CN105506674A - 一种提高金属陶瓷惰性阳极耐蚀性能的方法 - Google Patents
一种提高金属陶瓷惰性阳极耐蚀性能的方法 Download PDFInfo
- Publication number
- CN105506674A CN105506674A CN201610114959.7A CN201610114959A CN105506674A CN 105506674 A CN105506674 A CN 105506674A CN 201610114959 A CN201610114959 A CN 201610114959A CN 105506674 A CN105506674 A CN 105506674A
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- China
- Prior art keywords
- inert anode
- cermet inert
- alf
- anode
- resisting property
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 238000005260 corrosion Methods 0.000 title claims abstract description 32
- 239000000919 ceramic Substances 0.000 title abstract description 5
- 229910052751 metal Inorganic materials 0.000 title abstract description 5
- 239000002184 metal Substances 0.000 title abstract description 5
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 11
- 239000003792 electrolyte Substances 0.000 claims abstract description 8
- 239000011195 cermet Substances 0.000 claims description 35
- 238000005868 electrolysis reaction Methods 0.000 claims description 22
- 229910052596 spinel Inorganic materials 0.000 claims description 15
- 239000011029 spinel Substances 0.000 claims description 15
- 229910052802 copper Inorganic materials 0.000 claims description 8
- 229910052759 nickel Inorganic materials 0.000 claims description 8
- 239000008151 electrolyte solution Substances 0.000 claims description 7
- 229910052803 cobalt Inorganic materials 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 5
- 229910016569 AlF 3 Inorganic materials 0.000 claims description 4
- 229910004261 CaF 2 Inorganic materials 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminum Chemical compound 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- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 6
- 239000000470 constituent Substances 0.000 description 6
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- 238000001069 Raman spectroscopy Methods 0.000 description 5
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- 238000005530 etching Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
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Classifications
-
- 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
- C25C3/12—Anodes
-
- 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
- C25C3/18—Electrolytes
Abstract
本发明公开了一种提高金属陶瓷惰性阳极耐蚀性能的方法；该方法通过控制电解腐蚀条件使金属陶瓷阳极组元被电解质腐蚀并与电解质反应生成络合阴离子，该络合离子在电场作用下团聚在阳极周围使阳极腐蚀速度减缓，并且该络合离子在电解铝三场作用下向阴极迁移速度较慢，因此溶解在电解质中的阳极组元不容易在阴极放电生成单质金属，从而保持其阴极原铝具有较高的纯度；该方法操作简单、高效，有利于推广应用。
Description
技术领域
[0001]本发明涉及一种提高金属陶瓷惰性阳极耐蚀性能的方法，属于铝电解技术领域。
背景技术
[0002]为了降低金属陶瓷惰性阳极在高温熔盐电解质中的腐蚀速率，除了改变电解质组成降低电解温度外，还采用了在金属相表面包覆一定量的尖晶石型氧化物粉末避免金属相在高温熔盐中相比陶瓷相优先腐蚀(申请号:201110146867.4);或控制一定的电解腐蚀条件使金属陶瓷惰性阳极达到表层致密尖晶石型氧化物陶瓷腐蚀与金属陶瓷惰性阳极内部连续形成新的致密尖晶石型氧化物陶瓷层的动态腐蚀平衡(申请号:201210066342.4)。包覆的方法虽一定程度上降低了腐蚀速率，但阳极电导率下降反而提高了能耗;动态腐蚀平衡虽解决了阳极表层腐蚀与电导的统一问题，但阳极耐腐蚀性能还有待提高。并且阳极组元被高温电解质腐蚀进入电解质后其形成的络合离子结构与迀移特性至今未见报道。
发明内容
[0003]针对现有耐蚀技术存在的缺陷，本发明的目的是在于提供一种能有效提高金属陶瓷惰性阳极耐蚀性能，且保持阴极原铝具有较高纯度的方法;该方法操作简单、高效，有利于工业推广应用。
[0004]为了实现上述技术目的，本发明提供了一种提高金属陶瓷惰性阳极耐蚀性能的方法，该方法是将金属陶瓷惰性阳极置于电解液中，在温度为930〜960°C、电流密度为0.95〜
1.0A/cm2的条件下，电解10h以上；
[0005]所述的金属陶瓷惰性阳极包含尖晶石型氧化物、非尖晶石型氧化物和金属相；
[0006] 所述的电解液包含Na3AlF6和/或K3AlF6,与AlF3XaF2及Al2O3组成的电解质。
[0007]优选的方案，金属陶瓷惰性阳极包含以下质量百分比组分:尖晶石型氧化物50%〜95%，非尖晶石型氧化物I %〜30%，金属相I %〜30 %。
[0008]较优选的方案，尖晶石型氧化物为MFe2O4,其中，iC%N1、Cu、Mn、ZnSCo。
[0009] 较优选的方案，非尖晶石型氧化物为Ax0y，其中，x=l或2，y=l、2或3，A为N1、Cu、Mn、Zn或Co ο
[0010] 较优选的方案，金属相为Fe、N1、Cu、Co、Ag中的至少一种。
[0011] 优选的方案，电解质中包含以下质量百分比组分:Na3AlF6和/或K3A1F660〜80%，A1F35〜30%，CaF2 < 10%，Αΐ2θ37〜10%。
[0012]较优选的方案，金属陶瓷惰性阳极在电解液中电解，金属陶瓷惰性阳极组分与电解质组分发生反应生成1^14疋2(20—2a—3χ)—络合离子，其中肩为附、Fe和Cu中的至少一种，a和X均大于或等于零，且不同时为零，y和z均大于零。
[0013]本发明的技术原理及相对现有技术带来的有益技术效果:
[0014]原理:通过大量研究表明，在本发明的温度和电流密度下，将金属陶瓷惰性阳极置于适当的电解液中进行电解腐蚀，金属陶瓷惰性阳极中的组元被腐蚀后与电解质反应生成一种特殊的络合阴离这种络合离子在电场作用下团聚分布在阳极周围，能够有效减缓阳极腐蚀速度，同时，该络合离子在电解铝三场作用下向阴极迀移速度较慢，因此溶解在电解质中的阳极组元不容易在阴极放电生成单质金属，从而保持其阴极原铝具有较高的纯度。
[0015]有益效果:(I)本发明的技术方案可以同时提高铝电解用金属陶瓷惰性阳极的耐蚀性能和提高原铝纯度，采用合适的腐蚀工艺条件减缓了惰性阳极材料被氟化物高温熔盐电解质腐蚀后的耐蚀问题。(2)本发明的技术方案工艺简单、方便，易于推广应用。
附图说明
[0016]【图1】为实施例1中1300°C烧结4小时的22(20N1-Cu)/(NiFe204_10Ni0)金属陶瓷惰性阳极在960°C电解120h后表面致密层Fe2p峰的XPS谱。
[0017]【图2】为实施例1中1300°C烧结4小时的22(20N1-Cu)/(NiFe204_10Ni0)金属陶瓷惰性阳极表面层Fe2p峰的XPS谱。
[0018]【图 3】为实施例1 中电解质78.07%Na3AlF6-9.5 % A1F3_5.0 % CaF2_7.43 % Al2O3的拉曼光谱图。
[0019]【图4】为实施例1 中电解质78.07%Na3AlF6-9.5 % A1F3_5.0 % CaF2_7.43 % Al2O3 中加入1.0wt%Ni0的拉曼光谱图。
[0020]【图 5】为实施例1 中电解质78.07%Na3AlF6-9.5 % A1F3_5.0 % CaF2_7.43 % Al2O3 中加入1.0wt%Fe203的拉曼光谱图。
[0021 ]【图6】为实施例1 电解质78.07 % Na3AlF6-9.5%AlF3-5.0 % CaF2_7.43 ^Al2O3中加入1.0wt%Ni的拉曼光谱图。
[0022]【图 7】为实施例1 电解质78.07 % Na3AlF6-9.5%AlF3-5.0 % CaF2_7.43 ^Al2O3中加入1.0wt % Cu的拉曼光谱图。
[0023]【图8】为实施例2中1300°C烧结4小时的22(20N1-Cu)/(NiFe204_10Ni0)金属陶瓷惰性阳极在960°C电解240h后表面致密层Fe2p峰的XPS谱。
具体实施方式
[0024]下面结合实施例对本发明内容作进一步说明，而不是对本发明权利要求保护范围的限制。
[0025] 实施例1
[0026] 22(20祖-(:11)/85(祖卩6204-10附0)金属陶瓷惰性阳极在78.07%似3厶怀6-9.5%A1F3-5.0 % CaF2-7.43 ^Al2O3电解质中的电解 120小时:
[0027] 22(20N1-Cu)/85(NiFe204_10Ni0)金属陶瓷惰性阳极在电解质78.07 ^Na3AlF6-9.5%AlF3-5.0%CaF2-7.43%A1203，中电解温度960°C(初晶温度947°C，过热度 13°C，电流密度0.98A/cm2)电解120h后腐蚀样品表面致密层Fe2p峰的XPS谱分别如图1所示，其Fe2+/Fe3+比值分别为0.968，相比未电解样品Fe2+/Fe3+比值0.75(表面层Fe2p峰的XPS谱如图2所示)，电解后的样品Fe2VFe3+比值均有增加，说明其耐熔盐腐蚀性能均有所提高。经过图3-7拉曼光谱分析可知，在电解过程中溶解于电解质中的阳极组元与电解质形成了络合阴离子NiaAlx0yFz(2y+z—2a—3x)—、FeaAlx0yFz(2y+z—2a—3x)—和CuaAlx0yFz(2y+z—2a—3x)—(其中a和X大于等于零但不能同时为零，y和z大于零)。说明溶解于电解质中的阳极组元在电解质中形成了络合阴离子。
[0028] 实施例2
[0029] 22(20祖-(:11)/85(祖卩6204-10附0)金属陶瓷惰性阳极在78.07%似3厶怀6-9.5%A1F3-5.0%CaF2-7.43 ^Al2O3 电解质中的电解 240 小时:
[0030] 22(20N1-Cu)/85(NiFe204_10Ni0)金属陶瓷惰性阳极在电解质78.07 ^Na3AlF6-9.5%AlF3-5.0%CaF2-7.43%A1203，中电解温度960°C(初晶温度947°C，过热度 13°C，电流密度0.95A/cm2)电解240h后腐蚀样品表面致密层Fe2p峰的XPS谱如图8所示，其Fe2VFe3+比值为1.11，相比未电解样品Fe2VFe3+比值0.75，电解后的样品Fe2VFe3+比值均有增加，说明其耐熔盐腐蚀性能均有所提高。根据电解240h后电解质和原铝中的杂质计算其年腐蚀率为
0.63 cm/a，与没经过本发明方法处理过的金属陶瓷惰性阳极材料在电流密度0.8A/cm2同样电解条件下年腐蚀率是1.2cm/a，说明溶解于电解质中的阳极组元在电解质中形成络合阴离子提高了阳极的耐高温熔盐腐蚀性能。
Claims (7)
1.一种提高金属陶瓷惰性阳极耐蚀性能的方法，其特征在于:将金属陶瓷惰性阳极置于电解液中，在温度为930〜960°C、电流密度为0.95〜1.0A/cm2的条件下，电解10h以上； 所述的金属陶瓷惰性阳极包含尖晶石型氧化物、非尖晶石型氧化物和金属相； 所述的电解液包含Na3AlF6和/SK3AlF6，与AlF3、CaF2及Al2O3组成的电解质。
2.根据权利要求1所述的提高金属陶瓷惰性阳极耐蚀性能的方法，其特征在于:所述的金属陶瓷惰性阳极包含以下质量百分比组分:尖晶石型氧化物50%〜95%，非尖晶石型氧化物I %〜30%，金属相I %〜30 %。
3.根据权利要求2所述的提高金属陶瓷惰性阳极耐蚀性能的方法，其特征在于:所述的尖晶石型氧化物为MFe204，其中，M为N1、Cu、Mn、Zn或Co。
4.根据权利要求2所述的提高金属陶瓷惰性阳极耐蚀性能的方法，其特征在于:所述的非尖晶石型氧化物为AxOy，其中，x=]^2，y=l、2S3，ASN1、Cu、Mn、Zr^Co。
5.根据权利要求2所述的提高金属陶瓷惰性阳极耐蚀性能的方法，其特征在于:所述的金属相为Fe、N1、Cu、Co、Ag中的至少一种。
6.根据权利要求1所述的提高金属陶瓷惰性阳极耐蚀性能的方法，其特征在于，所述的电解质中包含以下质量百分比组分= Na3AlF6和/或K3A1F660〜80%，A1F35〜30% ,CaF2 <10%，Al2037〜10%o
7.根据权利要求1〜6任一项所述的提高金属陶瓷惰性阳极耐蚀性能的方法，其特征在于:所述的金属陶瓷惰性阳极在电解液中电解，金属陶瓷惰性阳极组分与电解质组分发生反应生成1^14疋2(20—2a—3χ)—络合离子，其中，M为N1、Fe和Cu中的至少一种，a和X均大于或等于零，且不同时为零，y和z均大于零。
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| CN103668343A (zh) * | 2013-12-03 | 2014-03-26 | 中南大学 | 一种提高金属陶瓷惰性阳极表面致密层电导率的方法 |
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