溶液燃烧法合成Co-Cu-Mn-Fe系纳米晶黑色陶瓷色料及性能研究

发布时间：2018-09-07 11:38

【摘要】：由第四周期过渡金属元素氧化物复合而成的黑色陶瓷色料,其着色力不仅与各金属离子含量有关,还与色料的颗粒粒径及粒径分布密切相关,制备粒径小且颗粒粒度分布窄的高着色力黑色色料一直是技术难点。本论文主要以硝酸铁、硝酸钴、硝酸锰、硝酸铜及DL-丙氨酸为原料,采用溶液燃烧法制备Co-Cu-Mn-Fe系纳米晶黑色色料,并考察其物化性能。首先,本论文通过优化试验获取了Co-Cu-Mn-Fe系黑色色料,同时,考察了点火温度、燃料加入量的影响。结果表明:当燃料与氧化剂为化学计量比(推进剂化学理论计算)、点火温度为400℃和Co2+:Cu2+:Mn2+:Fe3+为0.5:0.5:1:1时,得到平均晶粒粒径和平均颗粒粒径分别为16.4 nm、1μm的纳米晶黑色色料,其L*、a*、b*值分别为39.95、0.25、0.16。升高点火温度有利于色料合成,但不利于得到分散性好的色料颗粒。燃料在化学计量比体系下得到产物的分散性较贫燃体系和富燃体系条件下得到产物的分散性好,且颗粒粒径较小。其次,本论文系统地研究了惰性盐种类、惰性盐加入量及硝酸铵对溶液燃烧反应过程及燃烧产物性能的影响。结果表明:在未加盐、氯化锂、氯化钠、氯化钾体系下得到产物的颗粒粒径分别为1μm、650 nm、400 nm和300 nm,相应的比表面积分别为19.75 m2/g、32.46 m2/g、142.50 m2/g和131.66 m2/g。产物的颗粒粒径和比表面积相差较大的原因是与惰性盐溶解度有关,惰性盐的溶解度大,得到产物的颗粒粒径大、比表面积小;反之亦然。加入适量的惰性盐可获得小晶粒粒径和小颗粒粒径的目标产物,加入过量的惰性盐不利于反应进行,不能得到目标产物。加入硝酸铵不仅使溶液燃烧产物的晶粒粒径变大,还使产物的颗粒团聚严重、颗粒粒径变大。再次,本论文还考察了Co-Cu-Mn-Fe系纳米晶黑色色料应用在锌釉、镁釉、含钡透明釉、含钡亚光釉及高硼釉中的呈色性能。结果表明:色料在锌釉和镁釉中呈色不稳定,在钡釉和硼釉中显黑色且呈色好,且在高硼釉中着色性能最好,这说明色料宜用于钡釉和硼釉中,不宜应用于锌釉和镁釉中。最后,本论文给出了根据上述试验结果所获得的结论以及今后工作的展望。
[Abstract]:The coloring power of black ceramic pigments composed of transition metal element oxides in the fourth cycle is related not only to the content of metal ions, but also to the particle size and particle size distribution of the pigments. It has been a technical difficulty to prepare black pigments with small particle size and narrow particle size distribution. In this paper, Co-Cu-Mn-Fe nanocrystalline black color was prepared by solution combustion method with Fe, Co nitrate, mn nitrate, Cu nitrate and DL- alanine as raw materials, and their physicochemical properties were investigated. Firstly, the black color of Co-Cu-Mn-Fe system was obtained by optimization test, and the effects of ignition temperature and fuel addition were investigated. The results show that when the stoichiometric ratio of fuel to oxidant (theoretical calculation of propellant chemistry), ignition temperature is 400 鈩，

本文编号：2228153