in seconds.</span></p><p id="1030"><span id="1031" class="Dummy" xmlns="">Because the individual contributions of the two endmember M‐S‐H phases to the total precipitate volume could not be distinguished, upper and lower bounds for the growth rate were estimated by assuming the precipitates consisted entirely of either M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub>‐S‐H or M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H. In the <b xmlns="http://www.wiley.com/namespaces/wiley">Set 2</b> experiments, the [Mg]/[Si] ratio was held constant, while the saturation indices with respect to both M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub>‐S‐H or M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H increased. SAXS fitting results revealed that the volume distribution ranges remained similar across samples, indicating that variations in SI alone do not significantly affect the size of primary M‐S‐H particulates over the radius range 20–1000 Å (Figure <span href="#jace70435-fig-0002" id="1037" class="link">2A–C</span>). Moreover, the integrated area, which is proportional to the precipitate volume fraction, increased with increasing concentration (Figure <span href="#jace70435-fig-0002" id="1039" class="link">2D</span>). A decline in precipitation over time was also observed, consistent with the decreasing availability of Mg<sup xmlns="http://www.wiley.com/namespaces/wiley">2+</sup> and Si(OH)<sub xmlns="http://www.wiley.com/namespaces/wiley">3</sub>O<sup xmlns="http://www.wiley.com/namespaces/wiley">–</sup> ions in solution and a reduction in SI over time (Figure <span href="#jace70435-fig-0002" id="1044" class="link">2E,F</span>). Therefore, to determine the limiting growth rate at a given SI, the calculated rates were <del user="Erika La Plante" title="Erika La Plante deleted content on: 10 Dec, 05:14 PM" class="old" updatedon="10 Dec, 05:14 PM" mytype="content" id="21baf859-1831-40be-80b7-1d09eb21748b">linearly </del>extrapolated to time zero (Figure <span href="#jace70435-fig-0003" id="1046" class="link">3</span>, Table <span href="#jace70435-tbl-0002" id="1048" class="link">2</span>).</span></p><figure xmlid="jace70435-fig-0003" draggable="false"><div id="1052" class="mediaResourceGroup" xmlns="" draggable="false"><span user="Erika La Plante" title="Erika La Plante inserted comments on: 10 Dec, 05:07 PM" class="reComment fas fa-comment" style="margin-top: 79px; margin-left: 319px; z-index: 1000000;" updatedon="10 Dec, 05:07 PM" mytype="comment" id="3c62e218-7cf9-4285-85e2-7861ca380f0f"></span><span user="Erika La Plante" title="Erika La Plante inserted comments on: 10 Dec, 05:07 PM" class="reComment fas fa-comment" style="margin-top: 83px; margin-left: 94px; z-index: 1000000;" updatedon="10 Dec, 05:07 PM" mytype="comment" id="ec39510c-6ac8-4828-9880-735554cc158b"></span><img mimetype="image/png" rendition="webOriginal" alt="image" id="1055" class="mediaResource e-rte-image e-imginline e-resize tooltipobj" originalsrc="image_n/jace70435-fig-0003.png" src="https://arpasset1.pubmate.in/JACE_EV_JACE70435_fcc841d596c24ac1aa3ecacc8800bb99/ProofLink/image_n/jace70435-fig-0003.png" srchires="https://arpasset1.pubmate.in/JACE_EV_JACE70435_fcc841d596c24ac1aa3ecacc8800bb99/ProofLink/image_m/jace70435-fig-0003-m.png" originalsrchires="image_m/jace70435-fig-0003-m.png" iamrelocated="True" style="" /></div><div type="figureName" id="1051" class="title" xmlns="">FIGURE<label id="1050" iamrelocated="True" xmlns="http://www.wiley.com/namespaces/wiley">3</label><span id="1057" class="caption" xmlns="" iamrelocated="True">(A, B) E<del user="Erika La Plante" title="Erika La Plante deleted content on: 10 Dec, 05:14 PM" class="old" updatedon="10 Dec, 05:14 PM" mytype="content" id="b9c6afdb-d2b8-4d6a-b323-998bd6a2e009">xponential e</del>xtrapolation of experimental data to estimate the initial total precipitation rate at time zero. (C) Initial total precipitation rates plotted as a function of the saturation ratio, with fits based on an affinity‐driven kinetic framework.</span></div></figure><div xmlid="jace70435-tbl-0002" prights="unknown" erights="yes" copyright="John Wiley & Sons, Ltd." id="1058" class="tabular" xmlns=""><span iamplaceholderforid="1059"></span><div id="1060" class="titleGroup"><div type="tabularName" id="1061" class="title">TABLE<label id="1059" xmlns="http://www.wiley.com/namespaces/wiley" iamrelocated="True">2</label><span type="main" id="1062" class="title" iamrelocated="True">Extrapolated M‐S‐H precipitation rates as a function of SI.</span></div><span iamplaceholderforid="1062"></span></div><span iamplaceholderforid="1146"></span><div iamnewelement="True" class="TableOverFlow"><tgroup cols="5"><colspec colnum="1" colname="col1" align="left" id="1063" class="colspec" xmlns=""></colspec><colspec colnum="2" colname="col2" align="left" id="1064" class="colspec" xmlns=""></colspec><colspec colnum="3" colname="col3" align="left" id="1065" class="colspec" xmlns=""></colspec><colspec colnum="4" colname="col4" align="left" id="1066" class="colspec" xmlns=""></colspec><colspec colnum="5" colname="col5" align="left" id="1067" class="colspec" xmlns=""></colspec></tgroup><table frame="topbot" xmlns="http://www.wiley.com/namespaces/wiley"><thead><tr id="1068" xmlns=""><th colname="col1" id="1069" class="thentry"></th><th colname="col2" namest="col2" nameend="col3" rowsep="1" id="1070" colspan="2" class=""><span id="1071" class="Dummy">M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub><del user="Erika La Plante" title="Erika La Plante deleted content on: 10 Dec, 05:15 PM" class="old" updatedon="10 Dec, 05:15 PM" mytype="content" id="4f8d265b-1a80-4291-a292-395b5c65c8c7">S</del><ins user="Erika La Plante" title="Erika La Plante inserted content on: 10 Dec, 05:14 PM" class="new" updatedon="10 Dec, 05:14 PM" mytype="content" id="b8ea5db5-be9c-4d9e-828f-7eea82999879">-S</ins><ins user="Erika La Plante" title="Erika La Plante inserted content on: 09 Dec, 10:46 AM" class="new" updatedon="09 Dec, 10:46 AM" mytype="content" id="b622ce44-1487-41dd-8cd3-2fae000c7baf">-</ins>H</span></th><th colname="col4" namest="col4" nameend="col5" rowsep="1" id="1073" colspan="2" class=""><span id="1074" class="Dummy">M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub><del user="Erika La Plante" title="Erika La Plante deleted content on: 10 Dec, 05:15 PM" class="old" updatedon="10 Dec, 05:15 PM" mytype="content" id="39d19caa-6644-4f03-ae7c-7372e9d8c892">S</del><ins user="Erika La Plante" title="Erika La Plante inserted content on: 10 Dec, 05:15 PM" class="new" updatedon="10 Dec, 05:15 PM" mytype="content" id="a1b28ebe-dba4-4b9b-8394-b2644aa4cad9">-</ins><ins user="Erika La Plante" title="Erika La Plante inserted content on: 10 Dec, 05:15 PM" class="new" updatedon="10 Dec, 05:15 PM" mytype="content" id="d1391e54-0f59-4648-86ed-fdfcb8a7484d">S</ins><ins user="Erika La Plante" title="Erika La Plante inserted content on: 09 Dec, 10:46 AM" class="new" updatedon="09 Dec, 10:46 AM" mytype="content" id="2624d845-7d28-4305-8508-851522cecca4">-</ins>H</span></th></tr><tr rowsep="1" id="1076" xmlns=""><th colname="col1" id="1077" class="thentry">[Mg] = [Si] Concentration (mM)</th><th colname="col2" id="1078" class="thentry">Saturation index (SI)</th><th colname="col3" id="1079" class="thentry"><span id="1080" class="Dummy">Precipitation rate (×10<sup xmlns="http://www.wiley.com/namespaces/wiley">−7</sup> mol/L/s)</span></th><th colname="col4" id="1082" class="thentry">Saturation index (SI)</th><th colname="col5" id="1083" class="thentry"><span id="1084" class="Dummy">Precipitation rate (×10<sup xmlns="http://www.wiley.com/namespaces/wiley">−7</sup> mol/L/s)</span></th></tr></thead><tbody><tr id="1086" xmlns=""><td colname="col1" id="1087" class="entry">2</td><td colname="col2" id="1088" class="entry">5.97</td><td colname="col3" id="1089" class="entry">3.84</td><td colname="col4" id="1090" class="entry">5.81</td><td colname="col5" id="1091" class="entry">6.45</td></tr><tr id="1092" xmlns=""><td colname="col1" id="1093" class="entry">5</td><td colname="col2" id="1094" class="entry">6.58</td><td colname="col3" id="1095" class="entry">24.62</td><td colname="col4" id="1096" class="entry">6.61</td><td colname="col5" id="1097" class="entry">42.71</td></tr><tr id="1098" xmlns=""><td colname="col1" id="1099" class="entry">10</td><td colname="col2" id="1100" class="entry">7.00</td><td colname="col3" id="1101" class="entry">26.25</td><td colname="col4" id="1102" class="entry">7.19</td><td colname="col5" id="1103" class="entry">44.92</td></tr><tr id="1104" xmlns=""><td colname="col1" id="1105" class="entry">25</td><td colname="col2" id="1106" class="entry">7.51</td><td colname="col3" id="1107" class="entry">69.24</td><td colname="col4" id="1108" class="entry">7.93</td><td colname="col5" id="1109" class="entry">109.54</td></tr><tr id="1110" xmlns=""><td colname="col1" id="1111" class="entry">50</td><td colname="col2" id="1112" class="entry">7.88</td><td colname="col3" id="1113" class="entry">88.83</td><td colname="col4" id="1114" class="entry">8.49</td><td colname="col5" id="1115" class="entry">144.64</td></tr><tr id="1116" xmlns=""><td colname="col1" id="1117" class="entry">100</td><td colname="col2" id="1118" class="entry">8.21</td><td colname="col3" id="1119" class="entry">164.58</td><td colname="col4" id="1120" class="entry">9.06</td><td colname="col5" id="1121" class="entry">260.02</td></tr><tr id="1122" xmlns=""><td colname="col1" id="1123" class="entry">200</td><td colname="col2" id="1124" class="entry">8.52</td><td colname="col3" id="1125" class="entry">415.77</td><td colname="col4" id="1126" class="entry">9.63</td><td colname="col5" id="1127" class="entry">614.52</td></tr><tr id="1128" xmlns=""><td colname="col1" id="1129" class="entry">300</td><td colname="col2" id="1130" class="entry">8.69</td><td colname="col3" id="1131" class="entry">454.00</td><td colname="col4" id="1132" class="entry">9.96</td><td colname="col5" id="1133" class="entry">633.85</td></tr><tr id="1134" xmlns=""><td colname="col1" id="1135" class="entry">400</td><td colname="col2" id="1136" class="entry">8.82</td><td colname="col3" id="1137" class="entry">530.22</td><td colname="col4" id="1138" class="entry">10.19</td><td colname="col5" id="1139" class="entry">748.73</td></tr><tr id="1140" xmlns=""><td colname="col1" id="1141" class="entry">500</td><td colname="col2" id="1142" class="entry">8.94</td><td colname="col3" id="1143" class="entry">509.98</td><td colname="col4" id="1144" class="entry">10.35</td><td colname="col5" id="1145" class="entry">774.89</td></tr></tbody></table></div><div iamnewxmlelement="true" id="1146" class="noteGroup"></div></div><p id="1147"><span id="1148" class="Dummy" xmlns="">The precipitation rates of M‐S‐H were modeled using the affinity‐based kinetics (ABK) framework, which applies to both mineral dissolution and precipitation.<span href="#jace70435-bib-0048 #jace70435-bib-0049 #jace70435-bib-0050" id="1149" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">48–50</sup></span> This model assumes that the reaction rate is governed by the system's thermodynamic driving force, typically expressed either as <span user="Erika La Plante" title="Erika La Plante inserted comments on: 10 Dec, 05:18 PM" class="reComment fas fa-comment" style="" updatedon="10 Dec, 05:18 PM" mytype="comment" id="83833f8d-e75c-45a8-9098-a300c162779d"></span><i xmlns="http://www.wiley.com/namespaces/wiley">Ω</i> or the change in Gibbs free energy (ΔG). It also simplifies the full rate law in scenarios where multiple elementary reactions contribute to the overall rate. Additionally, the model assumes surface‐controlled kinetics. The general precipitation rate law is expressed as Equation (6)<span href="#jace70435-bib-0048 #jace70435-bib-0049 #jace70435-bib-0050" id="1152" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">48–50</sup></span>:</span><span xmlid="jace70435-disp-0006" type="mathematics" id="1154" class="displayedItem" xmlns=""><span iamnewelement="True"><i iamnewelement="True" class="fa fa-eye d-none" aria-hidden="true"></i><math xmlns="http://www.w3.org/1998/Math/MathML" display="block" altimg="urn:x-wiley:00027820:media:jace70435:jace70435-math-0012" p8:location="equation/jace70435-math-0012.png" xmlns:p8="http://www.wiley.com/namespaces/wiley/wiley" class="math" id="1156"><semantics xmlns=""><mrow><mi>r</mi><mo linebreak="badbreak">=</mo><mi>k</mi><mfenced separators="" open="(" close=")"><msup><mi>e</mi><mfrac><mrow><mi>n</mi><mi mathvariant="normal">Δ</mi><mi>G</mi></mrow><mrow><mi>R</mi><mi>T</mi></mrow></mfrac></msup><mo>−</mo><mn>1</mn></mfenced><mo>,</mo></mrow><annotation encoding="application/x-tex">$$\begin{equation}r = k\left({e^{\frac{{n\Delta G}}{{RT}}}} - 1\right),\end{equation}$$</annotation></semantics></math><label id="1155" xmlns="http://www.wiley.com/namespaces/wiley">6</label></span><span iamplaceholderforid="1156"></span></span><span id="1177" class="Dummy" xmlns="">where <i xmlns="http://www.wiley.com/namespaces/wiley">r</i> is the precipitation rate in mol/L/s, ΔG = <i xmlns="http://www.wiley.com/namespaces/wiley">RT</i> ln Ω, <i xmlns="http://www.wiley.com/namespaces/wiley">R</i> is the gas constant in J/K, <i xmlns="http://www.wiley.com/namespaces/wiley">T</i> is the temperature in Kelvin, <i xmlns="http://www.wiley.com/namespaces/wiley">k</i> is the apparent rate constant (mol/L/s), and <i xmlns="http://www.wiley.com/namespaces/wiley">n</i> is an empirical coefficient. This expression can be further simplified to Equation (7)<span href="#jace70435-bib-0051" id="1184" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">51</sup></span>:</span><span xmlid="jace70435-disp-0007" type="mathematics" id="1186" class="displayedItem" xmlns=""><span iamnewelement="True"><i iamnewelement="True" class="fa fa-eye d-none" aria-hidden="true"></i><math xmlns="http://www.w3.org/1998/Math/MathML" display="block" altimg="urn:x-wiley:00027820:media:jace70435:jace70435-math-0013" p8:location="equation/jace70435-math-0013.png" xmlns:p8="http://www.wiley.com/namespaces/wiley/wiley" class="math" id="1188"><semantics xmlns=""><mrow><mi>r</mi><mo linebreak="badbreak">=</mo><msup><mn>10</mn><mi>a</mi></msup><mfenced separators="" open="(" close=")"><mrow><msup><mi mathvariant="normal">Ω</mi><mi>b</mi></msup><mo>−</mo><mn>1</mn></mrow></mfenced><mo>,</mo></mrow><annotation encoding="application/x-tex">$$\begin{equation}r = {10^a} \left( {{{{\Omega}}^b} - 1} \right),\end{equation}$$</annotation></semantics></math><label id="1187" xmlns="http://www.wiley.com/namespaces/wiley">7</label></span><span iamplaceholderforid="1188"></span></span><span id="1205" class="Dummy" xmlns="">where 10<i xmlns="http://www.wiley.com/namespaces/wiley"><sup>a</sup></i> is the rate coefficient (s<sup xmlns="http://www.wiley.com/namespaces/wiley">−1</sup>), and <i xmlns="http://www.wiley.com/namespaces/wiley">b</i> is an empirical constant that reflects the rate's sensitivity to changes in saturation ratio. Based on the experimental data presented above, the best‐fit rate equations for M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub>‐S‐H and M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.5</sub>‐S‐H were determined to be Equations (8) and (9):</span><span xmlid="jace70435-disp-0008" type="mathematics" id="1211" class="displayedItem" xmlns="" numbered="yes"><span iamnewelement="True"><i iamnewelement="True" class="fa fa-eye" aria-hidden="true"></i><math xmlns="http://www.w3.org/1998/Math/MathML" display="block" altimg="urn:x-wiley:00027820:media:jace70435:jace70435-math-0014" p8:location="equation/jace70435-math-0014.png" xmlns:p8="http://www.wiley.com/namespaces/wiley/wiley" math="" user="Erika La Plante" isdeleteenable="true" updatedon="09 Dec, 08:14 PM" emptyvalue="true" 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" 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" mytype="equation" class="math updated-math" id="1248"><mrow xmlns=""><mtable displaystyle="true" xmlns="http://www.w3.org/1998/Math/MathML"><mtr><mtd columnalign="right"><msub><mi>r</mi><mrow><msub><mi mathvariant="normal">M</mi><mn>1.50</mn></msub><mo>-</mo><mi mathvariant="normal">S</mi><mo>-</mo><mi mathvariant="normal">H</mi></mrow></msub><mo>=</mo><msup><mn>10</mn><mrow><mo>−</mo><mn>8.21</mn><mo>±</mo><mn>0.45</mn></mrow></msup><mfenced open="(" close=")" separators=""><mrow><msup><mi mathvariant="normal">Ω</mi><mrow><mn>0.36</mn><mo>±</mo><mn>0.04</mn></mrow></msup><mo>−</mo><mn>1</mn></mrow></mfenced><mo>.</mo></mtd></mtr></mtable></mrow></math><mathold style="display: none;" iamrelocated="True"><math xmlns="http://www.w3.org/1998/Math/MathML" display="block" altimg="urn:x-wiley:00027820:media:jace70435:jace70435-math-0015" p8:location="equation/jace70435-math-0015.png" xmlns:p8="http://www.wiley.com/namespaces/wiley/wiley" math="" class="math"><mtable displaystyle="true"><mtr><mtd columnalign="right"><mrow><msub><mi>r</mi><mrow><msub><mi mathvariant="normal">M</mi><mn>1.50</mn></msub><mi>SH</mi></mrow></msub><mo linebreak="badbreak">=</mo><msup><mn>10</mn><mrow><mo>−</mo><mn>8.21</mn><mo>±</mo><mn>0.45</mn></mrow></msup><mfenced separators="" open="(" close=")"><mrow><msup><mi mathvariant="normal">Ω</mi><mrow><mn>0.36</mn><mo>±</mo><mn>0.04</mn></mrow></msup><mo>−</mo><mn>1</mn></mrow></mfenced><mo>.</mo></mrow></mtd></mtr></mtable></math></mathold><label id="1247" xmlns="http://www.wiley.com/namespaces/wiley">9</label></span><span iamplaceholderforid="1248"></span></span></p><p id="1281"><span id="1282" class="Dummy" xmlns="">These results indicate that M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub>‐S‐H precipitates at a significantly slower rate than M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H, but with less sensitivity to variations in the saturation state. The precipitation rates are on the order of 10<sup xmlns="http://www.wiley.com/namespaces/wiley">−7</sup> to 10<sup xmlns="http://www.wiley.com/namespaces/wiley">−5</sup> mol/L/s, depending on the SI and reaction time (Figure <span href="#jace70435-fig-0002" id="1287" class="link">2E,F</span>). This range aligns with the lower end of the reported homogeneous C‐S‐H precipitation rates, which span from 10<sup xmlns="http://www.wiley.com/namespaces/wiley">−7</sup> to 10<sup xmlns="http://www.wiley.com/namespaces/wiley">−4</sup> mol/L/s under similar conditions, that is, SI values between 2.6 and 10.7 at pH 10.<span href="#jace70435-bib-0052" id="1291" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">52</sup></span> The slower rate for M‐S‐H may be attributed to the stronger hydration of magnesium ions,<span href="#jace70435-bib-0053 #jace70435-bib-0054" id="1293" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">53,54</sup></span> which hinders the interaction between Mg<sup xmlns="http://www.wiley.com/namespaces/wiley">2+</sup> and silicate species, thereby reducing precipitation rate compared with calcium‐based systems.</span></p></section><section xmlid="jace70435-sec-0090" id="1296"><div type="main" id="1297" class="title" xmlns=""><span user="Erika La Plante" title="Erika La Plante inserted comments on: 11 Dec, 04:10 AM" class="reComment fas fa-comment" style="" updatedon="11 Dec, 04:10 AM" mytype="comment" id="be99a260-e75d-4748-b9ca-d0c5825a0800"></span>Influence of the [Mg]/[Si] ratio</div><p id="1298"><span id="1299" class="Dummy" xmlns="">In the Set 1 experiments, where the SI with respect to brucite was held constant, a shift of particle size distribution toward larger <span user="Erika La Plante" title="Erika La Plante inserted comments on: 10 Dec, 05:41 PM" class="reComment fas fa-comment" style="" updatedon="10 Dec, 05:41 PM" mytype="comment" id="71f1b3f9-a358-4956-a115-e15763d2f5cc"></span><i xmlns="http://www.wiley.com/namespaces/wiley">Q</i> values was detected (Figure <span href="#jace70435-fig-0004" id="1301" class="link">4A</span>), indicating a reduction in precipitate size (Figure <span href="#jace70435-fig-0004" id="1303" class="link">4B</span>). Specifically, the second population in the distribution showed a shift toward smaller average sizes (from 450 to 94 Å) as the [Mg]/[Si] ratio decreased (Figure <span href="#jace70435-fig-0004" id="1305" class="link">4B</span>). This reduction in particle size with decreasing [Mg]/[Si] ratio can be attributed to silicate chain oligomerization at high [Mg]/[Si] ratio, where the abundance of Mg<sup xmlns="http://www.wiley.com/namespaces/wiley">2+</sup> ions in solution promotes the condensation of silicate species.<span href="#jace70435-bib-0023" id="1308" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">23</sup></span> Silicate oligomerization happens rapidly at pH 8 and decreases as pH increases.<span href="#jace70435-bib-0055" id="1310" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">55</sup></span> Coincidentally, with increased nitrate and silicate, an increase in both ionic strength and pH was observed (Table <span href="#jace70435-tbl-0003" id="1312" class="link">3</span>). Therefore, a high [Mg]/[Si] ratio combined with lower pH may contribute to the faster silicate oligomerization. This behavior was not observed in Set 2 experiments with a [Mg]/[Si] ratio of 1.00, suggesting that the effect is specific to decreasing ratios of 1.00, 0.65, and 0.39 (Table <span href="#jace70435-tbl-0003" id="1314" class="link">3</span>). Meanwhile, the number of particles increased substantially, by two orders of magnitude (Figure <span href="#jace70435-fig-0004" id="1316" class="link">4C</span>).</span></p><figure xmlid="jace70435-fig-0004" draggable="false"><div id="1320" class="mediaResourceGroup" xmlns="" draggable="false"><span user="Erika La Plante" title="Erika La Plante inserted comments on: 09 Dec, 09:10 PM" class="reComment fas fa-comment far" style="margin-top: 51px; margin-left: 101px; z-index: 1000000;" updatedon="09 Dec, 09:10 PM" mytype="comment" id="d319d26c-4f62-46f1-a956-8c7451d8aeb0"></span><span user="Erika La Plante" title="Erika La Plante inserted comments on: 09 Dec, 10:45 AM" class="reComment fas fa-comment far" style="margin-top: 109px; margin-left: 481px; z-index: 1000000;" updatedon="09 Dec, 10:45 AM" mytype="comment" id="a1db149d-da8b-4461-b6fd-378957f097d6"></span><img mimetype="image/png" rendition="webOriginal" alt="image" id="1323" class="mediaResource e-rte-image e-imginline e-resize tooltipobj" originalsrc="image_n/jace70435-fig-0004.png" src="https://arpasset1.pubmate.in/JACE_EV_JACE70435_fcc841d596c24ac1aa3ecacc8800bb99/ProofLink/image_n/jace70435-fig-0004.png" srchires="https://arpasset1.pubmate.in/JACE_EV_JACE70435_fcc841d596c24ac1aa3ecacc8800bb99/ProofLink/image_m/jace70435-fig-0004-m.png" originalsrchires="image_m/jace70435-fig-0004-m.png" iamrelocated="True" style="" /></div><div type="figureName" id="1319" class="title" xmlns="">FIGURE<label id="1318" iamrelocated="True" xmlns="http://www.wiley.com/namespaces/wiley">4</label><span id="1325" class="caption" xmlns="" iamrelocated="True"><span id="1326" class="Dummy">(A) SAXS patterns from Set 1 experiments showing an increase in intensity with increasing SI, which coincides with a decrease in [Mg]:[Si]. (B, C) The corresponding volume size distribution and particle number distribution, assuming the formation of M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub>‐S‐H, both shift toward smaller particle sizes. Volume fraction and particle number distributions for M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H are given in Figure <span href="#jace70435-supinfo-0001" id="1329" class="link">S2</span>.</span></span></div></figure><div xmlid="jace70435-tbl-0003" prights="unknown" erights="yes" copyright="John Wiley & Sons, Ltd." id="1331" class="tabular" xmlns=""><span iamplaceholderforid="1332"></span><div id="1333" class="titleGroup"><div type="tabularName" id="1334" class="title">TABLE<label id="1332" xmlns="http://www.wiley.com/namespaces/wiley" iamrelocated="True">3</label><span type="main" id="1335" class="title" iamrelocated="True">M‐S‐H precipitation rates from Set 1 experiments conducted with a constant brucite SI, varying M‐S‐H SI, and at a reaction time of 24 min.</span></div><span iamplaceholderforid="1335"></span></div><span iamplaceholderforid="1411"></span><div iamnewelement="True" class="TableOverFlow"><tgroup cols="11"><colspec colnum="1" colname="col1" align="left" id="1336" class="colspec" xmlns=""></colspec><colspec colnum="2" colname="col2" align="left" id="1337" class="colspec" xmlns=""></colspec><colspec colnum="3" colname="col3" align="left" id="1338" class="colspec" xmlns=""></colspec><colspec colnum="4" colname="col4" align="left" id="1339" class="colspec" xmlns=""></colspec><colspec colnum="5" colname="col5" align="left" id="1340" class="colspec" xmlns=""></colspec><colspec colnum="6" colname="col6" align="left" id="1341" class="colspec" xmlns=""></colspec><colspec colnum="7" colname="col7" align="left" id="1342" class="colspec" xmlns=""></colspec><colspec colnum="8" colname="col8" align="left" id="1343" class="colspec" xmlns=""></colspec><colspec colnum="9" colname="col9" align="left" id="1344" class="colspec" xmlns=""></colspec><colspec colnum="10" colname="col10" align="left" id="1345" class="colspec" xmlns=""></colspec><colspec colnum="11" colname="col11" align="left" id="1346" class="colspec" xmlns=""></colspec></tgroup><table frame="topbot" xmlns="http://www.wiley.com/namespaces/wiley"><thead><tr id="1347" xmlns=""><th colname="col1" morerows="1" id="1348" class="thentry" rowspan="2">[Mg]/[Si]</th><th colname="col2" morerows="1" id="1349" class="thentry" rowspan="2">Ionic strength (mol/L)</th><th colname="col3" namest="col3" nameend="col5" rowsep="1" id="1350" class="thentry" colspan="3">Saturation indices</th><th colname="col6" namest="col6" nameend="col8" rowsep="1" id="1351" class="thentry" colspan="3"><span id="1352" class="Dummy">M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub>‐S‐H precipitation rate (×10<sup xmlns="http://www.wiley.com/namespaces/wiley">−7</sup> mol/L/s)<span href="#jace70435-tbl3-note-0001" id="1355" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">a</sup></span></span></th><th colname="col9" namest="col9" nameend="col11" rowsep="1" id="1356" class="thentry" colspan="3"><span id="1357" class="Dummy">M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H precipitation rate (×10<sup xmlns="http://www.wiley.com/namespaces/wiley">−7</sup> mol/L/s)<span href="#jace70435-tbl3-note-0001" id="1360" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">a</sup></span></span></th></tr><tr rowsep="1" id="1361" xmlns=""><th colname="col3" id="1362" class="thentry">Brucite</th><th colname="col4" id="1363" class="thentry"><span id="1364" class="Dummy">M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub>‐S‐H</span></th><th colname="col5" id="1366" class="thentry"><span id="1367" class="Dummy">M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H</span></th><th colname="col6" id="1369" class="thentry">P1</th><th colname="col7" id="1370" class="thentry">P2</th><th colname="col8" id="1371" class="thentry">Total</th><th colname="col9" id="1372" class="thentry">P1</th><th colname="col10" id="1373" class="thentry">P2</th><th colname="col11" id="1374" class="thentry">Total</th></tr></thead><tbody><tr id="1375" xmlns=""><td colname="col1" id="1376" class="entry">1</td><td colname="col2" id="1377" class="entry">0.0053</td><td colname="col3" id="1378" class="entry">2.73</td><td colname="col4" id="1379" class="entry">5.97</td><td colname="col5" id="1380" class="entry">5.81</td><td colname="col6" id="1381" class="entry">9.72</td><td colname="col7" id="1382" class="entry">0.80</td><td colname="col8" id="1383" class="entry">10.52</td><td colname="col9" id="1384" class="entry">14.58</td><td colname="col10" id="1385" class="entry">1.28</td><td colname="col11" id="1386" class="entry">15.86</td></tr><tr id="1387" xmlns=""><td colname="col1" id="1388" class="entry">0.65</td><td colname="col2" id="1389" class="entry">0.0087</td><td colname="col3" id="1390" class="entry">2.73</td><td colname="col4" id="1391" class="entry">6.41</td><td colname="col5" id="1392" class="entry">6.03</td><td colname="col6" id="1393" class="entry">8.83</td><td colname="col7" id="1394" class="entry">1.64</td><td colname="col8" id="1395" class="entry">10.47</td><td colname="col9" id="1396" class="entry">13.24</td><td colname="col10" id="1397" class="entry">2.53</td><td colname="col11" id="1398" class="entry">15.77</td></tr><tr id="1399" xmlns=""><td colname="col1" id="1400" class="entry">0.385</td><td colname="col2" id="1401" class="entry">0.0201</td><td colname="col3" id="1402" class="entry">2.73</td><td colname="col4" id="1403" class="entry">6.86</td><td colname="col5" id="1404" class="entry">6.25</td><td colname="col6" id="1405" class="entry">6.79</td><td colname="col7" id="1406" class="entry">2.39</td><td colname="col8" id="1407" class="entry">9.19</td><td colname="col9" id="1408" class="entry">10.97</td><td colname="col10" id="1409" class="entry">3.73</td><td colname="col11" id="1410" class="entry">14.70</td></tr></tbody></table></div><div id="1411" class="noteGroup"><div xmlid="jace70435-tbl3-note-0001" id="1412" class="note"><label id="1413" xmlns="http://www.wiley.com/namespaces/wiley"><sup>a</sup></label><p id="1414" xmlns="http://www.wiley.com/namespaces/wiley"><span id="1415" class="Dummy" xmlns="">Calculated based on the assumption of the formation of either M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub>‐S‐H only or M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H only.</span></p></div></div></div><p id="1418"><span id="1419" class="Dummy" xmlns="">Notably, decreasing [Mg]/[Si] with respect to M‐S‐H resulted in both greater amounts of M‐S‐H belonging to Population 2 and smaller amounts for Population 1. The result is an overall slight reduction in rate that interestingly coincides with an increase in the supersaturation with respect to M‐S‐H (Table <span href="#jace70435-tbl-0003" id="1420" class="link">3</span>). Together with the results presented in Section <span href="#jace70435-sec-0080" id="1422" class="link">3.2.1</span>, these findings imply that the growth rate is controlled not only by the supersaturation but also by the Mg/Si ratio of the growing M‐S‐H phase.</span></p></section><section xmlid="jace70435-sec-0100" id="1424"><div type="main" id="1425" class="title" xmlns="">Influence of solid saturation index on M‐S‐H formation</div><p id="1426"><span id="1427" class="Dummy" xmlns="">Set 3 experiments were designed to evaluate whether the formation of a specific M‐S‐H phase can be precisely controlled by the relative saturation indices of three solid phases. In this set, the SI of the M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub>‐S‐H phase was held constant, while the [Mg]/[Si] ratio varied from 0.76 to 15. This led to increasing saturation indices for both brucite and M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H. Consequently, the precipitation rate increased as saturation increased (Figure <span href="#jace70435-fig-0005" id="1430" class="link">5A</span>, Table <span href="#jace70435-tbl-0004" id="1432" class="link">4</span>). Since precipitation may result from contributions of both M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub>‐S‐H or M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H, considering only M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H formation could lead to an overestimation of the precipitation rate due to its lower density. Nonetheless, the best‐fit rate equation, based on precipitation rates measured at 76 min of reaction, is: </span><i iamnewelement="True" class="fa fa-eye d-none" aria-hidden="true" xmlns=""></i><math xmlns="" display="inline" altimg="urn:x-wiley:00027820:media:jace70435:jace70435-math-0016" p7:location="equation/jace70435-math-0016.png" xmlns:p7="http://www.wiley.com/namespaces/wiley/wiley" class="math" id="1437"><semantics xmlns=""><mrow><msub><mi>r</mi><mrow><msub><mi mathvariant="normal">M</mi><mn>1.50</mn></msub><mo>−</mo><mi mathvariant="normal">S</mi><mo>−</mo><mi mathvariant="normal">H</mi></mrow></msub><mo>=</mo><msup><mn>10</mn><mrow><mo>−</mo><mn>8.45</mn><mo>±</mo><mn>0.25</mn></mrow></msup><mrow><mo stretchy="false">(</mo><mrow><msup><mi mathvariant="normal">Ω</mi><mrow><mn>0.32</mn><mo>±</mo><mn>0.03</mn></mrow></msup><mo>−</mo><mn>1</mn></mrow><mo stretchy="false">)</mo></mrow></mrow><annotation encoding="application/x-tex">${r_{{{\mathrm{M}}_{1.50}} - {\mathrm{S}} - {\mathrm{H}}}} = {10^{ - 8.45 \pm 0.25}} ( {{\Omega ^{0.32 \pm 0.03}} - 1} )$</annotation></semantics></math><span id="1471" class="Dummy" xmlns=""> mol/L/s with a root mean square error of 8.12 × 10<sup xmlns="http://www.wiley.com/namespaces/wiley">−8</sup> mol/L/s (Figure <span href="#jace70435-fig-0005" id="1473" class="link">5A</span>).</span></p><figure xmlid="jace70435-fig-0005" draggable="false"><div id="1477" class="mediaResourceGroup" xmlns="" draggable="false"><img mimetype="image/png" rendition="webOriginal" alt="image" id="1480" class="mediaResource e-rte-image e-imginline tooltipobj" originalsrc="image_n/jace70435-fig-0005.png" src="https://arpasset1.pubmate.in/JACE_EV_JACE70435_fcc841d596c24ac1aa3ecacc8800bb99/ProofLink/image_n/jace70435-fig-0005.png" srchires="https://arpasset1.pubmate.in/JACE_EV_JACE70435_fcc841d596c24ac1aa3ecacc8800bb99/ProofLink/image_m/jace70435-fig-0005-m.png" originalsrchires="image_m/jace70435-fig-0005-m.png" iamrelocated="True" /></div><div type="figureName" id="1476" class="title" xmlns="">FIGURE<label id="1475" iamrelocated="True" xmlns="http://www.wiley.com/namespaces/wiley">5</label><span id="1482" class="caption" xmlns="" iamrelocated="True"><span id="1483" class="Dummy">(A) Precipitation rate as a function of M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H ratio for Set 3 experiments, assuming the formation of M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>SH. Mean particle size as a function of [Mg]/[Si] ratio of the M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H phase for Set 1 and Set 3 experiments for (B) Population 1 and (C) Population 2. A dashed curve is provided in (C) as a visual guide.</span></span></div></figure><div xmlid="jace70435-tbl-0004" prights="unknown" erights="yes" copyright="John Wiley & Sons, Ltd." id="1487" class="tabular" xmlns=""><span iamplaceholderforid="1488"></span><div id="1489" class="titleGroup"><div type="tabularName" id="1490" class="title">TABLE<label id="1488" xmlns="http://www.wiley.com/namespaces/wiley" iamrelocated="True">4</label><span type="main" id="1491" class="title" iamrelocated="True"><span id="1492" class="Dummy">M‐S‐H precipitation rates from Set 3 experiments, conducted with constant M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub>‐S‐H SI with varying brucite and M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H SI, measured at a reaction time of 76 min.</span></span></div><span iamplaceholderforid="1491"></span></div><span iamplaceholderforid="1583"></span><div iamnewelement="True" class="TableOverFlow"><tgroup cols="11"><colspec colnum="1" colname="col1" align="left" id="1495" class="colspec" xmlns=""></colspec><colspec colnum="2" colname="col2" align="left" id="1496" class="colspec" xmlns=""></colspec><colspec colnum="3" colname="col3" align="left" id="1497" class="colspec" xmlns=""></colspec><colspec colnum="4" colname="col4" align="left" id="1498" class="colspec" xmlns=""></colspec><colspec colnum="5" colname="col5" align="left" id="1499" class="colspec" xmlns=""></colspec><colspec colnum="6" colname="col6" align="left" id="1500" class="colspec" xmlns=""></colspec><colspec colnum="7" colname="col7" align="left" id="1501" class="colspec" xmlns=""></colspec><colspec colnum="8" colname="col8" align="left" id="1502" class="colspec" xmlns=""></colspec><colspec colnum="9" colname="col9" align="left" id="1503" class="colspec" xmlns=""></colspec><colspec colnum="10" colname="col10" align="left" id="1504" class="colspec" xmlns=""></colspec><colspec colnum="11" colname="col11" align="left" id="1505" class="colspec" xmlns=""></colspec></tgroup><table frame="topbot" xmlns="http://www.wiley.com/namespaces/wiley"><thead><tr id="1506" xmlns=""><th colname="col1" morerows="1" id="1507" class="thentry" rowspan="2">[Mg]/[Si]</th><th colname="col2" namest="col2" nameend="col4" rowsep="1" id="1508" class="thentry" colspan="3">Saturation Indices</th><th colname="col5" namest="col5" nameend="col6" rowsep="1" id="1509" class="thentry" colspan="2"><span id="1510" class="Dummy">Volume fraction (×10<sup xmlns="http://www.wiley.com/namespaces/wiley">−5</sup>)<span href="#jace70435-tbl4-note-0001" id="1512" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">a</sup></span></span></th><th colname="col7" namest="col7" nameend="col8" rowsep="1" id="1513" class="thentry" colspan="2"><span id="1514" class="Dummy">Mean size (Å)<span href="#jace70435-tbl4-note-0001" id="1515" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">a</sup></span></span></th><th colname="col9" namest="col9" nameend="col11" rowsep="1" id="1516" class="thentry" colspan="3"><span id="1517" class="Dummy">Precipitation Rate (×10<sup xmlns="http://www.wiley.com/namespaces/wiley">−7</sup> mol/L/s)<span href="#jace70435-tbl4-note-0001" id="1519" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">a</sup></span></span></th></tr><tr rowsep="1" id="1520" xmlns=""><th colname="col2" id="1521" class="thentry">Brucite</th><th colname="col3" id="1522" class="thentry"><span id="1523" class="Dummy">M<sub xmlns="http://www.wiley.com/namespaces/wiley">0.75</sub>‐S‐H</span></th><th colname="col4" id="1525" class="thentry"><span id="1526" class="Dummy">M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H</span></th><th colname="col5" id="1528" class="thentry">P1</th><th colname="col6" id="1529" class="thentry">P2</th><th colname="col7" id="1530" class="thentry">P1</th><th colname="col8" id="1531" class="thentry">P2</th><th colname="col9" id="1532" class="thentry">P1</th><th colname="col10" id="1533" class="thentry">P2</th><th colname="col11" id="1534" class="thentry">Total</th></tr></thead><tbody><tr id="1535" xmlns=""><td colname="col1" id="1536" class="entry">0.76</td><td colname="col2" id="1537" class="entry">2.49</td><td colname="col3" id="1538" class="entry">5.97</td><td colname="col4" id="1539" class="entry">5.63</td><td colname="col5" id="1540" class="entry">3.60</td><td colname="col6" id="1541" class="entry">1.82</td><td colname="col7" id="1542" class="entry">7.25</td><td colname="col8" id="1543" class="entry">372.12</td><td colname="col9" id="1544" class="entry">0.53</td><td colname="col10" id="1545" class="entry">0.27</td><td colname="col11" id="1546" class="entry">0.80</td></tr><tr id="1547" xmlns=""><td colname="col1" id="1548" class="entry">1.00</td><td colname="col2" id="1549" class="entry">2.73</td><td colname="col3" id="1550" class="entry">5.97</td><td colname="col4" id="1551" class="entry">5.81</td><td colname="col5" id="1552" class="entry">17.11</td><td colname="col6" id="1553" class="entry">4.36</td><td colname="col7" id="1554" class="entry">4.12</td><td colname="col8" id="1555" class="entry">423.79</td><td colname="col9" id="1556" class="entry">2.52</td><td colname="col10" id="1557" class="entry">0.77</td><td colname="col11" id="1558" class="entry">3.30</td></tr><tr id="1559" xmlns=""><td colname="col1" id="1560" class="entry">1.75</td><td colname="col2" id="1561" class="entry">3.52</td><td colname="col3" id="1562" class="entry">5.97</td><td colname="col4" id="1563" class="entry">6.40</td><td colname="col5" id="1564" class="entry">21.96</td><td colname="col6" id="1565" class="entry">6.12</td><td colname="col7" id="1566" class="entry">3.15</td><td colname="col8" id="1567" class="entry">277.68</td><td colname="col9" id="1568" class="entry">3.24</td><td colname="col10" id="1569" class="entry">0.90</td><td colname="col11" id="1570" class="entry">4.14</td></tr><tr id="1571" xmlns=""><td colname="col1" id="1572" class="entry">15</td><td colname="col2" id="1573" class="entry">7.25</td><td colname="col3" id="1574" class="entry">5.97</td><td colname="col4" id="1575" class="entry">9.19</td><td colname="col5" id="1576" class="entry">152.09</td><td colname="col6" id="1577" class="entry">50.99</td><td colname="col7" id="1578" class="entry">5.46</td><td colname="col8" id="1579" class="entry">98.87</td><td colname="col9" id="1580" class="entry">22.45</td><td colname="col10" id="1581" class="entry">7.53</td><td colname="col11" id="1582" class="entry">29.97</td></tr></tbody></table></div><div id="1583" class="noteGroup"><div xmlid="jace70435-tbl4-note-0001" id="1584" class="note"><label id="1585" xmlns="http://www.wiley.com/namespaces/wiley"><sup>a</sup></label><p id="1586" xmlns="http://www.wiley.com/namespaces/wiley"><span id="1587" class="Dummy" xmlns="">Calculated based on the assumption of the formation of M<sub xmlns="http://www.wiley.com/namespaces/wiley">1.50</sub>‐S‐H only.</span></p></div></div></div><p id="1589"><span id="1590" class="Dummy" xmlns="">The average particle size from Population 1 (5.38 Å) was slightly smaller than the size of the basic building blocks (average radius of 17 Å) of M‐S‐H reported previously.<span href="#jace70435-bib-0025" id="1591" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">25</sup></span> While there was no observed trend in mean size vs [Mg]/[Si] for Population 1 (Figure <span href="#jace70435-fig-0005" id="1593" class="link">5B</span>), the mean size of Population 2 initially increased and then decreased once the ratio exceeded 1.75 (Figure <span href="#jace70435-fig-0005" id="1595" class="link">5C</span>). Meanwhile, the volume fraction continued to rise, suggesting a greater total extent of precipitation as the mean size decreased. When combined with findings from the Set 1 experiments, these results indicate <ins user="Erika La Plante" title="Erika La Plante inserted content on: 10 Dec, 05:47 PM" class="new" updatedon="10 Dec, 05:47 PM" mytype="content" id="c95125c9-3fa7-4ea3-a122-58879be15791">that </ins>the <ins user="Erika La Plante" title="Erika La Plante inserted content on: 10 Dec, 05:47 PM" class="new" updatedon="10 Dec, 05:47 PM" mytype="content" id="d6f638a5-c687-4d18-95eb-70848c830c77">highest</ins><del user="Erika La Plante" title="Erika La Plante deleted content on: 10 Dec, 05:46 PM" class="old" updatedon="10 Dec, 05:46 PM" mytype="content" id="f30e7b1c-c99c-4ffc-9664-8062be568544">presence of an optimal </del>mean particle size<ins user="Erika La Plante" title="Erika La Plante inserted content on: 10 Dec, 05:47 PM" class="new" updatedon="10 Dec, 05:47 PM" mytype="content" id="726b6541-615e-4313-aa76-207495916f0c"> is obtained</ins> when magnesium and silicon concentrations are approximately equal (Figure <span href="#jace70435-fig-0005" id="1597" class="link">5C</span>). This trend can be attributed to a balance between nucleation and growth rates, with maximum growth and minimal nucleation occurring when [Mg] ≈ [Si], analogous to previous observations on calcite (CaCO<sub xmlns="http://www.wiley.com/namespaces/wiley">3</sub>).<span href="#jace70435-bib-0056 #jace70435-bib-0057" id="1600" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">56,57</sup></span> The data also imply that an excess of either magnesium or silicon reduces the efficiency of silicate oligomerization, limiting effective particle growth.</span></p></section></section>
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<section xmlid="jace70435-sec-0110" id="1602">
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<div type="main" id="1603" class="title" xmlns="">Implications for cementitious application</div>
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<p id="1604"><span id="1605" class="Dummy" xmlns="">These findings apply to systems in which M‐S‐H directly precipitates from an initially supersaturated solution. In the practical application of cements and concrete, the influence of impurity ions should be taken into consideration, as they can influence the nucleation and growth of M‐S‐H. For instance, in C‐S‐H, the presence of chloride, sulfate, alkali, or carbonate ions, which are commonly found in concrete pore solutions, has been shown to alter solution pH, C‐S‐H chemical composition, phase assemblage, and mechanical properties.<span href="#jace70435-bib-0058" id="1606" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">58</sup></span> For M‐S‐H, previous studies have shown that the incorporation of citrate anion into M‐S‐H might delay nucleation and growth, thereby influencing the rate of strength development in concrete.<span href="#jace70435-bib-0059" id="1608" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">59</sup></span> Moreover, as discussed above, silicate oligomerization can be influenced by solution pH,<span href="#jace70435-bib-0055" id="1610" class="link"><sup xmlns="http://www.wiley.com/namespaces/wiley">55</sup></span> suggesting the possibility of using additives to regulate particle size and therefore, microstructure of a cementitious M‐S‐H binder.</span></p>
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</section>
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</section>
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<section xmlid="jace70435-sec-0120" id="1612" xmlns="http://www.wiley.com/namespaces/wiley">
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<div type="main" id="1613" class="title" xmlns="">CONCLUSION</div>
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<p id="1614"><span id="1615" class="Dummy" xmlns="">In this study, M‐S‐H was synthesized without the formation of other phases using a solution‐based method. For the first time, M‐S‐H precipitation rates were quantified based exclusively on solid‐phase properties using synchrotron‐based SAXS. SAXS results reveal that the M‐S‐H structure is composed of two particle populations: Ångström‐scale spherical building blocks of M‐S‐H and nanoscale M‐S‐H aggregates. The precipitation rates ranged from 10<sup xmlns="http://www.wiley.com/namespaces/wiley">−7</sup> to 10<sup xmlns="http://www.wiley.com/namespaces/wiley">−5</sup> mol/L/s, depending on the initial SI. In comparison to C‐S‐H, M‐S‐H precipitates more slowly under equivalent saturation conditions, which could translate to a slower rate of strength gain. The precipitation rate laws derived here can be used to model cement hydration and microstructure, thereby predicting the time evolution of macroscopic properties</span></p>
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<p id="1618">SAXS analysis further revealed that variations in the [Mg]/[Si] ratio significantly impact particle size distribution. While the supersaturation remains a useful parameter, the results show that it cannot fully predict phase growth behavior on its own. This emphasizes the need to consider other influencing factors, particularly those related to nucleation and growth, such as the [Mg]/[Si] ratio, impurities and additives, and solution pH. Importantly, this finding presents an opportunity to tailor M‐S‐H particle sizes for specific applications. Given that particle size distribution and growth rates are critical factors influencing hydration and early‐age performance of cementitious materials, it is essential to understand and control these parameters.</p>
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</section>
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<section xmlid="jace70435-sec-0130" type="acknowledgments" numbered="no" id="1619" xmlns="http://www.wiley.com/namespaces/wiley">
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<div type="main" id="1620" class="title" xmlns="">ACKNOWLEDGMENTS</div>
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<p id="1621" xmlns="">The authors thank Jan Ilavsky at the Advanced Photon Source for valuable insights into data analysis. The authors gratefully acknowledge the financial support provided by the National Science Foundation through the CAREER Award #2342381. This work was conducted at the Materials Chemistry Laboratory (MCL) and the Peter A. Rock Thermochemistry Laboratory at the University of California, Davis. The authors express their appreciation for the support that has facilitated the operations of these laboratories. Efforts in X‐ray data analysis and interpretation by SSL were funded by the Department of Energy (DOE), Office of Science, Office of Basic Energy Sciences, Geosciences program (FWP# 57814) under Contract DE‐AC02‐06CH11357 to UChicago Argonne, LLC as operator of Argonne National Laboratory (ANL). <del user="Erika La Plante" title="Erika La Plante deleted content on: 10 Dec, 05:49 PM" class="old" updatedon="10 Dec, 05:49 PM" mytype="content" id="65fe6769-d7ed-4372-b81a-20b23ab0def8">SAXS measurements were conducted at Beamline 12‐ID‐B at the Advanced Photon Source (APS), ANL. </del>This research <ins user="Erika La Plante" title="Erika La Plante inserted content on: 10 Dec, 03:28 PM" class="new" updatedon="10 Dec, 03:28 PM" mytype="content" id="8fd16cfb-06d3-4cd6-86d5-053e1ea8cd49">was performed on APS beam time award (DOI: https://doi.org/10.46936/APS-183830/60011635) from the Advanced Photon Source, </ins><del user="Erika La Plante" title="Erika La Plante deleted content on: 10 Dec, 03:32 PM" class="old" updatedon="10 Dec, 03:32 PM" mytype="content" id="8c4fd766-1920-4888-861e-b3bdb984586a">used resources of APS, </del>a U.S. <ins user="Erika La Plante" title="Erika La Plante inserted content on: 10 Dec, 03:32 PM" class="new" updatedon="10 Dec, 03:32 PM" mytype="content" id="630d06f8-2a90-474a-b729-1635396f17ca">Department of Energy (</ins>DOE<ins user="Erika La Plante" title="Erika La Plante inserted content on: 10 Dec, 03:32 PM" class="new" updatedon="10 Dec, 03:32 PM" mytype="content" id="42661c40-0083-4a20-b623-36d5eb3194fd">)</ins> Office of Science <ins user="Erika La Plante" title="Erika La Plante inserted content on: 10 Dec, 03:32 PM" class="new" updatedon="10 Dec, 03:32 PM" mytype="content" id="f6f705f0-d306-4cd4-99fa-406f7ec733e3">u</ins><del user="Erika La Plante" title="Erika La Plante deleted content on: 10 Dec, 03:32 PM" class="old" updatedon="10 Dec, 03:32 PM" mytype="content" id="c0b52964-080e-430c-8672-db022f1df71f">U</del>ser <ins user="Erika La Plante" title="Erika La Plante inserted content on: 10 Dec, 03:32 PM" class="new" updatedon="10 Dec, 03:32 PM" mytype="content" id="c5d4edb4-70f0-4264-b061-7262fb6998b5">f</ins><del user="Erika La Plante" title="Erika La Plante deleted content on: 10 Dec, 03:32 PM" class="old" updatedon="10 Dec, 03:32 PM" mytype="content" id="155580d7-3d40-414b-a1ab-2d705870cbce">F</del>acility operated for the DOE Office of Science by <ins user="Erika La Plante" title="Erika La Plante inserted content on: 10 Dec, 03:32 PM" class="new" updatedon="10 Dec, 03:32 PM" mytype="content" id="2d032fde-6b9b-4f7a-96d8-3cae28377d29">Argonne National Laboratory</ins><del user="Erika La Plante" title="Erika La Plante deleted content on: 10 Dec, 03:32 PM" class="old" updatedon="10 Dec, 03:32 PM" mytype="content" id="a4e69db0-4066-4b72-918c-0fda1a17c0be">ANL</del> under Contract DE‐AC02‐06CH11357. The contents of this paper represent the views and opinions of the authors, who are responsible for the accuracy of the datasets presented herein. They do not reflect the views and/or policies of the funding agency, nor do the contents constitute a specification, standard, or regulation.</p>
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</section>
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<div xmlid="jace70435-supinfo-0001" id="157" class="supportingInformation" iamrelocated="True">
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<div xmlid="jace70435-supitem-0001" id="158" class="supportingInfoItem">
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<img href="https://arpasset1.pubmate.in/JACE_EV_JACE70435_fcc841d596c24ac1aa3ecacc8800bb99/ProofLink/supinfo/jace70435-sup-0001-SuppMat.pdf" alt="supplementary_material" rendition="webOriginal" id="159" class="mediaResource" originalsrc="supinfo/jace70435-sup-0001-SuppMat.pdf" src="https://arpasset1.pubmate.in/JACE_EV_JACE70435_fcc841d596c24ac1aa3ecacc8800bb99/ProofLink/supinfo/jace70435-sup-0001-SuppMat.pdf" srcHiRes=""></img>
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<span id="160" class="caption">Supporting Information</span>
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</div>
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</div><div xmlid="jace70435-bibl-0001" style="numbered" id="1622" class="bibliography">
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<div type="main" id="1623" class="title">REFERENCES</div>
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