Hierarchically Porous Oxides, Hybrids and Polymers via Sol-gel Accompanied by Phase Separation

2007 ◽  
Vol 1007 ◽  
Author(s):  
Kazuki Nakanishi

ABSTRACTIn various crosslinking systems containing metal oxides, organo-siloxane polymers and pure hydrocarbons, monolithic materials with hierarchical well-defined macropores and controlled mesopores have been synthesized. Synthetic progress in alkoxy-derived macroporous silica lead to the preparation of long-range ordered mesoporous skeletons in well-defined macroporous framework. Alkylene-bridged silicon alkoxides can also be prepared into similarly hierarchical porous structures with broadened variations in framework morphology. Macro-mesoporous alkoxy-derived pure titania and zirconia have been prepared using hydrochloric acid – mediated processes. Compared with those prepared from colloidal dispersions, alkoxy-derived macroporous titania exhibited much higher mechanical strength. Titania monolith is a promising candidate as a separation medium to discriminate phosphorylated compounds in a liquid chromatography mode. Pure alumina macroporous monolith has been first synthesized from aluminum salt using propylene glycol as a proton scavenger to thrust the solution pH from acidic into neutral conditions. Alumina-based complex oxides such as garnets and spinels can also be prepared in pure phases. Polymerization and phase separation in organic crosslinker system was also controlled to obtain well-defined co-continuous macro-frameworks instead of those composed of aggregated particles. These examples demonstrate the versatility of using phase-separation in gelling systems to obtain well-defined macroporous structures.

RSC Advances ◽  
2016 ◽  
Vol 6 (62) ◽  
pp. 57217-57226 ◽  
Author(s):  
A. R. Passos ◽  
S. H. Pulcinelli ◽  
V. Briois ◽  
C. V. Santilli

Mechanism of gelation process and phase separation for production of hierarchical porous alumina with high surface area.


Author(s):  
J. Tong ◽  
L. Eyring

There is increasing interest in composites containing zirconia because of their high strength, fracture toughness, and its great influence on the chemical durability in glass. For the zirconia-silica system, monolithic glasses, fibers and coatings have been obtained. There is currently a great interest in designing zirconia-toughened alumina including exploration of the processing methods and the toughening mechanism.The possibility of forming nanocrystal composites by a phase separation method has been investigated in three systems: zirconia-alumina, zirconia-silica and zirconia-titania using HREM. The morphological observations initially suggest that the formation of nanocrystal composites by a phase separation method is possible in the zirconia-alumina and zirconia-silica systems, but impossible in the zirconia-titania system. The separation-produced grain size in silica-zirconia system is around 5 nm and is more uniform than that in the alumina-zirconia system in which the sizes of the small polyhedron grains are around 10 nm. In the titania-zirconia system, there is no obvious separation as was observed in die alumina-zirconia and silica-zirconia system.


2000 ◽  
Vol 628 ◽  
Author(s):  
Guang-Way Jang ◽  
Ren-Jye Wu ◽  
Yuung-Ching Sheen ◽  
Ya-Hui Lin ◽  
Chi-Jung Chang

This work successfully prepared an UV curable organic-inorganic hybrid material consisting of organic modified colloidal silica. Applications of UV curable organic-inorganic hybrid materials include abrasion resistant coatings, photo-patternable thin films and waveguides. Colloidal silica containing reactive functional groups were also prepared by reacting organic silane and tetraethyl orthosilicate (TEOS) using sol-gel process. In addition, the efficiency of grafting organic moiety onto silica nanoparticles was investigated by applying TGA and FTIR techniques. Experimental results indicated a strong interdependence between surface modification efficiency and solution pH. Acrylate-SiO2 hybrid formation could result in a shifting of thermal degradation temperature of organic component from about 200°C to near 400°C. In addition, the stability of organic modified colloidal silica in UV curable formula and the physical properties of resulting coatings were discussed. Furthermore, the morphology of organic modified colloidal silica was investigated by performing TEM and SEM studies‥


2000 ◽  
Vol 628 ◽  
Author(s):  
Kazuki Nakanishi ◽  
Souichi Kumon ◽  
Kazuyuki Hirao ◽  
Hiroshi Jinnai

ABSTRACTMacroporous silicate thick films were prepared by a sol-gel dip-coating method accompanied by the phase separation using methyl-trimethoxysilane (MTMS), nitric acid and dimethylformamide (DMF) as starting components. The morphology of the film varied to a large extent depending on the time elapsed after the hydrolysis until the dipping of the coating solution. On a glass substrate, the films prepared by early dipping had inhomogeneous submicrometer-sized pores on the surface of the film. At increased reaction times, relatively narrow sized isolated macropores were observed and their size gradually decreased with the increase of reaction time. On a polyester substrate, in contrast, micrometer-sized isolated spherical gel domains were homogeneously deposited by earlier dippings. With an increase of reaction time, the volume fraction of the gel phase increased, then the morphology of the coating transformed into co-continuous gel domains and macropores, and finally inverted into the continuous gel domains with isolated macropores. The overall morphological variation with the reaction time was explained in terms of the phase separation and the structure freezing by the forced gelation, both of which were induced by the evaporation of methanol during the dipping operation.


2021 ◽  
Vol 13 (3) ◽  
pp. 371-380
Author(s):  
Yongjun Wu ◽  
Nina Xie ◽  
Lu Yu

A novel Ag–Si–TiO2 composite was prepared via sol–gel method for removing residual formaldehyde in shiitake mushroom. The structure of Ag–Si–TiO2 composite was characterized by scanning electron microscope (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) analyses. Ultraviolet-visible absorption spectroscopy (UV-Vis) and N2 adsorption-desorption tests showed that Ag and Si co-doped decreased the band gap, the Brunauer-Emmett-Teller (BET) specific surface area of the samples increased and the recombination probability of electron-hole pairs (e--h+) reduced. Effect on removal rate of formaldehyde with different Ag-Si co-doped content, formaldehyde concentration and solution pH were investigated, and the results showed that 6.0 wt%Ag-3.0 wt%Si-TiO2 samples had an optimum catalytic performance, and the degradation efficiency reached 96.6% after 40 W 365 nm UV lamp irradiation for 360 min. The kinetics of formaldehyde degradation by Ag–Si–TiO2 composite photocatalyst could be described by Langmuir-Hinshelwood first-order kinetic model.


2018 ◽  
Vol 768 ◽  
pp. 211-217 ◽  
Author(s):  
Rui Wang ◽  
Yu Kun Sun ◽  
Bao Jia Qi Jiang ◽  
Hui Yang ◽  
Xing Zhong Guo

Macroporous Ca12Al14O33(C12A7) mayenite monoliths have been successfully prepared via a sol-gel process in the presence of propylene oxide (PO) and poly (ethyleneoxide) (PEO). Gelation of CaO-Al2O3binary system with nitrates salts as additional precursors is accelerated by PO as an acid scavenger, while PEO works as a phase separation inducer to mediate the phase separation of the system. Appropriate PO and PEO amounts allow the formation of monolithic xerogel with interconnected macropores and co-continuous skeletons. The resultant dried gels are amorphous and the single crystalline phase Ca12Al14O33mayenite forms after heat-treatment at 1100 °C in air, while the macrostructure is preserved with a porosity as high as 78% and smoother and denser skeletons.


2012 ◽  
Vol 15 (2) ◽  
Author(s):  
Mohammad Hossein Habibi ◽  
Maryam Mikhak

AbstractNanostructured zinc titanate (NZT) was synthesized in high yield via a one-step and template-free sol-gel route. The prepared nanocomposite exhibited good size uniformity and regularity. The enhanced photocatalytic activity of the NZT was evaluated in the degradation and mineralization of Indocorn Brilliant Red (M5B) under metal halide lamp irradiation. The effects of different parameters such as pH of the solution, and initial dye concentration on photodegradation of M5B were analyzed. The degradation of M5B follows pseudo-first order kinetics according to the Langmuir-Hinshelwood model. The experimental results showed that the initial concentration of azo dye in the dye mixture greatly affected the degradation efficiency. At M5B concentrations of 10 mg/L, the optimum conditions for the highest degradation efficiency (94%) of azo dye were a photocatalyst dosage of 0.01 g/L and an initial solution pH of 9. This study provided new insight into the design and preparation of nanomaterial demonstrated an excellent ability to remove organic pollutants in wastewater.


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