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机构地区:[1]华南理工大学材料科学与工程学院,广州510640 [2]佛山市质量计量监督检测中心,广东佛山528225
出 处:《硅酸盐学报》2015年第4期411-417,共7页Journal of The Chinese Ceramic Society
基 金:广东省教育部产学研结合项目(2012B091000026)
摘 要:以硝酸钴、硝酸铜、硝酸锰和硝酸铁为氧化剂及DL-丙氨酸为燃料,采用溶液燃烧法合成(Co_(0.5)Cu_(0.5))(MnFe)O_4纳米晶黑色陶瓷色料。采用同步热分析仪对反应前驱体进行热性能分析,采用X射线衍射仪、扫描电子显微镜、分光光度计等手段对样品的物相、晶粒尺寸、颗粒形貌及尺寸、色度进行表征。结果表明:当丙氨酸与硝酸盐类之比按推进剂化学理论计算为化学计量比时,反应体系在230℃可以完成反应,且点火温度越高越有利于产物形成;当丙氨酸与硝酸盐类之比为化学计量比和点火温度为400℃时,样品的结晶度好,其晶粒和颗粒平均粒径分别为16.4nm和1μm,同时,样品无需后续煅烧在透明基础釉中有良好的着色力。另外,还研究了加入惰性盐氯化钾对合成产品的影响,结果表明,加入氯化钾合成样品的分散性好,其晶粒和颗粒平均粒径分别为10.8nm和300 nm,同时,其着色力比未加氯化钾合成样品的着色力有较大提高。Nanocrystalline(Co_(0.5)Cu_(0.5))(MnFe)O_4 black ceramic pigment was synthesized by a solution combustion method with cobalt nitrate,copper nitrate,manganese nitrate,ferric nitrate as oxidants and DL-alanine as an organic fuel.The precursor was analyzed by thermogravimetry-differential scanning calorimetry.The phase structure,crystallite/particle size,morphology and color property were characterized by X-ray diffraction,scanning electron microscopy and spectrophotometry,respectively.The results show that the reaction can be completed at 230℃ at the stoichiometric ratio of fuel to nitrates,and a higher ignition temperature can favor the product formation.The pigment product with the crystallite size of 16.4 nm and the particle size of 1 μm was obtained at the stoichiometric ratio of fuel to nitrates and 400℃.In addition,the influence of potassium chloride on the synthesis of the nanocrystalline pigment was also investigated.It is indicated that the pigment product with the crystallite size of 10.8 nm and the particle size of 300 nm obtained in the presence of potassium chloride is smaller than and more dispersive than that in the absence of potassium chloride in the synthesis.The pigment synthesized with potassium chloride has a higher tinting strength in ceramic glazes.
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