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Synthesis And Characterization Of Nanosized Inorganic Non-Metal Materials

Posted on:2006-03-06Degree:DoctorType:Dissertation
Country:ChinaCandidate:G ChuFull Text:PDF
GTID:1101360155458196Subject:Non-ferrous metallurgy
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Nanoparticles and nanocluster materials are a new class of advanced materials exhibiting unique chemical and physical properties compared to those of their bulk materials. Nanometer α-Al2O3 powder was prepared by the method of Low-temperature Combustion Synthesis (LCS) with aluminum nitrate and urea as raw materials. Through XRD, TEM, FT-IR and TG-DTA measurements the as-prepared powder was analyzed. It was found that polymorphic α-Al2O3 powders having an average gain size about 60-80 nm with the shape of approximate sphere can be synthesized under the condition that the A1(NO3)3·9H2O/CO(NH2)2 ratio was 1 to 2, the igniting temperature was 700 ℃ and with a temperature elevating rate faster than 100 ℃/min. TiO2 nanoparticles are prepared by adjusting the pH value of the reaction system, TiOSO4 as raw material, and organic acid as combustible component. When urea is used as combustible component, TiO2 is mainly rutile; when citric acid is used as combustible component, TiO2 is mainly anatase. XRD determination results show that the organic component is decomposed completely. TEM determination and the method of XRD single-peak fourier analysis calculation demonstrate that the grain size of TiO2 is 1025nm. Using hydrate ferric nitrate as starting materials and PVA as chelate agent, α-Fe2O3 nanoparticles were successfully prepared by the combustion method. The combustion products were analyzed and investigated by means of XRD and infrared spectroscope. The results show that the products of combustion reactionat 150 ℃ includes partial α-Fe2O3 and organic components. After calciningas-combusted product at 450℃ for 2h, the α-Fe2O3 is obtained and organic components is decomposed completely, The diameter of particles in the product of calcinations is 25nm to 50nm with the new Fourier single-peak analysis method forsubstructure size by XRD and TEM. The 01-AI2O3 nanoparticle was prepared by combustion synthesis method.Solid oxide fuel cell's cathode material Lao.9Sro.iMn03 was prepared by microwave synthesis. The thermal expansion coefficients of lattice parameters of Lao.9Sro.iMnC>3> Lao.ySrojMnOs and (X-AI2O3 were determined and discussed by means of dynamic high temperature powder XRD in the temperature rang from room temperature to 1200°C. We could conclude that there was linearity relation between expansion coefficients of lattice parameter and temperature by experimental result. The thermal expansion coefficient values of Aa/a<^ Ac/co and AV/Vo per degree of Lao.9Sro.iMn03> Lao.7Sro.3Mn03 and a-Al2O3 lattice were 9.1X10'6/°C, 11.8X10"6/ °C and 29.7 X106/°C\ 9.1xl()-6/0C, 11.8xlO"6/°C, 29.8xlO'6/°C and 7.27X I(r6/°C> 7.50X 10-6/°C and 21.92X 10"6/°C respectively. From the XRD analysis it also could be concluded that there was no phase change or construct change in the temperature range showed above.Zinc complex of 1,2,3,4-butanetetracarboxylate was synthesized by a reaction of ZnSC>4 with sodium 1,2,3,4-butanetetracarboxylate. The results of elemental analysis and TG analysis show that the formula of the complex is Z^CCgHeOs^HbO. FT-IR analysis confirmed the formation of the complex. TG analysis shows that the starting decomposion temperature of the complex is about 400 °C. Nano-ZnO was prepared by thermal decomposion of Zn2(CgH6Og)-2H2O. TEM observation showed the average size of nano-ZnO is about 20-50nm.The mechanism of the thermal decomposition process of Mg(OH)2 at different temperatures is studied by means of dynamic high temperature powder XRD for the purpose of finding the ways to produce different particles sized nonaparticles under the best conditions. In the temperature rang from room temperature to 1200°C, the average size of MgO is 25 to 200nm at 450 to 900°C.A new method for quantitative phase analysis is proposed by using XRD multi-peak match intensity ratio. This method can obtain the multi-peak match intensity ratio among each phase in the mixture sample by using multi-peak data of XRD pattern in the mixture sample and combining the relative intensity distribution...
Keywords/Search Tags:Combustion Synthesis, Microwave Synthesis, Inorganic Non-Metal Materials, Nanoparticles, Thermal Decomposition Thermal Expansion Coefficients of tile Lattice, Dynamic high temperature powder XRD, Characterization
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