Microwave-Induced Combustion Synthesis of Nanocrystalline TiO2–SiO2 Binary Oxide Material

2004 ◽  
Vol 19 (4) ◽  
pp. 1015-1023 ◽  
Author(s):  
I. Ganesh ◽  
R. Johnson ◽  
Y.R. Mahajan ◽  
A. Khan ◽  
S.S. Madhavendra ◽  
...  

A nanocrystalline titania–silica (1:1 molar ratio) binary oxide material was synthesized by microwave-induced combustion process in a modified domestic microwave oven (operated at 2.45 GHz frequency and 700 W power) in approximately 60 min from in situ synthesized titanyl nitrate and siliconyl nitrate using urea as fuel. For the sake of comparison, two different types of TiO2–SiO2 powders were also synthesized by the sol-gel and the co-precipitation methods. All the synthesized powders were characterized with the help of thermogravimetriy/differential thermal analysis, x-ray diffraction, transmission electron microscopy (TEM), and Brunauer–Emmett–Teller surface area measurements and the results compared. The as-synthesized TiO2–SiO2 powder obtained by the combustion process showed an average crystallite size of 10 nm and the specific surface area of 115 m2g-1. Among the three differently synthesized TiO2-SiO2 powders, only the microwave-induced combustion synthesis yielded crystalline material. TEM in particular confirmed the presence of nano-sized particles in the microwave-induced combustion-synthesized powder. Among the three analogies, microwave synthesis was found to be superior in terms of ease of processing leading to time and power savings.

2020 ◽  
Vol 63 (7) ◽  
pp. 126-132
Author(s):  
Lyubov V. Furda ◽  
◽  
Evgenia A. Tarasenko ◽  
Sofya N. Dudina ◽  
Olga E. Lebedeva ◽  
...  

In the present work amorphous silica-aluminas were synthesized by the coprecipitation method during the hydrolysis of an alcohol solution of tetraethoxysilane (with a tetraethoxysilane: alcohol mass ratio of 1: 1) and 6% aqueous solution of aluminum nitrate at pH values of 1, 3, and 10. The Si/Al molar ratio for all synthesized samples were 4.72 (± 0.29). The amorphous character of the investigated materials was confirmed by X-ray phase analysis. According to the results of scanning electron microscopy, it was found that the resulting powders have particles with a size of 1-20 μm. It was shown that the conditions of synthesis affected the specific surface area and porosity of the materials under study. By the method of low-temperature adsorption-thermodesorption of nitrogen it was established that silica-aluminas obtained under acidic conditions were microporous materials. For the sample obtained under alkaline conditions (pH = 10), the contribution of macropores is very significant. A decrease in surface area is observed as the pH of the synthesis increases. The Hammett indicator method was used to identify and quantify surface centers of different acidity. All studied silica-aluminas are characterized by the presence of both Brønsted basic (pKax from 7 to 12.8) and acidic (pKax from 0 to 7) centers, and Lewis basic (pKax from -4.4 to 0) with a pronounced maximum at pKax = 1.02. It was found that the synthesis conditions had a significant effect on the concentration of active centers. The values of the Hammett function are practically the same for the 3 studied silica-aluminas and describe the studied samples as materials of medium acidity. The variety of Lewis and Brønsted centers on the surface indicates the amphoteric properties of the materials under study. This gives the samples the properties of polyfunctional sorbents and catalysts.


2011 ◽  
Vol 341-342 ◽  
pp. 215-220
Author(s):  
Bao Wen Wang ◽  
Chuan Chang Gao ◽  
Hai Bo Zhao ◽  
Chu Guang Zheng

Fe2O3/Al2O3 composite at the mass ratio of 3:2 was prepared by sol-gel combustion synthesis using urea as fuel. The optimized preparation parameters were determined by the robust orthogonal experimental design (OED) method. Standard L9(34) orthogonal array was adopted, and the four factors were determined as the molar ratio of oxidizer nitrates to fuel urea Ф, relative amount of the deionized water added Rw, ignition temperature and sintering temperature. Range analysis of the relative importance of those four factors on the mean weight loss rate for the reduction of synthesized Fe2O3/Al2O3 with 50 vol% H2 indicated that the most influential factor was Ф, sintering temperature, Rw and ignition temperature in the descending order. And the optimized preparation parameters for Fe2O3/Al2O3 composite were Ф=1, Rw=7.5, ignition and sintering temperatures stabilized as 600°C and 950°C,respectively. Finally, the reaction characteristics of Fe2O3/Al2O3 prepared by SGCS and the other two reference methods (including sol-gel method and mechanical mixing method) were compared and the results verified that the optimized SGCS was the best option to synthesize Fe2O3/Al2O3 composite with good reaction performance.


2013 ◽  
Vol 829 ◽  
pp. 332-336
Author(s):  
Soheila Kharratian Khameneh ◽  
M. Heydarzadeh Sohi ◽  
Abolghasem Ataie ◽  
Saeed Mehrizi

A study of the incorporation of barium hexaferrite nanoparticles into a CoFe matrix by means of electrodeposition over brass substrates has been performed. Barium hexaferrite nanoparticles were prepared by co-precipitation route using solution of iron and barium nitrates with a Fe3+/Ba2+molar ratio of 8, by addition of NaOH with a OH-/NO3- molar ratio of 2. X-ray diffraction (XRD) results indicated that in a sample synthesized from aqueous solution and annealed at 900 °C for 1 hour, BaFe12O19 was the dominant phase. Field emission scanning electron microscopy (FE-SEM) showed plate-like particles of barium hexaferrite by mean diameter of 300 nm and thickness of 45 nm. CoFe-BaFe12O19 nanocomposite thin films were then electrodeposited froma Co-Fe bath containing the barium hexaferrite particles obtained in the first stage of this work. Finally, FE-SEM equipped with energy dispersive spectroscopy (EDS) analyzer and XRD analysis was applied on the deposited films, to confirm presence of the nanoparticles in the film. The average crystallite size of the deposits was around 30 nm. It was also noticed that increasing the concentration of the particles in the electroplating bath, caused a rise in the BaFe12O19 content of the deposits but had no significant effect on the composition of the CoFe matrix.


2012 ◽  
Vol 519 ◽  
pp. 83-86 ◽  
Author(s):  
Guang Wu Liu ◽  
Xing Yuan Ni ◽  
Bin Zhou ◽  
Qiu Jie Yu

This paper deals with the synthesis of ultralow density silica aerogels using tetramethyl orthosilicate (TMOS) as the precursor via sol-gel process followed by supercritical drying using acetonitrile solvent extraction. Ultralow density silica aerogels with 6 mg/cc of density was made for the molar ratio by this method. The microstructure and morphology of the ultralow density silica aerogels was characterized by the specific surface area, SBET, SEM, and the pore size distribution techniques. The results show that the ultralow density silica aerogel has the high specific surface area of 812m2/g. Thermal conductivities at desired temperatures were analyzed by the transient plane heat source method. Thermal conductivity coefficients of silica aerogel monoliths changed from 0.024 to 0.043W/ (m K) as temperature increased to 400°C, revealed an excellent heat insulation effect during thermal process.


2007 ◽  
Vol 336-338 ◽  
pp. 2286-2289
Author(s):  
Fei He ◽  
Xiao Dong He ◽  
Yao Li

Low-density xSiO2-(1-x)Al2O3 xerogels with x=0.9, 0.8, 0.7, 0.6 (mole fractions) were prepared by sol-gel and non-supercritical drying. Silica alkogels, which were the framework of binary composite materials, formed from tetraethyl orthosilicate (TEOS) by hydrolytic condensation with a molar ratio of TEOS: H2O: alcohol: hydrochloric acid: ammonia =1: 4: 10: 7.5×10-4: 0.0375. Aluminum hydroxide derived from Al(NO3)3·9H2O and NH4OH acting in the alcohol solution under the condition of catalyst. After filtrating and washing, the precipitation was mixed into silica sols to form SiO2-Al2O3 mixed oxide gels with different silicon and aluminum molar ratio. The structural change and crystallization of the binary xerogels were investigated after heat treatment at 600 for 2 h by the means of X-ray diffraction. Nitrogen adsorption experiment was performed to estimate specific surface area, porous volume and pore size distribution. The structural change of xerogels was observed by FT-IR spectroscopy. The resulting mixed xerogels possess of mesoporous structure which is characteristic of cylindrical pores, high specific surface area of 596-863 m2/g and a relatively narrow pore distribution of 2.8-30 nm. Al2O3 is introduced into the SiO2 phase and some of Al-O-Si bonds form.


2005 ◽  
Vol 893 ◽  
Author(s):  
Stephane Grandjean ◽  
Chapelet-Arab Bénédicte ◽  
Lemonnier Stéphane ◽  
Robisson Anne-Charlotte ◽  
Vigier Nicolas

AbstractActinides contained in the used nuclear fuel need to be managed in the future fuel cycles for the sustainability of this source of energy. The major ones such as uranium or plutonium are very valuable for energy production within a new fuel. The minor ones such as neptunium, americium or curium are responsible for the long-term radiotoxicity of the ultimate waste if not separated and transmuted within new fuels or dedicated targets. Whatever the choice of management in the present or future, innovative synthesis methods are studied in many research institutions to elaborate new actinides based materials.Innovative concepts for future fuels or transmutation targets focus on mixed actinides or mixed actinide-inert element materials. For their synthesis, wet methods fulfill very useful requirements such as flexibility, compatibility with a hydrometallurgical fuel processing, less dissemination of radioactive dusts during processing, and above all a better accessibility to very homogeneous compounds and interesting nanostructures. When dealing with plutonium or minor actinides, this last characteristic is of great importance in order to avoid the so-called “hot spots” and to limit macroscopic defects in the fuel material.In this communication, experimental results are given to illustrate interesting achievements to control the composition or the structure of mixed actinides compounds at a molecular or at a nanometric scale using co-precipitating techniques or sol-gel methods.The first illustration describes the flexibility of the oxalate ligand to modulate the nanostructure of actinides-based solid precursors and obtain mixed actinides oxide following a thermal treatment of the oxalate precursor. New mixed oxalate structures which present original features such as accepting in the same crystallographic site either a tetravalent actinide or a trivalent one are noticeably detailed. Monocharged cations equilibrate the charge in the 3D structure depending on the molar ratio of trivalent to tetravalent actinides. These oxalate compounds are particularly suitable precursors of oxide solid solutions for various actinides systems.The second illustration deals with the control of inorganic condensation reactions of tri- and tetravalent cations in solution by using suitable ligands with a view to obtaining homogeneous oxy-hydroxyde mixtures. The results obtained using Zr(IV), Y(III) and Am(III) or Nd(III) are quite original: a very stable colloidal sol is obtained at pH 5-6 and a nanostructured mixed oxy-hydroxide phase is formed by adapting the sol-gel transition conditions. The initial interactions between the oxy-hydroxide Zr nanoparticles, the ligand and the trivalent cations at a nanometric scale in the sol give access, after gel formation and thermal treatment, to a crystallized phase (Am-bearing cubic Y-stabilized Zirconia) at comparatively low temperatures.In both cases, the simultaneous co-precipitation or co-gelation of the involved actinides remains a challenge because of the specific properties of each actinide, properties which moreover differ according to various possible oxidation states.


2018 ◽  
Vol 127 (1A) ◽  
pp. 15
Author(s):  
Ngô Minh Đức

Hydrotalcite was synthesized using the co-precipitation method with  the Mg/Al molar ratio of 3.0 and then  calcined at 450 °C, for 5 h. The obtained solid was characterized by XRD, BET. As seen from results of physical characterization, the synthesized Hydrotalcite material owns large surface area of  309.3 m<sup>2</sup>/g, mean capillary diameter of 11.52 nm. Hydrotalcite application as adsorbent of heavy metal ions. The results of adsorption experiment for Pb<sup>2+</sup> in water showed that the absorption equilibrium was attained after 90 minutes at pH = 5 with maximum adsorption loading capacity of 144.93 mg/g. The synthesized adsorbent could be regenerated with HNO<sub>3</sub> (1M) solution


2002 ◽  
Vol 726 ◽  
Author(s):  
Fei Cheng ◽  
John S. Bradley

AbstractA silicon oximide gel was prepared by a reaction in N,N-dimethylformamide between tris(dimethylamino)silylamine (Me2N)3SiNH2 (TDSA) and formamide in a 1:2 molar ratio at 50C. The 29Si, 13C CP-MAS NMR and IR analyses indicated that the gel mainly comprised oximino silicon networks [SiOC(H)=NSi]x. The gel exhibited a microporous structure and had a total surface area of 339 m2/g. A microporous structure with a BET surface area of 195 m2/g was also obtained after pyrolysis of the gel at 1000°C for 2 h. Pyrolysis of the gel under N2 up to 1485°C gave an amorphous silicon oxycarbonitride glass.


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