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    <title language="eng">Robocasting of ordered mesoporous silica‐based monoliths: Rheological, textural, and mechanical characterization</title>
    <abstract language="eng">Hierarchically porous, high‐surface‐area silica materials are excellent candidates for multiple applications like catalysis and environmental remediation. Shaping these materials with additive manufacturing (AM) techniques, like robocasting, could enable their use with the benefit of on‐demand, customized shaping and maximizing performance. Herein, ordered mesoporous silica COK‐12 slurries were robocasted into monoliths, containing different ratios of uncalcined COK‐12 and sodium bentonite (0–25 wt.%). The rheology of the mixed slurries is characterized by lower flow indexes (0.69 vs. 0.32) and higher yield stresses (96 vs. 259 Pa) compared to pure COK‐12 ones. Monoliths were printed in woodpile structures and calcined at 600°C. Micro‐CT measurements showed a linear shrinkage of 25% after calcination. Mechanical characterization showed increased uniaxial strength (0.20 ± 0.07 to 1.0 ± 0.3 MPa) with increasing binder/solids ratio from 13 to 25%. The amorphous, mesoporous structure of COK‐12 was retained. The structures exhibited open porosities of 52 ± 4% and showed higher specific mesopore volumes, and increased average mesopore size (6 vs. 8 nm) compared to COK‐12. Small‐angle x‐ray scattering analysis revealed an increased lattice parameter (10.3 vs. 11.0 nm) and reduced wall thickness (3.1 nm vs. 4.1 nm) of the COK‐12 in the monoliths. These properties indicate suitability for their application as porous supports and adsorbents.</abstract>
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Shaping these materials with additive manufacturing (AM) techniques, like robocasting, could enable their use with the benefit of on\u2010demand, customized shaping and maximizing performance. Herein, ordered mesoporous silica COK\u201012 slurries were robocasted into monoliths, containing different ratios of uncalcined COK\u201012 and sodium bentonite (0\u201325\u00a0wt.%). The rheology of the mixed slurries is characterized by lower flow indexes (0.69\u00a0vs. 0.32) and higher yield stresses (96\u00a0vs. 259\u00a0Pa) compared to pure COK\u201012 ones. Monoliths were printed in woodpile structures and calcined at 600\u00b0C. Micro\u2010CT measurements showed a linear shrinkage of 25% after calcination. Mechanical characterization showed increased uniaxial strength (0.20\u00a0\u00b1\u00a00.07 to 1.0\u00a0\u00b1\u00a00.3\u00a0MPa) with increasing binder\/solids ratio from 13 to 25%. The amorphous, mesoporous structure of COK\u201012 was retained. 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    <author>E. S. Dal Molin</author>
    <author>L. M. Henning</author>
    <author>J. T. Müller</author>
    <author>Glen Jacob Smales</author>
    <author>Brian Richard Pauw</author>
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      <value>Porous materials</value>
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      <value>Robocasting</value>
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      <value>X-ray scattering</value>
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    <title language="eng">Synthesis and properties of COK-12 large-pore mesocellularsilica foam</title>
    <abstract language="eng">Large, ink-bottle-shaped pores in mesocellular foams (MCFs) are desired for various applications requiring enhanced mass transfer or the immobilization of larger compounds. Hence, the cylindrical pores of COK-12, an ordered mesoporous silica structurally comparable to SBA-15 but synthesized at room-temperature at quasi-neutral pH, are chemically swollen into ink-bottle pores. Therefore, p-xylene is used as a more sustainable swelling agent compared to popular alternatives. Its high boiling point allows for an additional thermal aging step to amplify the mesostructure enlargement without needing additional chemicals. For COK-12, the MCFs obtained at room temperature reach an unprecedented plateau for the modal mesopore cell and window diameter of 19.9 and 5.5 nm, respectively, with an underlying broad pore size distribution and distorted hexagonal lattice up to 14.5 nm, involving hexagonal and spherical structures. The combined chemical and thermal swelling resulted in the selective enlargement of the window diameter to more than 200% and a slightly increased cell diameter, pore size distribution, and hexagonal lattice distortion in comparison to the room temperature synthesis. Such materials are thought to be promising alternatives to SBA-15-based MCFs, often utilizing toxic catalysts during synthesis. The presented results pave the way for enhanced adsorptive, catalytic, and drug delivery performances for COK-12-based materials.</abstract>
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    <author>L. M. Henning</author>
    <author>Glen Jacob Smales</author>
    <author>M. G. Colmenares</author>
    <author>M. F. Bekheet</author>
    <author>U. Simon</author>
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    <title language="eng">Grafting and stabilization of ordered mesoporous silica COK-12 with graphene oxide for enhanced removal of methylene blue</title>
    <abstract language="eng">Large-pore ordered mesoporous silica (OMS) COK-12, analogous to the well-known SBA-15, but synthesized in a more environmentally friendly way and exhibiting a shorter plate-like structure, was grafted with different amounts of graphene oxide (GO) for the first time in an inexpensive and rapid process, that was successfully upscaled. Samples were examined with nitrogen sorption analysis, SAXS, Raman spectroscopy, XPS, and zeta potential analysis. Adsorption experiments with the cationic dye methylene blue (MB) were conducted on the grafted materials and on pure COK-12, taking into account the influence of initial dye concentration (30–600 mg L-1), adsorbent dosage (0.2–14 g L-1), contact time (0.3–300 min), solution pH (4 10), and influence of salts and temperature (0–1 M NaCl, 80 C) to simulate industrial dye effluent. The adsorption process was found to be represented best by the Langmuir isotherm model, i.e., adsorption is a monolayer process. The calculated maximum Adsorption capacities were found to be 20.2 and 197.5 mg g-1 at dosages of 5 and 0.5 g L-1 for pure COK-12 and COK-12 grafted with 50 wt% GO, respectively, at pH 5.65 and MB concentration of 100 mg L-1.&#13;
Adsorption kinetics were found to follow the pseudo-second order model, i.e., chemisorption is the rate controlling step. The adsorption performances could be well preserved at simulated dye effluent.&#13;
Desorption was found to be most effective with hydrochloric acid. The COK-12 grafted with GO presented in this work shows superior adsorption properties in comparison to other grafted OMS materials. In addition, grafting with GO remarkably improved the stability of COK-12 in aqueous solution.</abstract>
    <parentTitle language="eng">RSC Advances</parentTitle>
    <identifier type="doi">10.1039/c9ra05541j</identifier>
    <identifier type="url">https://pubs.rsc.org/en/content/articlehtml/2019/ra/c9ra05541j</identifier>
    <identifier type="urn">urn:nbn:de:kobv:b43-497788</identifier>
    <enrichment key="date_peer_review">05.12.2019</enrichment>
    <licence>Creative Commons - CC BY - Namensnennung 4.0 International</licence>
    <author>L. M. Henning</author>
    <author>U. Simon</author>
    <author>A. Gurlo</author>
    <author>Glen Jacob Smales</author>
    <author>M. F. Bekheet</author>
    <subject>
      <language>eng</language>
      <type>uncontrolled</type>
      <value>COK-12</value>
    </subject>
    <subject>
      <language>eng</language>
      <type>uncontrolled</type>
      <value>Mesoporous Silica</value>
    </subject>
    <subject>
      <language>eng</language>
      <type>uncontrolled</type>
      <value>Graphene Oxide</value>
    </subject>
    <subject>
      <language>eng</language>
      <type>uncontrolled</type>
      <value>Large-pore</value>
    </subject>
    <collection role="ddc" number="620">Ingenieurwissenschaften und zugeordnete Tätigkeiten</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>
    <thesisPublisher>Bundesanstalt für Materialforschung und -prüfung (BAM)</thesisPublisher>
    <file>https://opus4.kobv.de/opus4-bam/files/49778/006_Henning_Grafting_and_stabilization_of_ordered_mesoporous_silica_COK-12.pdf</file>
  </doc>
  <doc>
    <id>55592</id>
    <completedYear/>
    <publishedYear>2022</publishedYear>
    <thesisYearAccepted/>
    <language>eng</language>
    <pageFirst>1</pageFirst>
    <pageLast>17</pageLast>
    <pageNumber/>
    <edition/>
    <issue/>
    <volume/>
    <type>article</type>
    <publisherName>Royal Society of Chemistry</publisherName>
    <publisherPlace>Cambridge</publisherPlace>
    <creatingCorporation/>
    <contributingCorporation/>
    <belongsToBibliography>1</belongsToBibliography>
    <completedDate>--</completedDate>
    <publishedDate>--</publishedDate>
    <thesisDateAccepted>--</thesisDateAccepted>
    <title language="eng">Hierarchically porous and mechanically stable monoliths from ordered mesoporous silica and their water filtration potential</title>
    <abstract language="eng">Mechanically stable structures with interconnected hierarchical porosity combine the benefits of both small&#13;
and large pores, such as high surface area, pore volume, and good mass transport capabilities. Hence, lightweight micro-/meso-/macroporous monoliths are prepared from ordered mesoporous silica COK-12 by means of spark plasma sintering (SPS, S-sintering) and compared to conventionally (C-) sintered monoliths. A multi-scale model is developed to fit the small angle X-ray scattering data and obtain information on the hexagonal lattice parameters, pore sizes from the macro to the micro range, as well as the dimensions of the silica population. For both sintering techniques, the overall mesoporosity, hexagonal pore ordering, and amorphous character are preserved. The monoliths' porosity (77–49%), mesopore size (6.2–5.2 nm), pore volume (0.50–0.22 g cm-3&#13;
), and specific surface area (451–180 m2 g-1) decrease with increasing processing temperature and pressure. While the difference in porosity is enhanced, the&#13;
structural parameters between the C-and S-sintered monoliths are largely converging at 900 C, except for the mesopore size and lattice parameter, whose dimensions are more extensively preserved in the&#13;
S-sintered monoliths, however, coming along with larger deviations from the theoretical lattice. Their higher mechanical properties (biaxial strength up to 49 MPa, 724 MPa HV 9.807 N) at comparable porosities and ability to withstand ultrasonic treatment and dead-end filtration up to 7 bar allow S-sintered monoliths to reach a high permeance (2634 L m-2 h-1 bar-1), permeability (1.25 x 10^-14 m2), and ability to reduce the chemical oxygen demand by 90% during filtration of a surfactant-stabilized oil in water emulsion, while indicating reasonable resistance towards fouling.</abstract>
    <parentTitle language="eng">Nanoscale Advances</parentTitle>
    <identifier type="doi">10.1039/D2NA00368F</identifier>
    <identifier type="issn">2516-0230</identifier>
    <identifier type="urn">urn:nbn:de:kobv:b43-555928</identifier>
    <enrichment key="opus.source">publish</enrichment>
    <enrichment key="date_peer_review">01.09.2022</enrichment>
    <enrichment key="opus.doi.autoCreate">false</enrichment>
    <enrichment key="opus.urn.autoCreate">true</enrichment>
    <licence>Creative Commons - Namensnennung 3.0</licence>
    <author>L. M. Henning</author>
    <author>J. T. Müller</author>
    <author>Glen Jacob Smales</author>
    <author>Brian Richard Pauw</author>
    <author>J. Schmidt</author>
    <author>M. F. Bekheet</author>
    <author>A. Gurlo</author>
    <author>U. Simon</author>
    <subject>
      <language>eng</language>
      <type>uncontrolled</type>
      <value>SAXS</value>
    </subject>
    <subject>
      <language>eng</language>
      <type>uncontrolled</type>
      <value>Hierarchically porous</value>
    </subject>
    <subject>
      <language>eng</language>
      <type>uncontrolled</type>
      <value>Silica</value>
    </subject>
    <subject>
      <language>eng</language>
      <type>uncontrolled</type>
      <value>Water filtration</value>
    </subject>
    <collection role="ddc" number="543">Analytische Chemie</collection>
    <collection role="ddc" number="620">Ingenieurwissenschaften und zugeordnete Tätigkeiten</collection>
    <collection role="institutes" number="">6 Materialchemie</collection>
    <collection role="institutes" number="">6.5 Synthese und Streuverfahren nanostrukturierter Materialien</collection>
    <collection role="themenfelder" number="">Material</collection>
    <collection role="themenfelder" number="">Chemie und Prozesstechnik</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="">Advanced Materials</collection>
    <thesisPublisher>Bundesanstalt für Materialforschung und -prüfung (BAM)</thesisPublisher>
    <file>https://opus4.kobv.de/opus4-bam/files/55592/029_Henning_Hierarchically_porous_and_mechanically_stable_monoliths.pdf</file>
  </doc>
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