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Synthesis and Characterization of Ultrafine Powders of Metal and Oxides via Hydrothermal and Solvothermal Methods

Author: WeiMingZhen
Tutor: WenShuLin
School: Shandong University
Course: Materials Science
Keywords: Hydrothermal method Solvothermal Copper Cuprous oxide Iron-based materials
CLC: TB383.3
Type: Master's thesis
Year: 2007
Downloads: 206
Quote: 0
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Abstract


This article aims to explore copper and iron-based materials, low-temperature hydrothermal and solvothermal synthesis of new methods, new routes, in order to optimize the synthesis conditions, the study also part of the copper and iron-based materials under the conditions of the hydrothermal and solvothermal The formation mechanism. The completed work can be summarized as the following three parts: First, the use of low-temperature hydrothermal method, CuSO 4 · 5H 2 O as the source of copper, α-D- glucose as a reducing agent, synthesized at 100 ℃ spherical Cu 2 O grain cubic Cu 2 O single crystal particles synthesized under the conditions of 120 ° C; hydrothermal synthesis process of experimental parameters on the product of the reaction temperature, reaction time, concentration of precursors and additives; by XRD, TEM were used to characterize the resulting product. This series of experiments, the reaction mechanism of crystal growth mechanism. The two types of aggregation Cu 2 O growth unit and hydrothermal conditions under grain growth, and on this basis to discuss the different morphology of Cu 2 O crystal particles formation mechanism, and that in the crystallization process at the same time there are two mechanisms, i.e. diffusion mechanisms and gathering mechanisms, the spherical grains of the formation is due to the aggregation mechanism to play a major role in the growth process of the grains formed, and the formation of cubic monocrystalline is due to play a major role in the growth process of crystal grains due to the diffusion mechanism. Second, the design of the new route viable solvothermal synthesis to CuSO 4 · 5H 2 O, NaOH as raw materials, in anhydrous ethanol or alcohol-water mixed solvent changing the experimental conditions was prepared nanosized copper the monocrystalline and cuprous oxide nanorods, ethanol in the solvent at the same time also acts as a reductant of the reaction system. EDS, XRD, FESEM, TEM, HRTEM characterization methods were used to characterize the resulting product. The thermal synthesis process of the solvent the reaction temperature, reaction time, the influence of the content of water in the solvent, and the type of precursor and other experimental parameters on the resulting product, the results show that: the reaction temperature and the solvent in the water content is to determine the product phase major factor. A simple analysis of the experimental reaction mechanism of the formation mechanism of Cu nanocrystals and Cu 2 O nanorod formation mechanism. Third, by hydrothermal method to anhydrous FeCl 3 NiSO 4 · 6H 2 O and NaOH as raw materials, through the control of NaOH added amount, under the conditions of 180 ° C, respectively prepared fusiform α-Fe 2 O 3 nanocrystalline cubic phase NiFe 2 O 4 nanocrystals. XRD, TEM, HRTEM characterization methods were used to characterize the resulting product. The effects of the influence of the reaction temperature, reaction time, the amount of NaOH added and the type of precursor and other test parameters on the resultant was phase in the hydrothermal reaction process. The results showed that, of NaOH added in an amount to determine the main factors of the product phase. Discussed the reaction mechanism of the experimental analysis of the solution Cl - , the SO 4 2 - ions on the crystallization process.

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