酸性鍍銅工藝及鍍層特性
(華南理工大學(xué) 化學(xué)與化工學(xué)院 廣東省高等學(xué)校新能源技術(shù)重點(diǎn)實(shí)驗(yàn)室, 廣州 510640)
摘 要: 鋰離子電池用負(fù)極集流體銅箔材料目前主要采用電沉積法制備。為制備良好的電解銅箔，采用不同電鍍工藝參數(shù)，在基于三乙醇胺(TEA)和乙二胺四乙酸二鈉(EDTA·2Na)雙絡(luò)合體系的CuSO4/H2SO4溶液中進(jìn)行鍍銅工藝研究。通過線性掃描、循環(huán)伏安、SEM 和XRD手段對鍍液性質(zhì)、鍍層微觀形貌和結(jié)構(gòu)進(jìn)行測定和表征，并進(jìn)行鍍層質(zhì)量重復(fù)性實(shí)驗(yàn)。結(jié)果表明：選擇含P 0.1%的磷銅作為陽極，采取機(jī)械攪拌鍍液的方式，在CuSO4·5H2O為300 g/L、H2SO4為90 g/L、Cl−為40~80 mg/L、TEA為3.5 g/L和EDTA·2Na為5 g/L中適量添加劑P的鍍液中，以電流密度為490 mA/cm2，鍍液溫度為40~60 ℃，施鍍5~10 min能得到良好鍍層；添加劑明顯降低循環(huán)伏安陰極峰電流，Cu2+的還原速度減慢；添加劑提高鍍層表面的結(jié)晶細(xì)化程度，使晶體顆粒變小，致密性提高，鍍層質(zhì)量變好，整平作用明顯，Cu鍍層呈現(xiàn)(111)晶面擇優(yōu)取向；鍍速可達(dá)19.4 mg/min，鍍層質(zhì)量有很好的重現(xiàn)性。
關(guān)鍵字: 電解銅箔；TEA；EDTA·2Na；鍍速；槽電壓；擇優(yōu)取向
coating properties based on system of TEA and EDTA·2Na
（Key Laboratory of New Energy Technology for Guangdong Universities, School of Chemistry and Chemical Engineering,
South China University of Technology, Guangzhou 510640, China）
Abstract:The copper foils for the anode current collectors of lithium-ion battery were prepared by electrodeposition. In order to obtain better electrodeposited copper foils, considering different electroplating technology parameters, the copper electrodepositing process based on the system of TEA and EDTA·2Na was studied in CuSO4/H2SO4 electrolytes. The morphology and structure of coating were characterized by SEM and XRD, and the property of electrolyte was tested by linear sweep voltammetry and cyclic voltammetry. The reproducibility of coating was also tested. The results show that a good coating can be got in the better condition that is as follows: 0.1% phosphor bronze as the anode, mechanical stirring, CuSO4·5H2O (300 g/L), H2SO4(90 g/L), Cl−(40−80 mg/L), TEA(3.5 g/L), EDTA·2Na (5 g/L), appropriate amount of additive P, current density (490 mA/cm2), bath temperature(40−60 ℃) and deposition time(5−10 min). The additives remarkably decrease the cathode peak current of cyclic voltammetry and slow down the reduction rate of copper ions. The additives can improve the crystallization refinement of the coating, reduce crystal particles and raise the compactness, owing to its significantly leveling effect. The copper coating has an orientation along (111) crystal plane. The deposition rate reaches up 19.4 mg/min, and the coating quality has good reproducibility.
Key words: electrodeposited copper foil; TEA; EDTA·2Na; deposition rate; bath voltage; preferred orientation
