CN112323099A - 一种镍铬合金表面制备有抗氧化耐腐蚀涂层的惰性阳极 - Google Patents
一种镍铬合金表面制备有抗氧化耐腐蚀涂层的惰性阳极 Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
- C25C3/08—Cell construction, e.g. bottoms, walls, cathodes
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- C22C19/03—Alloys based on nickel or cobalt based on nickel
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Abstract
本发明适用于铝等一些电解工业，涉及一种镍铬合金表面制备有抗氧化耐腐蚀涂层的惰性阳极。本发明提供一种金属基体表面制备有金属氧化物涂层的惰性阳极及其制备方法，适用于800℃及以下的电解质体系。该惰性阳极在作为铝电解的阳极时，阳极表面会有氧气生成，这样可以消除CO2的排放，进而可以保护环境，符合当下的节能减排的宗旨。由于本发明通过在GH3030表面电镀制备的Ni‑Fe合金涂层在高温下进行氧化后，最后阳极的外层形成含有尖晶石以及三氧化二铬的氧化层，且故呈现出较好的好的抗冰晶石熔盐腐蚀性能和抗高温氧化性能，且导电性良好。
Description
技术领域
本发明涉及有色金属冶金熔盐电解领域，尤其涉及铝电解及其惰性金属阳极的制备。
背景技术
目前铝电解工业主要使用的原铝生产方法是Hall-Héorult法，Hall-Héorult法是一种通过电解氧化铝-冰晶石熔体来生产原铝的方法。该方法的阳极是碳素阳极，其生产原铝的电解过程中发生的反应为：2Al2O3＋3C→4Al＋3CO2。
碳素阳极用于铝电解工业中会有一些问题存在：一方面在电解铝过程中碳阳极会由于参与反应而被消耗，在工作一段时间以后需要对碳阳极进行更换，大量优质石墨被消耗，这就增加了企业的成本，而且使得工人劳动强度变大。而且在频繁的更换阳极过程中会对电解槽的热平衡造成一定的影响。另一方面铝电解时会产生大量CO2和CO氟炭化合物等，在预焙炭阳极过程中还有大量硫化物和碳氮化物生成，既恶化了工作条件又污染了环境。另外，使用碳素阳极电解铝时电解过程中会发生阳极效应。
由于炭阳极的种种弊端，国内外对惰性阳极进行了众多研究，希望以此来解决以碳素材料作为阳极所存在的种种缺陷。惰性阳极指的是在冰晶石熔盐中不消耗和微消耗的阳极。在铝电解过程中使用惰性阳极可以大大改善以上缺陷，其电解过程的反应式为：2Al2O3→4Al+3O2。可以看出相比于传统的碳素阳极，惰性阳极有着一些显著的优点：一方面由于惰性阳极在铝电解工程中不被消耗或者微量消耗，就不必频繁更换阳极，这样企业的成本就节约了，同时工人劳动强度也会降低，而且还易维持电解槽的热平衡，这对于生产的连续性和自动化有利。另外，使用惰性阳的电解过程中，有氧气的生成，这就不会污染环境，也改善了工人的工作条件，也不必再预焙炭阳极，这就避免了排放大量污染的气体。
尽管惰性阳极材料的研究已经进行的很广泛深入，但仍未有惰性阳极材料成功应用于实际生产中。GH3030镍铬基合金在高温下具有很好的抗氧化性，而且成分简单，但若直接使用该合金的用于电解，需要提高其抗冰晶石熔盐腐蚀的性能。
发明内容
(一)要解决的技术问题
本发明的目的是针对以上所述的不足，提供一种用于铝电解工业的惰性金属阳极，以解决当前铝电解工业中排污量大和能耗高的问题。
(二)技术方案
本发明的目的是通过以下技术方案实现的。
一种镍铬合金表面制备有抗氧化耐腐蚀涂层的惰性阳极，适用于铝电解中作为阳极，是由GH3030合金基体以及合金基体表面的复合涂层组成。
所述的金属基表面制备有金属复合涂层的金属惰性阳极，其特征在于：所述GH3030合金的质量百分比成分20.23% Cr、0.14% Si、 0.42% Mn、0.03% P、0.031% C、0.02%S、0.809% Fe、0.29% Ti、其余为Ni。
所述金属氧化物涂层是首先通过电镀制备的镍铁的复合镀层，再经由预氧化获得致密的氧化层，氧化层是由三氧化二铬、氧化镍、镍铁尖晶石和三氧化二铁构成；
所述电镀制备的镍铁的复合镀层的质量百分比成分Fe含量为20～37％，Ni含量为63～80％。
所述电镀液配制为：200g/l NiSO4·6H2O、60g/l FeSO4·7H2O、30g/l 柠檬酸钠、40g/l H3BO3、30g/l NaCl、3g/l 糖精、0.3g/l 苯亚磺酸钠、0.3g/l 十二烷基硫酸钠。
所述致密的氧化层，高温时有较好的导电特性。
附图说明
图1为电镀设施图。
图2为施例1惰性阳极在800℃氧化30h后横截面形貌图。
图3为施例1惰性阳极在800℃氧化30h后表面形貌图。
具体实施方式
下面结合实施例对本发明作进一步详细的描述，但本发明的实施方式不限于此。
本发明适用于铝电解的惰性阳极，以GH3030合金为基体制备金属金属氧化物涂层。
实施例1
将GH3030合金切割加工成样品，依次对样品进行机械整平、丙酮超声除油、碱洗除油以及酸洗去除氧化膜。并且使用双石墨阳极、单阴极的方法在PH=3.5、电流密度15A/dm2及60℃恒温水浴条件下对GH3030合金基体电镀20min。电镀装置示意图见图1
镀层的具体化学成分按质量百分比计，具体化学成分37.11%Fe、62.89%Ni。
对相同条件下对进行电镀20min后的样品1＃、2＃、3＃在800℃下进行预氧化30h，其增重分别为3.51mg/ cm2、3.83mg/ cm2、3.45mg/ cm2。
取其平均值，则该样品在800℃下进行30h后该合金增重约为3.60mg/ cm2，随炉冷却氧化层无明显剥落现象，表明基体与氧化物间的结合性比较好。
实施例2
将GH3030合金切割加工成样品，依次对样品进行机械整平、丙酮超声除油、碱洗除油以及酸洗去除氧化膜。同样使用双石墨阳极、单阴极的方法在PH=3.5、电流密度15A/dm2 及60℃恒温水浴条件下对GH3030合金基体电镀30min。
镀层的具体化学成分按质量百分比计，具体化学成分20.73%Fe、79.27%Ni。
对相同条件下对进行电镀20min后的样品1＃、2＃、3＃在800℃下进行预氧化30h，其增重分别为4.47mg/ cm2、4.53mg/ cm2、4.62mg/ cm2。
取其平均值，则该样品在800℃下进行30h后该合金增重约为4.54mg/ cm2，随炉冷却氧化层无明显剥落现象，表明基体与氧化物间的结合性比较好。
实施例3
如图2和图3所示，实施例2的样品在800℃下进行30h氧化后，对其进行X射线衍射和扫描电镜分析后：合金表面氧化物主要为尖晶石结构，其氧化物厚度约11～14μm；氧化物为致密连续的混合氧化层。说明氧化过程中形成的氧化物提高了阳极的高温抗氧化性能。
实施例4
对实施例2的样品进行30h预氧化使阳极样品表面生成氧化物保护膜。以该样品为阳极，阴极为高纯石墨，3.0cm极距，800℃温度下，以0.5A/cm2阳极电流密度，在电解质组质量比组成为58.25Na3AlF6-32.35AlF3-5CaF2-4.4Al2O3的熔盐体系中进行了长达数10小时的电解。电解时，阳极通过导电杆连接并垂直插入带有刚玉内衬的石墨坩埚。在电解过程中，槽电压在4.2～4.7伏特，阳极腐蚀速率慢，且导电性较好。说明该样品作为阳极在熔盐冰晶石中高温抗氧化性和抗电化学腐蚀性能良好。
Claims (6)
1.一种镍铬合金表面制备有抗氧化耐腐蚀涂层的惰性阳极，其特征在于，所述惰性阳极是由GH3030合金基体以及合金基体表面的金属氧化物复合涂层组成。
2.根据权利要求1所述一种镍铬合金表面制备有抗氧化耐腐蚀涂层的惰性阳极，其特征在于，所述GH3030合金的质量百分比成分20.23% Cr、0.14% Si、 0.42% Mn、0.03% P、0.031% C、0.02% S、0.809% Fe、0.29%Ti、其余为Ni。
3.根据权利要求1所述一种镍铬合金表面制备有抗氧化耐腐蚀涂层的惰性阳极，其特征在于，所述金属氧化物涂层是首先通过配置电镀液来电镀制备镍铁合金镀层，再经由预氧化获得致密的氧化层，氧化层是由三氧化二铬、氧化镍、镍铁尖晶石和三氧化二铁构成。
4.根据权利要求3所述一种镍铬合金表面制备有抗氧化耐腐蚀涂层的惰性阳极，其特征在于，所述电镀制备的镍铁的复合镀层的质量百分比成分Fe含量为20～37％，Ni含量为63～80％。
5.根据权利要求3所述一种镍铬合金表面制备有抗氧化耐腐蚀涂层的惰性阳极，其特征在于，所述所述电镀液配制方案：200g/l NiSO4·6H2O、60g/l FeSO4·7H2O、30g/l 柠檬酸钠、40g/l H3BO3、30g/l NaCl 、3g/l 糖精、0.3g/l 苯亚磺酸钠、0.3g/l 十二烷基硫酸钠。
6.根据权利要求3所述一种镍铬合金表面制备有抗氧化耐腐蚀涂层的惰性阳极，其特征在于，所述致密的氧化层，高温时有较好的导电特性。
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| CN116970896A (zh) * | 2023-09-22 | 2023-10-31 | 成都先进金属材料产业技术研究院股份有限公司 | 一种提高Ni-Cr电热合金产品预氧化效果的方法 |
| CN116970896B (zh) * | 2023-09-22 | 2024-02-02 | 成都先进金属材料产业技术研究院股份有限公司 | 一种提高Ni-Cr电热合金产品预氧化效果的方法 |
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