正交设计法优化高分散超细银粉的制备工艺

Optimization for Preparation Technique of Highly Dispersive Ultrafine Silver Powders by Orthogonal Design

摘要:

以AgNO3为银源，抗坏血酸为还原剂，通过液相还原法制备了超细银粉。运用L25(56)的正交试验设计，考察了AgNO3浓度、抗坏血酸浓度、分散剂种类、分散剂用量、溶液pH值及反应温度对超细银粉的分散性及粒度的影响。分析得出制备超细银粉的优化条件：AgNO3浓度为0.15 mol·L-1，抗坏血酸浓度为0.40 mol·L-1，油酸为分散剂，分散剂用量为8%（相对AgNO3质量），pH值为4，反应温度为50 ℃。在优化的实验条件下，制备出高分散近球形的超细银粉，其平均粒度为0.89 μm。并运用SEM、XRD对其进行了表征。

Abstract:

Using ascorbic acid (C6H8O6) as the reducing agent and AgNO3 as the source of Ag, the ultrafine silver powders were prepared by a liquid phase reduction method. By means of the orthogonal design method of six factors and five levels, the effects of the following factors on the dispersion and particles size of silver powders were studied, such as the concentration of AgNO3, the concentration of C6H8O6, the selection of dispersers, the doses of disperser, pH and the temperature. The optimized conditions for the ultrafine silver powders preparation were obtained. The pure ultrafine silver powders with near-spherical shape and mean diameter of 0.89 μm can be synthesized under the conditions of AgNO3 concentration of 0.15 mol·L-1, C6H8O6 concentration of 0.40 mol·L-1, oleic acid (C18H34O2) as disperser, C18H34O2/AgNO3 mass ratio of 8:100, pH=4 and at 50 oC. The ultrafine silver powders were characterized by scanning electron microscopy (SEM) and XRD