硫酸钡为内核的金红石型复合二氧化钛制备研究
[Abstract]:Rutile Ti O2 has a high dielectric constant. It is often used as a dielectric constant regulator in the preparation of high frequency microwave substrate materials. The direct use of micron Ti O2 will lead to a waste of titanium resources. In this paper, Ba SO4/ rutile Ti O 2 composites were prepared by using Ti Cl4 as titanium source and Ba SO4 as core. Ba SO4/ rutile type Ti O 2 composites were prepared under low calcination temperature by means of heating hydrolysis process, thus maximizing the utilization of resources. The process has the advantages of cheap raw material price, simple and controllable process and low energy consumption. It provides a theoretical and practical basis for the industrial production of rutile composite Ti O2. The main contents of this paper are as follows: (1) the preparation of micrometer near-spherical Ba SO4 core with narrow particle size distribution. Firstly, the direct precipitation method was used to select different precipitators with Ba Cl2 as the source of barium. The Ba SO4 core was prepared by homogeneous precipitation method and EDTA complex precipitation method. The effects of reaction temperature, reactant concentration, system pH, feeding rate, aging time on the particle size, particle size distribution and morphology of Ba SO4 were investigated. The results of SEM and particle size analysis show that only the Ba SO4 particles prepared by H2SO4 route and EDTA complexation precipitation method basically meet the requirements of the core of composite Ti O2 for substrate. However, the Ba SO4 obtained from the former has some shortcomings, such as wide particle size distribution and irregular morphology of larger particles. In contrast, the EDTA complex precipitation method can effectively control the particle size and morphology of the precipitate at the same time. The optimum conditions are as follows: at room temperature (25 oC), the complex system p H = 8o Ba Cl degree is 0.20 mol/L, complex ratio, and the optimum process conditions are as follows: at room temperature (25 oC), the complexation ratio of pH to Ba is 0.20 mol/L,. The concentration of Na2SO4 is 0.25 mol/L,Na2SO4, the feeding rate is 5 mL / min, the reaction time is 1 h. Under this reaction condition, the average particle size of spherical Ba SO4, with uniform particle size distribution is 1.2 渭 m without aging. Then, the Ti O 2 coating effect of Ba SO4 core obtained by direct precipitation method and EDTA complexation precipitation method was compared. The results showed that the Ba SO4 prepared by EDTA complex precipitation method was more favorable to Ti O 2 coating. (2) the preparation of rutile composite Ti O _ 2 first investigated the effects of initial pH, hydrolysis temperature, sulfate ion and calcination temperature on the crystal morphology of single Ti O _ 2 particles. The process of preparing rutile Ti O 2 by Ti Cl4 heating hydrolysis was determined. On the basis of the above technology, the effects of hydrolysis time, hydrolysis temperature, amount of Ti Cl4 and concentration of titanium in hydrolysis mixture on the coating effect of Ba SO4 prepared by EDTA complexation precipitation under the optimum conditions were further investigated. Finally, the optimum conditions of preparing Ba SO4/ rutile Ti O 2 composite powder by heating hydrolysis method were determined: the initial pH of hydrolysis system was 0.1, and the concentration of titanium in hydrolysis mixture was 0.20 mol/L,. The amount of Ti Cl4 was 2, the hydrolysis temperature was 80 oC, the hydrolysis time was 1.5 h, the calcination temperature was 500 oC, the calcination time was 2 h. Under this condition, the composite Ti O has rutile coating with high coating efficiency, uniform and dense coating layer, good spherical morphology and good dispersion.
【学位授予单位】:江南大学
【学位级别】:硕士
【学位授予年份】:2015
【分类号】:TQ134.11
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