Wu Fan,Zhang Zhiguo,Suo Yange*.Preparation and properties of micron-sized silver powder by liquid phase reduction[J].Plating & Finishing,2023,(3):18-25.[doi:10.3969/j.issn.1001-3849.2023.03.003]
液相还原法制备微米级银粉及其性能研究
- Title:
- Preparation and properties of micron-sized silver powder by liquid phase reduction
- Keywords:
- liquid phase reduction ; micron-sized silver powder ; spherical ; flakes ; sintering temperature ; resistivity
- 分类号:
- TQ423
- 文献标志码:
- A
- 摘要:
- 为解决导电银浆用银粉烧结温度高和电阻率大的问题,以硝酸银( AgNO 3 )为原料,硫酸亚铁( FeSO 4 ·7H 2 O )为还原剂,柠檬酸( C 6 H 8 O 7 ·H 2 O )为添加剂制备银粉。采用正交实验探究不同工艺参数对银粉尺寸和形貌的影响。通过 X 射线衍射仪( XRD )、扫描电子显微镜( SEM )、四探针测试仪等对制备产物的晶体结构、形貌、烧结温度、电阻率等进行了表征。结果表明:改变柠檬酸的浓度可以调整银粉的尺寸大小和形貌,无柠檬酸条件下可以得到尺寸大小约为 3 μ m 的球形银粉,且在最佳烧结温度 550 ℃ 下电阻率为 2.39×10 -7 Ω ·m ;浓度为 0.015 mol·L -1 条件下可以得到尺寸大小约为 3.5 μ m 的片状银粉,且在最佳烧结温度 150 ℃ 下电阻率为 4.77×10 -6 Ω ·m ;浓度为 0.060 mol·L -1 条件下可以得到尺寸大小约为 0.5 μ m 的球形银粉,且在最佳烧结温度 250 ℃ 下电阻率为 1.92×10 -6 Ω ·m 。因此,本研究制备的银粉具有低的烧结温度和电阻率,可满足实际应用要求。
- Abstract:
- : To solve the problem of high sintering temperature and high resistivity of silver powder for conductive silver paste , silver powder is prepared with silver nitrate ( AgNO 3 ) as precursor , ferrous sulphate ( FeSO 4 ·7H 2 O ) as reducing agent and citric acid ( C 6 H 8 O 7 ·H 2 O ) as additive. The effect of different experimental parameters on the particle size and morphology of the silver powder was investigated using orthogonal tests. The crystalline structure , morphology , sintering temperature and resistivity of the prepared products were characterized by X-ray diffractometer ( XRD ), scanning electron microscope ( SEM ) and four-probe tester. The results show that the size and morphology of silver powder can be adjusted by changing the concentration of citric acid. A spherical silver powder with a particle size of about 3 μ m and a resistivity of 2.39×10 -7 Ω ·m at a sintering temperature of 550 °C was obtained without C 6 H 8 O 7 ·H 2 O. At a concentration of 0.015 mol·L -1 , flake silver powder with a particle size of about 3.5 μ m and a resistivity of 4.77×10 -6 Ω ·m at a sintering temperature of 150 °C was obtained. At a concentration of 0.060 mol·L -1 , a spherical silver powder with a particle size of about 0.5 μ m and a resistivity of 1.92×10 -6 Ω ·m at a sintering temperature of 250 °C was obtained. Therefore , the silver powder pre pared in this study has a low sintering temperature and resistivity , which can meet the requirements of practical applications.
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备注/Memo
收稿日期: 2022-07-20 修回日期: 2022-08-09 作者简介: 吴凡( 1998 —),男,硕士研究生, email : 1564723743@qq.com 通信作者: 索艳格( 1982 —),女,博士,副教授, email : suoyg@126.com 基金项目: 国家自然科学基金项目( 21805244 )