Generalized Synthesis of Mesoporous Rare Earth Oxide Thin Films through Amphiphilic Ionic Block Copolymer Templating

Xiao, Ying; You, Shusen; Yao, Yuan; Zheng, Tao; Chen, Lin; Roth, Stephan V.; Müller‐Buschbaum, Peter; Steffen, Werner; Sun, Ling‐Dong; Yan, Chun‐Hua; Gutmann, Jochen S.; Yin, Meizhen; Fu, Jun; Cheng, Ya‐Jun

doi:10.1002/ejic.201201524

Cited by 8 publications

(12 citation statements)

References 31 publications

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“…[15,18,[20][21][22][23][24][25][26] However, to our knowledge, only few crystalline rare-earth sesquioxides with an ordered mesoporous structure have been reported so far. [27][28][29][30] Castro et al reported the synthesis and optical properties of Eu 2 O 3 and Y 2 O 3 . [28,29] They showed that both materials can be templated to produce mesoporous thin films, but the synthesis involved several different steps and was rather complicated and time-consuming.…”

Section: Introductionmentioning

confidence: 99%

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Facile and General Synthesis of Thermally Stable Ordered Mesoporous Rare-Earth Oxide Ceramic Thin Films with Uniform Mid-Size to Large-Size Pores and Strong Crystalline Texture

Reitz

Haetge²,

Suchomski

et al. 2013

Chem. Mater.

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We describe the general synthesis of sub-micron-thick rare-earth/lanthanide sesquioxide (RE 2 O 3 ) films with tailorable pore and grain sizes by polymer templating of hydrated chloride salt precursors. Mesostructured RE 2 O 3 (RE = Sm, Tb-Lu) ceramics with cubic pore symmetry and high surface area (S BET ≥ 50 m 2 •g -1 ) were prepared using different diblock copolymer structure-directing agents and were characterized by a combination of electron microscopy, in situ and ex situ grazing incidence small-angle X-ray scattering, N 2 -physisorption, X-ray photoelectron spectroscopy, X-ray diffraction including Rietveld refinement, and UV-vis spectroscopy. In the present work, we specifically focus on Dy 2 O 3 and Yb 2 O 3 and use both of these materials as model systems to study, among other things, the film formation and microstructure. Our research data collectively demonstrate that (1) record pore sizes of up to 42 nm in diameter can be achieved without the need for swelling agents, (2) the nanostructure can be preserved up to 1000 °C for the heavier oxides, (3) the sizes of the optical band gaps (4.9-5.6 eV) are comparable to those reported for single crystals, (4) the sol-gel derived materials are single phase and adopt the C-type crystal structure, and that (5) and Lu 2 O 3 films (March G 2 parameters of under 0.1). Overall, the synthesis parameters described in this work provide a blueprint for the preparation of thermally stable rare-earth oxide ceramics with both a mesoporous morphology and iso-oriented nanocrystalline walls.

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Section: Introductionmentioning

confidence: 99%

“…[30] SDA used produced materials with rather small repeat distances is not beneficial as it strongly limits the thermal stability of the materials. Nevertheless, this approach is the only one in the literature that tends to be of a more general nature.…”

mentioning

confidence: 99%

Facile and General Synthesis of Thermally Stable Ordered Mesoporous Rare-Earth Oxide Ceramic Thin Films with Uniform Mid-Size to Large-Size Pores and Strong Crystalline Texture

Reitz

Haetge²,

Suchomski

et al. 2013

Chem. Mater.

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“…Xiao et al. chose a diblock copolymer of poly(styrene‐ b ‐acrylic acid) as a pore‐directing agent to synthesize a series of mesoporous RE 2 O 3 thin films with a pore size of about 11 nm . Brezesinski et al.…”

Section: Figurementioning

confidence: 99%

“…[14] Xiao et al chose ad iblock copolymer of poly(styrene-b-acrylic acid) as ap ore-directing agent to synthesize as eries of mesoporous RE 2 O 3 thin films with ap ore size of about 11 nm. [15] Brezesinski et al reported an ew method to synthesize ordered mesoporous RE 2 O 3 thin films, in which poly(ethylene-co-butylene-bethylene oxide) (KLE)a nd poly(isobutylene-b-ethylene oxide) workeda sp ore-directing agentsa nd glacial acetic acid played ac rucial role in suppressing the recrystallization of RE 2 O 3 . [16,17] Use of the KLE template was also reported for the preparation of mesoporous Eu 2 O 3 thin films.…”

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confidence: 99%

Easy and General Synthesis of Large‐Sized Mesoporous Rare‐Earth Oxide Thin Films by ′Micelle Assembly′

Bastakoti

Imura

et al. 2015

Chemistry An Asian Journal

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Large-sized (ca. 40 nm) mesoporous Er2O3 thin films are synthesized by using a triblock copolymer poly(styrene-b-2-vinyl pyridine-b-ethylene oxide) (PS-b-P2VP-b-PEO) as a pore directing agent. Each block makes different contributions and the molar ratio of PVP/Er(3+) is crucial to guide the resultant mesoporous structure. An easy and general method is proposed and used to prepare a series of mesoporous rare-earth oxide (Sm2O3, Dy2O3, Tb2O3, Ho2O3, Yb2O3, and Lu2O3) thin films with potential uses in electronics and optical devices.

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“…In this block copolymer assisted synthetic route, the hydrolysis and condensation products of the organic precursors are preferentially incorporated into one of the blocks through hydrogen bonds. Accordingly, the morphology control of the corresponding functional inorganic part can be realized by phase separation behavior of the sol–gel solution . Templin and coauthors prepared a kind of organically modified aluminosilicate mesostructures from amphiphilic poly(isoprene‐b‐ethylene oxide) block copolymers.…”

Section: Introductionmentioning

confidence: 99%

Key Factors for Template‐Oriented Porous Titania Synthesis: Solvents and Catalysts

et al. 2020

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Various types of titania nanostructures are synthesized with a polymer‐templated sol–gel method based on the amphiphilic diblock copolymer polystyrene‐b‐polyethylene oxide (PS‐b‐PEO) in combination with selective incorporation of the titania precursor titanium tetraisopropoxide. Custom tailoring of different types of titania morphologies is realized by changing the phase separation behavior of the PS‐b‐PEO template. Particularly, application of solvents from different categories is found to have a major impact upon the phase separation behavior of PS‐b‐PEO and the final titania film morphology. The amount of available hydrochloric acid catalyst during the gelation process is seen as an additional key factor to induce controllable morphological changes. Scanning electron microscopy and grazing incidence small angle X‐ray scattering measurements are carried out to study the surface and inner structure of porous titania films. Systematic analysis and comparison of different characterization results allow attributing the following three factors to the respectively formed titania nanostructure: the surface energy between PS blocks and surrounding solvent, the aggregation behavior of the titania nanoparticles, and the block‐specific selectivity of the used solvent. For all synthesized titania thin films, an anatase‐type crystallization is confirmed through X‐ray powder diffraction.

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Generalized Synthesis of Mesoporous Rare Earth Oxide Thin Films through Amphiphilic Ionic Block Copolymer Templating

Cited by 8 publications

References 31 publications

Facile and General Synthesis of Thermally Stable Ordered Mesoporous Rare-Earth Oxide Ceramic Thin Films with Uniform Mid-Size to Large-Size Pores and Strong Crystalline Texture

Facile and General Synthesis of Thermally Stable Ordered Mesoporous Rare-Earth Oxide Ceramic Thin Films with Uniform Mid-Size to Large-Size Pores and Strong Crystalline Texture

Easy and General Synthesis of Large‐Sized Mesoporous Rare‐Earth Oxide Thin Films by ′Micelle Assembly′

Key Factors for Template‐Oriented Porous Titania Synthesis: Solvents and Catalysts

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