微波水热合成纳米CoAl_2O_4色料的工艺研究

Study on Microwave Hydrothermal Synthesis Technique for CoAl_2O_4 Nano Pigments

以Co Cl2·6H2O和Al Cl3为起始原料,Na OH为沉淀剂,用微波水热法合成了纳米Co Al2O4钴蓝色料。分别研究了填充度、p H值、n Co/n Al、起始原料浓度等对合成色料物相组成、颗粒大小与形貌和呈色的影响。用XRD、TEM和色度仪对样品进行了表征。结果表明：Co Cl2·6H2O和Al Cl3的浓度分别为0.15 mol/L和0.30 mol/L,在填充度为50%、p H值为13、n Co/n Al为1∶2的条件下,230℃微波水热反应3 h可制得呈色较好的尖晶石型钴蓝色料;其形态为八面体,晶型完整、发育良好,粒径多为70-80 nm左右。

Co Al2O4 nano cobalt blue pigments were synthesized by a microwave hydrothermal approach using Co Cl2·6H2O and Al Cl3 as starting materials and Na OH as precipitant,respectively. The influence of filling factors,p H values,n Co / n Al ratios and the concentrations of starting materials on the phase composition,particle size and morphology and coloration of the as-prepared samples was systematically investigated. The samples were characterized using XRD、TEM and colorimetric analysis. The results indicate that spinel type cobalt blue pigments were achieved by microwave hydrothermal treatment at 230℃ for 3 h using Co Cl2·6H2O and Al Cl3 with concentration of 0. 15 mol / L and 0. 30 mol / L,filling factor of 50%,p H value of 13 and n Co / n Al of 1∶ 2,respectively. The as-prepared pigment crystals are of octahedral shape with high perfection and most of the sizes are of 70-80 nm.