Rapid (&lt;3 min) microwave synthesis of block copolymer templated ordered mesoporous metal oxide and carbonate films using nitrate–citric acid systems

Zhang, Yuanzhong; Bhaway, Sarang M.; Wang, Yi; Cavicchi, Kevin A.; Becker, Matthew L.; Vogt, Bryan D.

doi:10.1039/c4cc09808k

Cited by 16 publications

(29 citation statements)

References 18 publications

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“…2,5,7 Alternative nonequilibrium methods have been explored for the rapid formation of single crystal and polycrystalline inorganic nanostructures on shorter time frames. [20][21][22][23][24][25][26][27][28][29] For example, Tan et al demonstrated an all-laser-induced approach coupling BCP-directed self-assembly of resols with sub-millisecond laser heating (B-WRITE) to write hierarchically mesoporous polymer and carbon thin film structures. 21 Periodically ordered mesoporous crystalline silicon nanostructures were then obtained by filling the continuous network polymer template with amorphous silicon, followed by nanosecond laser-induced melt-crystallization and template removal.…”

Section: Main Textmentioning

confidence: 99%

“…[21][22][23] Microwave annealing of mesoporous metal oxide thin films has been described but it required several minutes attaining limited crystallinity. 25 More recently, Hu et al and Tour et al reported a rapid Joule heating-based method generating discrete high-entropy metal nanoparticles, 26,27 sintered pellets of garnet ceramics with low porosity 28 and turbostratic graphene layers 29 on the milli-to tens of second timescales. We hypothesize pairing soft matter-directed self-assembly with Joule heating to form highly crystalline, wellordered mesoporous inorganic structures could open new pathways to access unique functional property profiles, expand parameter and application space, as well as develop new fundamental understanding of processing-structure-property correlations.…”

Section: Main Textmentioning

confidence: 99%

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Ultrafast Crystallization of Ordered Mesoporous Metal Oxides and Carbon in Seconds

Wang¹,

Seah²,

Li³

et al. 2021

Preprint

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This Communication describes a facile strategy coupling block copolymer-directed self-assembly with high-power Joule heating to form highly crystalline and long-range ordered mesoporous oxide and carbon nanostructures in just a few seconds. The combined approach is compatible with various self-assembled hybrid systems, generating mesoporous composites of γ-Al2O3-carbon, γ-Al2O3/MgO-carbon and anatase-TiO2-carbon with p6mm symmetry, as well as mesoporous non-close-packed carbon structures. Removing the polymer/carbon gives well-defined mesoporous all-γ-Al2O3 and all-anatase-TiO2 structures. Impregnation of chloroplatinic acid followed by Joule heating yields platinum nanoparticles decorated on the channel walls of mesoporous γ-Al2O3-carbon structures. The rapid formation of thermally stable and periodically ordered crystalline oxide, carbon and oxide-carbon structures. <br>

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Section: Main Textmentioning

confidence: 99%

Section: Main Textmentioning

confidence: 99%

Ultrafast Crystallization of Ordered Mesoporous Metal Oxides and Carbon in Seconds

Wang¹,

Seah²,

Li³

et al. 2021

Preprint

View full text Add to dashboard Cite

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“…In general, rapid thermal annealing techniques using laser heating, radiation in rapid thermal processing, or microwave energy have been able to provide similar (or even better) ordering kinetics without the same EHS concerns . As such there has been significant interest in microwave annealing for DSA.…”

Section: Introductionmentioning

confidence: 99%

Evolution in surface morphology during rapid microwave annealing of PS‐b‐PMMA thin films

Qiang¹,

Ye²,

Lin³

et al. 2016

J Polym Sci B Polym Phys

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Microwave annealing enables rapid (60 s) ordering and orientation of block copolymer films. The developed morphology in polystyrene-block-poly(methyl methacrylate) (PS-b-PMMA) thin films depends on details of the heating rate that is controlled by microwave output energy as well as the sample location in the microwave. Over a wide heating rate (1.1-2.7 8C/ s), perpendicular orientation of the cylindrical mesostructure at the surface is >50% after 60 s, but goes through a maximum at 1.8 8C/s leading to approximately 97% perpendicular cylinders at the surface. The propagation of this perpendicular surface morphology through the film thickness is also dependent upon the microwave annealing conditions. The surface structure evolves with the microwave annealing time from imperfect ordering to perpendicular cylinders to parallel cylinders as the annealing time increases. This work demonstrates the importance of controlling the heating rate during microwave annealing, which will be critical for optimizing microwave conditions for directed self-assembly.

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“…Since the discovery of mesoporous silica in 1990s, [13] ad iverse range of porous powders and films has been produced through hard-(e.g.,o rdered mesoporous silica, latex polymer beads) [14][15][16][17] and soft-templating (e.g.,s urfactants, triblock copolymers) [18][19][20][21][22][23][24][25] approaches. The templates can be removed by decomposition (calcination) with as tructuralt ension.…”

Section: Introductionmentioning

confidence: 99%

Analytical Understanding of the Materials Design with Well‐Described Shrinkages on Multiscale

Dutta

et al. 2018

Chemistry A European J

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Shrinkages derived from condensation of frameworks are one of the significant steps for fabricating demanded materials having unique morphologies and properties. Enormous efforts have been dedicated to understanding their mechanisms that are quite useful for the materials design. In this context, diversified measuring and observing tools have been facilitated to evaluate structural contractions and corresponding driving forces. All of the investigations are crucial to encourage the utilization of such shrinkages for the precise design of nanomaterials. In this review, we summarize significant works how to analyze shrinkages in multiscale during the synthesis of materials, which will be useful as a follow-up review to our latest contribution. Well-defined porous materials are also selected as a good candidate for understanding well-described shrinkages. This review aims to provide a detailed glimpse of the development of analyses on shrinking behaviors in multiscale for the materials design. Shrinking degree and direction in multiscale, which are driven by condensation of frameworks, are predominant for understanding and/or predicting final nanostructures of materials after shrinkages.

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Rapid (<3 min) microwave synthesis of block copolymer templated ordered mesoporous metal oxide and carbonate films using nitrate–citric acid systems

Cited by 16 publications

References 18 publications

Ultrafast Crystallization of Ordered Mesoporous Metal Oxides and Carbon in Seconds

Ultrafast Crystallization of Ordered Mesoporous Metal Oxides and Carbon in Seconds

Evolution in surface morphology during rapid microwave annealing of PS‐b‐PMMA thin films

Analytical Understanding of the Materials Design with Well‐Described Shrinkages on Multiscale

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