scholarly journals Chemical Structure and Microstructure Characterization of Ladder-Like Silsesquioxanes Derived Porous Silicon Oxycarbide Materials

Materials ◽  
2021 ◽  
Vol 14 (6) ◽  
pp. 1340
Author(s):  
Jakub Marchewka ◽  
Piotr Jeleń ◽  
Izabela Rutkowska ◽  
Patryk Bezkosty ◽  
Maciej Sitarz

The aim of this work was to synthesize porous ceramic materials from the SiOC system by the sol-gel method and the subsequent pyrolysis. The usage of two types of precursors (siloxanes) was determined by Si/C ratio in starting materials. It allows us to control the size of the pores and specific surface area, which are crucial for the potential applications of the final product after thermal processing. Methyltrimethoxysilane and dimethyldiethoxysilane were mixed in three different molar ratios: 4:1, 2:1, and 1:1 to emphasize Si/C ratio impact on silicon oxycarbide glasses properties. Structure and microstructure were examined both for xerogels and obtained silicon oxycarbide materials. Brunauer-Emmett-Teller (BET) analysis was performed to confirm that obtained materials are porous and Si/C ratio in siloxanes precursors affects porosity and specific surface area. This kind of porous ceramics could be potentially applied as gas sensors in high temperatures, catalyst supports, filters, adsorbents, or advanced drug delivery systems.

2021 ◽  
Author(s):  
Prakash Parajuli ◽  
Sanjit Acharya ◽  
Julia Shamshina ◽  
Noureddine Abidi

Abstract In this study, alkali and alkaline earth metal chlorides with different cationic radii (LiCl, NaCl, and KCl, MgCl2, and CaCl2) were used to gain insight into the behavior of cellulose solutions in the presence of salts. The specific focus of the study was evaluation of the effect of salts’ addition on the sol-gel transition of the cellulose solutions and on their ability to form monoliths, as well as evaluation of the morphology (e.g., specific surface area, pore characteristics, and microstructure) of aerocelluloses prepared from these solutions. The effect of the salt addition on the sol-gel transition of cellulose solutions was studied using rheology, and morphology of resultant aerogels was evaluated by Scanning Electron Microscopy (SEM) and Brunauer-Emmett-Teller (BET) analysis, while the salt influence on the aerocelluloses’ crystalline structure and thermal stability was evaluated using powder X-Ray Diffraction (pXRD) and Thermogravimetric Analysis (TGA), respectively. The study revealed that the effect of salts’ addition was dependent on the component ions and their concentration. The addition of salts in the amount below certain concentration limit significantly improved the ability of the cellulose solutions to form monoliths and reduced the sol-gel transition time. Salts of lower cationic radii had a greater effect on gelation. However, excessive amount of salts resulted in the formation of fragile monoliths or no formation of gels at all. Analysis of surface morphology demonstrated that the addition of salts resulted in a significant increase in porosity and specific surface area, with salts of lower cationic radii leading to aerogels with much larger (~1.5 and 1.6-fold for LiCl and MgCl2, respectively) specific surface area compared to aerocelluloses prepared with no added salt. Thus, by adding the appropriate salt into the cellulose solution prior to gelation, the properties of aerocelluloses that control material’s performance (specific surface area, density, and porosity) could be tailored for a specific application.


Clay Minerals ◽  
2018 ◽  
Vol 53 (4) ◽  
pp. 665-674 ◽  
Author(s):  
Emmanuel Ajenifuja ◽  
Abimbola P.I. Popoola ◽  
Kabir O. Oyedotun ◽  
Olawale Popoola

ABSTRACTKaolin and diatomite are abundant and widely available geological materials that may immobilize or stabilize functional chemical species on their surfaces for various applications. Acid-treated kaolin and diatomite were intercalated with photocatalyst Ag-TiO2nanoparticles using the sol–gel technique to prepare nanocomposite ceramic materials. The nanocomposites were sintered between 900°C and 1000°C to induce thermal reactions and to enhance nanoparticle–substrate attachment. Chemical and thermal characterizations of the acid-treated materials and intercalated nanocomposites were performed with energy-dispersive X-ray (EDX) analysis and differential scanning calorimetry (DSC), respectively. The Brunauer–Emmett–Teller (BET)-specific surface area and scanning electron microscopy (SEM) were employed for physical and microstructural characterization of the nanocomposites, respectively. Morphological studies revealed a uniform distribution of Ag-TiO2nanocrystallites in pores and on mineral particle surfaces. The BET analysis showed remarkable surface and grain modification by sintering. Decreases in the BET-specific surface area were observed for the sintered ceramic nanocomposite, Ag-TiO2-kaolin (20.244 to 5.446 m2/g) and Ag-TiO2-diatomite (19.582 to 10.148 m2/g).


Materials ◽  
2019 ◽  
Vol 12 (23) ◽  
pp. 3862 ◽  
Author(s):  
Fangtong Xie ◽  
Emanuel Ionescu ◽  
Marcela Arango-Ospina ◽  
Ralf Riedel ◽  
Aldo R. Boccaccini ◽  
...  

In the present work, Ca-containing silicon oxycarbides (SiCaOC) with varying Ca content have been synthesized via sol-gel processing and thermal treatment in inert gas atmosphere (pyrolysis). It has been shown that the as-prepared SiCaOC materials with low Ca loadings (Ca/Si molar ratios = 0.05 or 0.12) were X-ray amorphous; their glassy network contains Q3 sites, indicating the presence of Ca2+ at non-bridging-oxygen sites. SiCaOC with high Ca content (i.e., Ca/Si molar ratio = 0.50) exhibits the presence of crystalline calcium silicate (mainly pseudowollastonite). Furthermore, it has been shown that the incorporation of Ca into the SiOC glassy network has a significant effect on its porosity and specific surface area. Thus, the as-prepared Ca-free SiOC material is shown to be non-porous and having a specific surface area (SSA) of 22.5 m2/g; whereas SiCaOC with Ca/Si molar ratio of 0.05 exhibits mesoporosity and a SSA value of 123.4 m2/g. The further increase of Ca content leads to a decrease of the SSA and the generation of macroporosity in SiCaOC; thus, SiCaOC with Ca/Si molar ratio of 0.12 is macroporous and exhibits a SSA value of 39.5 m2/g. Bioactivity assessment in simulated body fluid (SBF) confirms the hydroxyapatite formation on all SiCaOC samples after seven days soaking, unlike the relatively inert ternary silicon oxycarbide reference. In particular, SiCaOC with a Ca/Si molar ratio of 0.05 shows an increased apatite forming ability compared to that of SiCaOC with Ca/Si molar ratio of 0.12; this difference is considered to be a direct consequence of the significantly higher SSA of the sample with the Ca/Si ratio of 0.05. The present work indicates two effects of Ca incorporation into the silicon oxycarbide glassy network on its bioactivity: Firstly, Ca2+ is shown to contribute to the slight depolymerization of the network, which clearly triggers the hydroxyapatite formation (compare the bioactive behavior of SiOC to that of SiCaOC with Ca/Si molar ratio 0.12 upon SBF exposure); secondly, the Ca2+ incorporation seems to strongly affect the porosity and SSA in the prepared SiCaOC materials. There is an optimum of Ca loading into the silicon oxycarbide glassy network (at a Ca/Si molar ration of 0.05), which provides mesoporosity and reaches maximum SSA, both highly beneficial for the bioactive behavior of the materials. An increase of the Ca loading leads, in addition to the crystallization of calcium silicates, to a coarsening of the pores (i.e., macroporosity) and a significant decrease of the SSA, both negatively affecting the bioactivity.


2020 ◽  
Vol 850 ◽  
pp. 273-278
Author(s):  
Ilmārs Zālīte ◽  
Līga Grase ◽  
Santa Lagzdina ◽  
Dzintra Rašmane

For sintering Al2O3 porous ceramic were used plasma-chemical synthesed powders with a specific surface area of 30 and 50 m2/g. Sintering were carried out in various conditions: sintering in nitrogen atmosphere, in air or vacuum at 1200-1700 °C. The most suitable sintering conditions are sintering in air at 1200-1500 °C using Al2O3 nanopowder with a specific surface area of 50 m2/g. Samples with open porosity of 35-45% and average pore size of 100-200 nm were obtained under these conditions.


2020 ◽  
Vol 67 (1) ◽  
pp. 148-155
Author(s):  
Anatoliy V. Fedotov ◽  
Viktor S. Grigoriev ◽  
Dmitriy A. Kovalev ◽  
Andrey A. Kovalev

To speed up the wastewater treatment under aerobic conditions and to optimize the processes of anaerobic wastewater treatment in digesters, immobilization technologies of microorganisms and enzymes on solid carriers are used. Ceramic carriers based on aluminosilicates and alumina are one of the promising inorganic biomass carriers. (Research purpose) To study the structure of porous ceramic biomass carriers for anaerobic processing of organic waste and evaluate the prospects for their use. (Materials and methods) The substrate for anaerobic digestion was a mixture of sediments of the primary and secondary sewage sumps of the Lyubertsy treatment facilities. K-65 cattle feed was used to ensure the constancy of the composition of organic substances in substrates as a cosubstrate. The authors used the method of low-temperature nitrogen adsorption of Bruner-Emmett-Teller to study the pore structure and specific surface of solid carriers on a specific surface analyzer Quntachrome Autosorb-1. (Results and discussion) The main characteristics (specific surface, volume of micro- and mesopores, predominant pore radius, water absorption and others) of chamotte foam lightweight and highly porous corundum ceramics were determined. It was revealed that ceramic materials with a developed surface and electrically conductive material provided an increase in biogas yield by 3.8-3.9 percent with an increase in methane content by an average of 5 percent. (Conclusions) The results of anaerobic digestion showed a positive effect of both a conductive carrier and highly porous ceramic materials on the process of anaerobic bioconversion of organic waste into biogas. It is advisable to expand experimental studies on the use of a conductive carrier with a developed surface based on highly porous ceramics.


2011 ◽  
Vol 10 (2) ◽  
pp. 25
Author(s):  
Anirut Leksomboon ◽  
Bunjerd Jongsomjit

In this present study, the spherical silica support was synthesized from tetraethyloxysilane (TEOS), water, sodium hydroxide, ethylene glycol and n-dodecyltrimethyl ammonium bromide (C12TMABr). The particle size was controlled by variation of the ethylene glycol co-solvent weight ratio of a sol-gel method preparation in the range of 0.10 to 0.50. In addition, the particle size apparently increases with high weight ratio of co-solvent, but the particle size distribution was broader. The standard deviation of particle diameter is large when the co-solvent weight ratio is more than 0.35 and less than 0.15. However, the specific surface area was similar for all weight ratios ranging from 1000 to 1300 m2/g. The synthesized silica was spherical and has high specific surface area. The cobalt was impregnated onto the obtained silica to produce the cobalt catalyst used for CO2 hydrogenation.</


2013 ◽  
Vol 831 ◽  
pp. 263-266
Author(s):  
Chung Hsin Wu ◽  
Chao Yin Kuo ◽  
Chih Hao Lai ◽  
Wei Yang Chung

This study explored the decolorization of C.I. Reactive Red 2 (RR2) by the ultraviolet (UV)/TiO2, UV/TiO2 + In2O3, and UV/TiO2-In2O3 systems. The TiO2-In2O3 was generated by the sol-gel method and TiO2 + In2O3 was created by mixing TiO2 and In2O3 powders. The surface properties of TiO2, In2O3, and TiO2-In2O3 were analyzed by X-ray diffraction, a specific surface area analyzer, UV-vis spectroscopy, and scanning electron microscopy. The specific surface area of TiO2, In2O3, and TiO2-In2O3 was 29.5, 44.6, and 35.7 m2/g, respectively; additionally, the band gap of TiO2, In2O3, and TiO2-In2O3 was 2.95, 2.64, and 2.91 eV; respectively. The decolorization rate constant fit pseudo-first-order kinetics and that of the UV/TiO2, UV/TiO2 + In2O3, and UV/TiO2-In2O3 systems was 0.0023, 0.0031, and 0.0072 min-1; respectively.


2007 ◽  
Vol 336-338 ◽  
pp. 1102-1104 ◽  
Author(s):  
Ming Sheng He ◽  
Jian Bao Li ◽  
Bo Wen Li ◽  
Hong Lin ◽  
Xiao Zhan Yang ◽  
...  

Wollastonite powder was selected as a starting material with carbonate as pore-forming agent and binder added. The porous ceramics were prepared at different temperature by sintering method. The process includes batching, granulating, pressing molding, drying and sintering. It is discussed the influence of sintering temperature, dosage of binder, dosage of pore-forming agent, pressure of molding and holding time on the performance of porous ceramics. According to the principle of particles stack, the porous wollastonite ceramics for filtration with various diameters, shapes and porosity were fabricated by serial experiments. These products have 1 to 10 microns in pore size, 30.04 to 66.15% in porosity, 2.82 m2/g in specific surface area.


2011 ◽  
Vol 403-408 ◽  
pp. 1205-1210
Author(s):  
Jaleh Babak ◽  
Ashrafi Ghazaleh ◽  
Gholami Nasim ◽  
Azizian Saeid ◽  
Golbedaghi Reza ◽  
...  

In this work ZnO nanocrystal powders have been synthesized by using Zinc acetate dehydrate as a precursor and sol-gel method. Then the products have been annealed at temperature of 200-1050°C, for 2 hours. The powders were characterized using X-ray diffraction (XRD), UV-vis absorption and photoluminescence (PL) spectroscopy. The morphology of refrence ZnO nanoparticles have been studied using Transmission Electron Microscope (TEM). During the annealing process, increase in nanocrystal size, defects and energy gap quantitative, and decrease in specific surface area have been observed.


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