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以酸碱含铜刻蚀废液为原料,采用酸碱中和-过滤-H_2SO_4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-H_2还原的方法制备出质量分数2%的纳米Al_2O_3弥散强化Cu粉末。采用火焰原子吸收光谱法测定过滤液中Cu~(2+)的含量,研究了酸碱混合比对Cu~(2+)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、Al_2O_3-CuO复合粉末、Al_2O_3-Cu粉末、Al_2O_3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H_2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,Cu~(2+)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℃,H_2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Al_2O_3。
The copper-containing solution with acid-base copper-containing etching solution was prepared by acid-base neutralization-filtration-H 2 SO 4 dissolution and the soluble aluminum salt was added to the solution. Finally, complex coprecipitation-calcination-H 2 Reduction method to prepare a mass fraction of 2% nano Al 2 O 3 dispersion strengthened Cu powder. The content of Cu 2+ in the filtrate was determined by flame atomic absorption spectrometry. The effect of acid-base mixing ratio on the extraction efficiency of Cu 2+ was studied. The effect of coprecipitation precursor Powder, Al 2 O 3-CuO composite powder, Al 2 O 3-Cu powder and Al 2 O 3 dispersed phase were prepared. The calcination and H 2 reduction process in powder preparation were analyzed by TG-DTA. The results showed that when the volume ratio of acid-base copper-containing waste liquid was 2: 3, the neutralization reaction was the best, the extraction rate of Cu 2+ reached 96.75% (mass fraction); the precipitant was added in an instant, The precursor powders were fine and homogeneous without agglomeration. The optimal calcination temperature was 500 ℃ and the H 2 reduction temperature was 550 ℃. The dispersed phase was uniform and the particle size was less than 200 nm. The dispersion phase was further confirmed by Nano-Al_2O_3.