超临(lin)界二氧化(hua)碳电(dian)(dian)(dian)(dian)(dian)镀(du)装置(zhi)，用(yong)行(xing)超临(lin)界二氧化(hua)碳电(dian)(dian)(dian)(dian)(dian)镀(du)钴(gu)薄(bo)膜(mo)制备(bei)及力学和磁(ci)学性能研究，电(dian)(dian)(dian)(dian)(dian)镀(du)是通(tong)过(guo)电(dian)(dian)(dian)(dian)(dian)解质中金(jin)属(shu)离子的电(dian)(dian)(dian)(dian)(dian)化(hua)学反应，在基(ji)材上形成(cheng)(cheng)金(jin)属(shu)涂层(ceng)的薄(bo)膜(mo)生长(zhang)工艺(yi)之(zhi)一，也叫电(dian)(dian)(dian)(dian)(dian)沉积。电(dian)(dian)(dian)(dian)(dian)镀(du)过(guo)程主要包括(kuo)将待(dai)镀(du)物(wu)（阴极(ji)）浸入含有(you)电(dian)(dian)(dian)(dian)(dian)解质和辅(fu)助电(dian)(dian)(dian)(dian)(dian)极(ji)（阳极(ji)）的容器中，然后将两个电(dian)(dian)(dian)(dian)(dian)极(ji)连(lian)接到外部电(dian)(dian)(dian)(dian)(dian)源(yuan)以使电(dian)(dian)(dian)(dian)(dian)流流动。待(dai)镀(du)物(wu)与电(dian)(dian)(dian)(dian)(dian)源(yuan)负极(ji)相(xiang)连(lian)，使金(jin)属(shu)离子还原为金(jin)属(shu)原子，最终在表面形成(cheng)(cheng)沉积物(wu)。可控(kong)制电(dian)(dian)(dian)(dian)(dian)镀(du)参数，如电(dian)(dian)(dian)(dian)(dian)解质的成(cheng)(cheng)分、电(dian)(dian)(dian)(dian)(dian)流密度、浴温、pH 值等以获得所(suo)需的镀(du)层(ceng)性能。

超临界二(er)氧化碳电(dian)(dian)(dian)(dian)(dian)(dian)镀(du)装置，如今，电(dian)(dian)(dian)(dian)(dian)(dian)镀(du)已在从冶金和(he)(he)重工(gong)程(cheng)(cheng)工(gong)业到微电(dian)(dian)(dian)(dian)(dian)(dian)子(zi)和(he)(he)纳(na)米技术的各(ge)种(zhong)技术领域(yu)中经常(chang)用(yong)于实际科研生产中。电(dian)(dian)(dian)(dian)(dian)(dian)镀(du)通(tong)常(chang)以两种(zhong)控(kong)制(zhi)模(mo)式进行(xing)：恒(heng)电(dian)(dian)(dian)(dian)(dian)(dian)位(wei)法(fa)和(he)(he)恒(heng)电(dian)(dian)(dian)(dian)(dian)(dian)流(liu)法(fa)。对(dui)恒(heng)电(dian)(dian)(dian)(dian)(dian)(dian)位(wei)法(fa)，除(chu)了(le)阳(yang)极(ji)(ji)（工(gong)作电(dian)(dian)(dian)(dian)(dian)(dian)极(ji)(ji)）和(he)(he)阴极(ji)(ji)（对(dui)电(dian)(dian)(dian)(dian)(dian)(dian)极(ji)(ji)）外，还需要参比(bi)电(dian)(dian)(dian)(dian)(dian)(dian)极(ji)(ji)来控(kong)制(zhi)金属离子(zi)的还原电(dian)(dian)(dian)(dian)(dian)(dian)位(wei)。使(shi)用(yong)此方法(fa)可精(jing)确控(kong)制(zhi)阴极(ji)(ji)和(he)(he)参比(bi)电(dian)(dian)(dian)(dian)(dian)(dian)极(ji)(ji)之间的电(dian)(dian)(dian)(dian)(dian)(dian)位(wei)差(cha)；而在电(dian)(dian)(dian)(dian)(dian)(dian)镀(du)过程(cheng)(cheng)中，电(dian)(dian)(dian)(dian)(dian)(dian)解质(zhi)的形态变(bian)化或(huo)成(cheng)分变(bian)化，电(dian)(dian)(dian)(dian)(dian)(dian)流(liu)密度可能会发生变(bian)化，导致难以估(gu)计电(dian)(dian)(dian)(dian)(dian)(dian)镀(du)层(ceng)厚度和(he)(he)电(dian)(dian)(dian)(dian)(dian)(dian)流(liu)密度效(xiao)率。对(dui)恒(heng)电(dian)(dian)(dian)(dian)(dian)(dian)流(liu)方法(fa)，在电(dian)(dian)(dian)(dian)(dian)(dian)镀(du)过程(cheng)(cheng)中使(shi)用(yong)固定的电(dian)(dian)(dian)(dian)(dian)(dian)流(liu)密度，并且可通(tong)过简单(dan)的电(dian)(dian)(dian)(dian)(dian)(dian)源(yuan)产生。此方法(fa)只需要阳(yang)极(ji)(ji)和(he)(he)阴极(ji)(ji)，它在工(gong)业上(shang)被广泛使(shi)用(yong)，特别是(shi)用(yong)于大(da)型(xing)物体(ti)的电(dian)(dian)(dian)(dian)(dian)(dian)镀(du)。

超临界二氧化(hua)碳电镀装置，钴(gu)及钴(gu)合(he)金(jin)因其优(you)越磁(ci)性(xing)(xing)(xing)，大量(liang)应(ying)用(yong)于高性(xing)(xing)(xing)能(neng)磁(ci)性(xing)(xing)(xing)材料，在电(dian)(dian)子信息(xi)领域起着非(fei)常(chang)重(zhong)要(yao)的(de)作用(yong)，随着电(dian)(dian)子设备小型化(hua)、轻量(liang)化(hua)，钴(gu)薄膜(mo)磁(ci)制动(dong)器等可用(yong)于微(wei)(wei)电(dian)(dian)机系统。以钴(gu)薄膜(mo)为主要(yao)研究(jiu)对(dui)象，采(cai)用(yong)超临界（15MPa，40℃）二(er)氧(yang)化(hua)碳电(dian)(dian)镀，对(dui)比亚临界（15MPa，30℃）、高压（15MPa，25℃）二(er)氧(yang)化(hua)碳和(he)常(chang)规电(dian)(dian)镀，制备了 FCC 和(he) HCP 双相电(dian)(dian)镀钴(gu)薄膜(mo)，为获(huo)得无缺(que)陷、表面质量(liang)良(liang)好，优(you)异(yi)力(li)(li)学和(he)磁(ci)性(xing)(xing)(xing)的(de)钴(gu)薄膜(mo)，研究(jiu)了钴(gu)薄膜(mo)晶(jing)体结构、晶(jing)粒(li)尺(chi)寸与微(wei)(wei)压缩力(li)(li)学性(xing)(xing)(xing)能(neng)、磁(ci)性(xing)(xing)(xing)的(de)关(guan)系。主要(yao)通(tong)过(guo) XRD、SEM、TEM、AFM、VSM 和(he) MFM 测试等表征手段对(dui)材料的(de)物相，结构，形(xing)貌，磁(ci)性(xing)(xing)(xing)，结合(he)微(wei)(wei)压缩和(he)分子动(dong)力(li)(li)学模拟微(wei)(wei)压缩、纳米压痕、维氏硬(ying)度等试验，对(dui)力(li)(li)学性(xing)(xing)(xing)能(neng)、磁(ci)性(xing)(xing)(xing)进行(xing)分析。

超临界二氧化(hua)碳电镀装置，水(shui)电(dian)(dian)解质电(dian)(dian)镀钴薄(bo)膜：含水(shui)电(dian)(dian)解质中(zhong)，酸性(xing)条件下(xia) 298K 时(shi)，Co2+/Co 电(dian)(dian)极电(dian)(dian)势为-0.28 V，不需络合物(wu)形成络合离子即可在水(shui)溶液中(zhong)电(dian)(dian)镀钴薄(bo)膜。电(dian)(dian)镀钴薄(bo)膜一(yi)般从从含有(you)氯化物(wu)、硫酸盐等(deng)水(shui)溶液的不同(tong)电(dian)(dian)解槽中(zhong)电(dian)(dian)镀获得[25]，反(fan)(fan)应式(shi)如下(xia)：Co2+ + 2e− → Co ↓ (s) ； 水(shui)电(dian)(dian)解质中(zhong)，水(shui)可电(dian)(dian)离为氢(qing)(qing)氧根和氢(qing)(qing)离子，同(tong)时(shi)也会发生副(fu)反(fan)(fan)应，如下(xia)：2H+ + 2e− → H2 ↑ (g) 。

超(chao)临界二氧化电(dian)(dian)镀(du)前处理(li)(li)铜片(pian)用(yong) 10 wt%的脱脂溶液(ye)和(he) 10 wt%的 HCl 溶液(ye)电(dian)(dian)镀(du)过程(cheng)之前分(fen)别处理(li)(li) 70 秒(miao)和(he) 10 秒(miao)，每道(dao)工序处理(li)(li)后使用(yong)纯水浸泡清洗后，安装(zhuang)于高(gao)(gao)压(ya)釜(fu)盖上，电(dian)(dian)解质组成为 350 g/L CoSO4·7H2O、45 g/L CoCl2·6H2O 和(he) 40 g/L H3BO3，电(dian)(dian)解质 pH 值为 3.5，无表面活性(xing)剂。将 40 mL 电(dian)(dian)解质、阴(yin)阳(yang)极放入高(gao)(gao)压(ya)釜(fu)中，关闭高(gao)(gao)压(ya)釜(fu)，加热(re)高(gao)(gao)压(ya)釜(fu)中电(dian)(dian)解质温度至(zhi)为 40℃，压(ya)力(li)容(rong)器(qi)注入 CO2，利用(yong)背(bei)压(ya)阀调节压(ya)力(li)至(zhi) 15MPa，体积分(fen)数(shu)为 20% CO2，接通(tong)导(dao)线，开启直流稳压(ya)电(dian)(dian)源进(jin)行电(dian)(dian)镀(du)。使用(yong) 5、10、12 和(he) 15 A/dm2 (ASD) 的不同电(dian)(dian)流密度电(dian)(dian)镀(du)。