溶液雾化氧化法制备超细Co_3O_4粒子及其性能表征

Preparation and characterization of ultrafine Co_3O_4 particles by solution spray-oxidation method

以氯化钴水溶液为原料采用雾化氧化法制备纯度较高的超细Co3O4粒子。采用热重-差热分析(TGA-DTA)对CoCl2·6H2O在空气中的热行为进行研究。由CoCl2·6H2O配制成原料溶液,以压缩空气为载气,采用内混合气流式喷嘴雾化溶液,并直接在竖立管式高温电阻炉内进行氧化反应,制备的产物通过X线衍射分析(XRD)、傅里叶红外光谱分析(FT-IR)和扫描电镜(SEM)等进行表征,同时对产物采用电位滴定法定量测定余氯含量,研究雾化氧化反应温度对产物的影响。实验结果表明:通过控制一定反应条件,氯化钴溶液采用直接雾化氧化法可以制备纯度较高的Co3O4粉体粒子;在雾化氧化过程中,反应温度对所得产物纯度、形貌与结晶度产生重要影响。

The ultrafine Co3O4 particles were synthesized using cobalt chloride solution as reactant by solution spray-oxidation method. The thermal behavior of CoCl2·6H2O in air atmosphere was studied by TGA-DTA analysis. The feed solution prepared by CoCl2·6H2O was sprayed using inner mixed air-nozzle and oxidized in the pipe high-temperature resistance furnace with compressed air as the carrier gas. The as-prepared products were characterized by X-ray diffraction analysis （XRD）, infrared spectroscopy （FT-IR） and scanning electron microscopy （SEM）, and the remaining chlorine content of the as-product was determined by potential titration. The reaction temperature of spray-oxidation process was investigated. The results show that by controlling the appropriate conditions, pure Co3O4 particles are prepared using cobalt chloride solution by spray-oxidation, and the reaction temperature has an important impact on Co3O4 particles purity, micro-structure morphology and crystallization during the process of spray-oxidation.