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    <completedYear/>
    <publishedYear>2023</publishedYear>
    <thesisYearAccepted/>
    <language>eng</language>
    <pageFirst>4333</pageFirst>
    <pageLast>4344</pageLast>
    <pageNumber/>
    <edition/>
    <issue>30</issue>
    <volume>25</volume>
    <type>article</type>
    <publisherName>CrystEngComm</publisherName>
    <publisherPlace>London</publisherPlace>
    <creatingCorporation/>
    <contributingCorporation/>
    <belongsToBibliography>1</belongsToBibliography>
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    <publishedDate>--</publishedDate>
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    <title language="eng">Phase stability studies on transition metal phosphates aided by an automated synthesis</title>
    <abstract language="eng">Transition metal phosphates (TMPs) have attracted interest as materials for (electro-) catalysis, and electrochemistry due to their low-cost, stability, and tunability. In this work, an automated synthesis platform was used for the preparation of transition metal phosphate crystals to efficiently explore the multidimensional parameter space, determining the phase selection, crystal sizes, shapes. By using X-ray diffraction and spectroscopy-based methods and electron microscopy imaging, a complete characterization of the phase stability fields, phase transitions, and crystal morphology/sizes was achieved. In an automated three-reactant synthesis, the individual effect of each reactant species NH4+, M2+, and PO43- on the formation of transition metal phosphate phases: M-struvite NH4MPO4·6H2O, M-phosphate octahydrate M3(PO4)2·8H2O with M = Ni, Co and an amorphous phase, was investigated. The NH4+ concentration dictates the phase composition, morphology, and particle size in the Ni-system (crystalline Ni-struvite versus amorphous Ni-PO4 phase), whereas in the Co-system all reactant species - NH4+, Co2+, and PO43- - influence the reaction outcome equivalently (Co-struvite vs. Co-phosphate octahydrate). The coordination environment for all crystalline compounds and of the amorphous Ni-PO4 phase was resolved by X-ray absorption spectroscopy, revealing matching characteristics to its crystalline analogue, Ni3(PO4)2·8H2O. The automated synthesis turned out to be significantly advantageous for the exploration of phase diagrams due to its simple modularity, facile traceability, and enhanced reproducibility compared to a typical manual synthesis.</abstract>
    <parentTitle language="eng">Royal Society of Chemistry (RSC)</parentTitle>
    <identifier type="doi">10.1039/D3CE00386H</identifier>
    <identifier type="urn">urn:nbn:de:kobv:b43-579151</identifier>
    <enrichment key="opus.source">publish</enrichment>
    <enrichment key="date_peer_review">07.08.2023</enrichment>
    <licence>Creative Commons - CC BY - Namensnennung 4.0 International</licence>
    <author>Stephanos Karafiludis</author>
    <author>T. W. Ryll</author>
    <author>Ana de Oliveira Guilherme Buzanich</author>
    <author>Franziska Emmerling</author>
    <author>Tomasz Maciej Stawski</author>
    <subject>
      <language>eng</language>
      <type>uncontrolled</type>
      <value>Automated synthesis</value>
    </subject>
    <subject>
      <language>eng</language>
      <type>uncontrolled</type>
      <value>Phase diagrams</value>
    </subject>
    <subject>
      <language>eng</language>
      <type>uncontrolled</type>
      <value>Transition metals</value>
    </subject>
    <subject>
      <language>eng</language>
      <type>uncontrolled</type>
      <value>Phosphates</value>
    </subject>
    <subject>
      <language>eng</language>
      <type>uncontrolled</type>
      <value>Local structure</value>
    </subject>
    <subject>
      <language>eng</language>
      <type>uncontrolled</type>
      <value>Struvite</value>
    </subject>
    <collection role="ddc" number="620">Ingenieurwissenschaften und zugeordnete Tätigkeiten</collection>
    <collection role="institutes" number="">6 Materialchemie</collection>
    <collection role="institutes" number="">6.3 Strukturanalytik</collection>
    <collection role="themenfelder" number="">Material</collection>
    <collection role="literaturgattung" number="">Verlagsliteratur</collection>
    <collection role="fulltextaccess" number="">Datei für die Öffentlichkeit verfügbar ("Open Access")</collection>
    <collection role="unnumberedseries" number="">Wissenschaftliche Artikel der BAM</collection>
    <collection role="themenfelder" number="">Materialdesign</collection>
    <thesisPublisher>Bundesanstalt für Materialforschung und -prüfung (BAM)</thesisPublisher>
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  <doc>
    <id>59135</id>
    <completedYear/>
    <publishedYear>2023</publishedYear>
    <thesisYearAccepted/>
    <language>eng</language>
    <pageFirst>10645</pageFirst>
    <pageLast>10657</pageLast>
    <pageNumber/>
    <edition/>
    <issue>24</issue>
    <volume>35</volume>
    <type>article</type>
    <publisherName>American Chemical Society (ACS)</publisherName>
    <publisherPlace>Washington D.C.</publisherPlace>
    <creatingCorporation/>
    <contributingCorporation/>
    <belongsToBibliography>1</belongsToBibliography>
    <completedDate>--</completedDate>
    <publishedDate>--</publishedDate>
    <thesisDateAccepted>--</thesisDateAccepted>
    <title language="eng">Nonclassical Crystallization Pathway of Transition Metal Phosphate Compounds</title>
    <abstract language="eng">Here, we elucidate nonclassical multistep crystallization pathways of transition metal phosphates from aqueous solutions. We followed precipitation processes of M-struvites, NH4MPO4·6H2O, and M-phosphate octahydrates, M3(PO4)2·8H2O, where M = Ni, Co, or NixCo1–x, by using in situ scattering and spectroscopy-based techniques, supported by elemental mass spectrometry analyses and advanced electron microscopy. Ni and Co phosphates crystallize via intermediate colloidal amorphous nanophases, which change their complex structures while agglomerating, condensing, and densifying throughout the extended reaction times. We reconstructed the three-dimensional morphology of these precursors by employing cryo-electron tomography (cryo-ET). We found that the complex interplay between metastable amorphous colloids and protocrystalline units determines the reaction pathways. Ultimately, the same crystalline structure, such as struvite, is formed. However, the multistep process stages vary in complexity and can last from a few minutes to several hours depending on the selected transition metal(s), their concentration, and the Ni/Co ratio.</abstract>
    <parentTitle language="eng">Chemistry of Materials</parentTitle>
    <identifier type="doi">10.1021/acs.chemmater.3c02346</identifier>
    <identifier type="issn">1520-5002</identifier>
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    <author>Stephanos Karafiludis</author>
    <author>Z. Kochovski</author>
    <author>E. Scoppola</author>
    <author>Anika Retzmann</author>
    <author>Vasile-Dan Hodoroaba</author>
    <author>J. E. ten Elshof</author>
    <author>Franziska Emmerling</author>
    <author>Tomasz Maciej Stawski</author>
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      <value>Non-classical crystallization theory</value>
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      <language>eng</language>
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      <value>Transition metals</value>
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      <type>uncontrolled</type>
      <value>Phosphates</value>
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    <subject>
      <language>eng</language>
      <type>uncontrolled</type>
      <value>Amorphous phases</value>
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      <language>eng</language>
      <type>uncontrolled</type>
      <value>Intermediate phases</value>
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