加料方式对超细氧化亚铜粉体分散性与粒度稳定性的影响

doi:10.3724/SP.J.1077.2012.00195

摘要/Abstract

摘要：

在不加任何添加剂和高反应物浓度的条件下, 用CuSO₄、NaOH、葡萄糖为原料制备了Cu₂O球形粉体. 利用扫描电镜和smileview软件对Cu₂O粉体进行了表征分析, 主要考察了加料方式对Cu₂O颗料的分散性与粒度稳定性的影响, 并根据Lamer模型初步探讨了其影响机理. 结果表明, 当采用先将NaOH溶液与CuSO₄溶液分步缓慢混合制备Cu(OH)₂作为铜源, 再加入葡萄糖还原Cu(OH)₂制备Cu₂O的加料方式时, Cu₂O颗粒按“爆发成核, 缓慢生长”的模式形成, 制得的Cu₂O粉体分散性高, 粒度稳定性好. 分散性高是由于缓慢的晶核生长有利于通过搅拌作用使初始晶核间的软团聚体再分散, 避免软团聚体进一步通过化学键合发展成为硬团聚. 粒度稳定性好的原因是将NaOH溶液分步缓慢加入到CuSO₄溶液中制备的前驱体Cu(OH)₂热稳定性好, 较好地保持了前驱体升温过程中铜源组分的单一性, 避免了还原过程中出现二次成核现象.

关键词: 氧化亚铜粉体, 葡萄糖还原, 分散性, 粒度控制

Abstract:

Spherical Cu₂O particles were prepared under high reaction concentration and without any additives using CuSO₄, NaOH, and glucose as raw materials. The products were characterized by XRD, SEM and smileview software. The effects of reactant mixing modes on dispersibility and size stability of Cu₂O particles were investigated. It is found that when Cu(OH)₂ was prepared by slowly mixing NaOH and CuSO₄ solutions at first step, and then reduced by adding glucose solution at second step, Cu₂O particles were formed by so-called “rapid nucleation- slow growth” model, and well-dispersed spherical Cu₂O particles with stable particle size were prepared. The good dispersibility of Cu₂O particles can be explained by the slow growth of Cu₂O particles, which allows the soft agglomeration of Cu₂O particles to be broken by stirring and prevented from becoming hard agglomeration through chemical bond between crystal nuclei. The good particle size stability can be explained by good thermal stability of Cu(OH)₂ which allows the precursor to keep oneness during heating up and prevents the renucleation in the reduction.

Key words: cuprous oxide powder, glucose reduction, dispersibility, particle size control

中图分类号:

TQ131

王岳俊, 周康根, 蒋志刚. 加料方式对超细氧化亚铜粉体分散性与粒度稳定性的影响[J]. 无机材料学报, 2012, 27(2): 195-200.

WANG Yue-Jun, ZHOU Kang-Gen, JIANG Zhi-Gang. Effects of Reactant Mixing Mode on Dispersibility and Particle Size Stability of Cuprous Oxide Particles[J]. Journal of Inorganic Materials, 2012, 27(2): 195-200.

图/表 8

图1 不同加料方式所得Cu2O粒子的SEM照片

Fig. 1 SEM images of Cu2O particles prepared by different reactant mixing modes

Table 1 Particle diameter of different Cu2O particles prepared by reactant mixing mode iii

Cu₂O particles	Diameter /μm	Standard deviation
a	0.85	0.231
b	0.75	0.211
c	1.35	0.230

Table 2 Particle diameter of different Cu2O particles prepared by reactant mixing mode iv

Cu₂O particles	Diameter /μm	Standard deviation
a	1.25	0.093
b	1.29	0.094
c	1.32	0.061

图2 加料方式iii的重复实验所得Cu2O颗粒的SEM照片以及粒径分布统计

Fig. 2 SEM images and particle size (a, b, c) for different tests distribution of Cu2O powders prepared by reactant mixing mode iii

图3 加料方式iv的重复实验所得Cu2O颗粒的SEM照片以及粒径分布统计

Fig. 3 SEM images and particle size (a, b, c) for different tests distribution of different Cu2O prepared by reactant mixing mode iv

图4 实验制备的Cu2O的XRD图谱

Fig. 4 XRD pattern of Cu2O powders prepared in the experiments

图5 晶体成核生长与溶质浓度的Lamer模型示意图[21]

Fig. 5 Lamer modle of nucleation and growth dependences with concentration[21]

图6 成核与生长速度的浓度关系曲线[21]

Fig. 6 Concentration dependences of nucleation and growth rates[21], where V is the total volume of the precipitate[21]

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