(1. 東北大學(xué) 材料各向異性與織構(gòu)教育部重點(diǎn)實(shí)驗(yàn)室,沈陽(yáng) 110819;
2. 東北大學(xué) 中荷生物醫(yī)學(xué)與信息工程學(xué)院,沈陽(yáng) 110169)
摘 要: 研究以抗壞血酸為還原劑、采用液相還原法制備微納米銅粉過(guò)程中pH值、混合方式和混合速率對(duì)銅粉形貌和粒徑的影響。采用X射線衍射儀(XRD)和掃描電子顯微鏡(SEM)對(duì)合成產(chǎn)物進(jìn)行表征。結(jié)果表明:液相反應(yīng)溶液體系的pH值對(duì)反應(yīng)產(chǎn)物的物相及其形貌有決定性的影響;當(dāng)pH值控制為3~8時(shí),還原產(chǎn)物為純銅相;當(dāng)pH為9~12時(shí),產(chǎn)物是金屬Cu與Cu2O混合相;當(dāng)pH值高于13時(shí),還原產(chǎn)物為Cu2O相;反向滴定即CuSO4溶液向抗壞血酸溶液中滴定時(shí)制備的銅粉顆粒粗大呈微米級(jí),正向滴定獲得的銅粉細(xì)小呈亞微米級(jí);以快速傾倒方式獲得的銅粉顆粒尺寸分布窄且分散性良好,以慢速滴注獲得的銅粉的尺寸與形狀與前者的相近,但分布不均勻。
關(guān)鍵字: 銅粉;抗壞血酸;混合方式;混合速率
(1. Key Laboratory of Anisotropy and Texture of Materials, Ministry of Education, Northeastern University, Shenyang 110819, China;
2. Sino-Dutch Biomedical and Information Engineering School, Northeastern University, Shenyang 110169, China)
Abstract:The micro/nano copper powders were prepared by liquid phase reduction using ascorbic acid as reducing agent. Meanwhile, the effects of pH value, mixing ways and mixing rates on the characteristics of copper powders were discussed. The as-synthesized products were characterized by X-ray diffractometry (XRD) and scanning electron microscopy (SEM). The results show that the pH value of reactive solution system has key effect on phase type and morphology of the products. Pure Cu phase is obtained in the pH range of 3-8, and then Cu and Cu2O mixed phases are obtained, finally it is pure Cu2O as the pH exceeds 13. The particle size of copper powders prepared by reverse titration is large and in micron grade. Conversely, it is small and in submicron size. The distribution of Cu powder size obtained by dump is narrow and well dispersed compared to that of the powder prepared by slow dripping.
Key words: Cu powder; ascorbic acid; mixing mode; mixing rate


