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以含铜废液为原料制备Al2O3弥散强化Cu粉的工艺研究
Process study of Al2O3 dispersion strengthened copper powders prepared with waste cupric liquor
【摘要】 以酸碱含铜刻蚀废液为原料,采用酸碱中和-过滤-H2SO4溶解制备出一定浓度的含铜溶液,并向溶液中添加可溶性铝盐,最终采用络合共沉淀-煅烧-H2还原的方法制备出质量分数2%的纳米Al2O3弥散强化Cu粉末。采用火焰原子吸收光谱法测定过滤液中Cu2+的含量,研究了酸碱混合比对Cu2+提取效率的影响;采用扫描电镜、X射线衍射仪分析了共沉淀前驱体粉末、Al2O3-CuO复合粉末、Al2O3-Cu粉末、Al2O3弥散相的粒度、形貌及组成;并采用TG-DTA试验对粉末制备过程中的煅烧及H2还原过程进行了分析。结果表明:酸碱含铜废液的体积比为2∶3时,中和反应进行最充分,Cu2+的提取率达到96.75%(质量分数);沉淀剂采用瞬间加入方式,得到的前驱体粉末细小均匀、无团聚;最佳的煅烧温度为500℃,H2还原温度为550℃,制备的弥散相分布均匀,粒度小于200 nm;经弥散相萃取试验观察,进一步证明弥散相为纳米Al2O3。
【Abstract】 Using acidic and alkaline waste cupric liquor as raw material,the copper solution was prepared with the processes of acid and alkali neutralization,filtration and sulfuric acid dissolution. Then,the soluble aluminum salt was added into the copper solution. Finally,the nano-Al2O3-dispersed strengthening copper-based powders with 2%(mass percent) alumina were prepared with the methods of complex chemical co-precipitation,calcination and hydrogen reduction. The Cu2+content in filtrate was measured by flame atomic absorption spectrometry,and the influences of mixing ratio of acidic and alkaline waste cupric liquor on the Cu2+extraction efficiency were studied. The particle size,morphology and composition of precursor powder,Al2O3-CuO composite powder,Al2O3-Cupowder and Al2O3 dispersed phase were analyzed through scanning electron microscope and X-ray diffraction. The calcination and hydrogen reduction processes were analyzed with TG-DTA test. The results show that,neutralization reaction is completed fully when acidic and alkaline waste cupric liquor has the volume ratio of 2 to3,and Cu2+extraction efficiency is 96.75%(mass percent). Precursor powder with fine particle size and no agglomeration is obtained by the way of rapid precipitator addition. The optimum calcination and hydrogen reduction temperature is 500 ℃ and 550 ℃,respectively. The dispersion phase distributes uniformly and the particle size is less than 200 nm. The extraction experiments prove that the dispersed phase is nano Al2O3.
【Key words】 waste cupric liquor; co-precipitation; dispersion strengthening; nano Al2O3; copper recovery;
- 【文献出处】 粉末冶金工业 ,Powder Metallurgy Industry , 编辑部邮箱 ,2017年02期
- 【分类号】TF123.74
- 【被引频次】2
- 【下载频次】64