脉冲电沉积纳米晶铬-镍-铁合金工艺及其基础理论研究
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摘要
传统的铬或铬合金镀层采用六价铬镀液，由于电流效率低并且镀液毒性大等的缘故，已经不能满足当今社会对环保，节能和经济效益的需要，人们希望用三价铬镀液取代六价铬镀液。但三价铬电镀的研究还有待深入，有些问题尚未完全解决，其中最为突出的就是，镀层无法随沉积时间的延长而持续增厚，这使得电镀功能性厚镀层时采用三价铬电镀还很困难。因此，本文在电沉积出镍-铁合金纳米晶的基础上，采用脉冲电沉积的方法研究了在三价铬体系中获得纳米晶铬和铬-镍-铁合金纳米晶厚镀层的工艺及其基础理论，以期解决三价铬镀液完全代替六价铬电镀的难题。
本文首次研究了制备用于电磁屏蔽等领域的电沉积铁-镍纳米晶合金箔和铁-镍-铬纳米晶合金箔的方法；系统研究了各工艺条件对合金成分和电流效率的影响；确定了获得铁-镍合金箔的最优工艺条件为：FeSO_4·7H_2O为52g·l~(-1)，镍铁离子浓度摩尔比为4.7～5左右，H_3BO_345g·l~(-1)，稳定剂Ⅰ的浓度控制在29～34g·l~(-1)，稳定剂Ⅱ浓度为10g·l~(-1)，阴极电流密度为5A·dm~(-2)，温度控制在48～52℃，pH值控制在1.75～2.25；确定了获得电沉积高电阻率铁-镍-铬合金箔的最佳工艺配方为：CrCl_3·6H_2O 20g·l~(-1)，FeSO_4·7H_2O 65～70g·l~(-1)，NiSO_4·6H_2O180 g·l~(-1)，NiCl_2·6H_2O 45g·l~(-1)，H_3BO_345g·l~(-1)，稳定剂Ⅰ25～30 g·l~(-1)，稳定剂Ⅱ 10 g·l~(-1)，光亮剂1～5 g·l~(-1)，润湿剂0.2～0.5g·l~(-1)。电流密度10～12 A·dm~(-2)，温度58~65℃，溶液pH值2.20～2.50，在上述条件下获得的合金箔厚度在50μm左右，成分均匀、结晶细致、镀层光亮；其中铁-镍合金箔成分为48％～50％Ni，50％～52％Fe，微量的Cr，P与S，B，C；铁-镍-铬合金箔成分为65％～70％Ni，30％～35％Fe，1％～2％Cr和微量的P与S，B，C。实验证明在直流电沉积条件下从水溶液中获得质量优良含Cr量＞2％的三元合金镀层是比较困难的。
本文首次系统的研究了从含Cr~(3+)的水／N，N-二甲基甲酰胺(DMF)溶液或含镍、铁、铬离子的合金水／DMF溶液中脉冲电沉积纳米晶铬和铬-镍-铁合金纳米晶厚镀层的方法；系统研究了脉冲电沉积条件下脉冲周期、脉冲工作比、溶液中各主盐浓度、溶液的pH值、电沉积时间等工艺条件对电沉积铬和铬-镍-铁合金的沉积速度、电流效率、合金成分、表面形貌、晶粒尺寸等的影响；电沉积获得纳米晶铬以及纳米晶铬-镍-铁合金镀层都具有镜面光亮的外观，其中的铬-镍-铁合金镀层最厚可以达到80μm以上，较文献报道的厚度要厚；铬-镍-铁合金镀层的成分分别为Cr40％～60％，Ni10％～40％，Fe10％～30％，以及其他一些元素，如S，B，C，O，H等。确定脉冲电沉积获得纳米晶铬镀层的最佳工艺为CrCl_3·6H_2O含量为0.8～1.2mol·l~(-1)，脉冲周期为100ms，占空比0.3-0.5，电流密度18～20 A·dm~(-2)，温度为30℃左右，溶液pH值为1.0左右，溶液循环速度保持在1.36～1.98ml·min~(-1)；获得铬-镍-铁合金纳米晶的最佳工艺条件为脉冲周期为100ms，工作比为0.3～0.5，平均电流密度为18～20A·dm~(-2)，镀液温度30℃左右，pH值控制在0.9～1.5，在这种条件下脉冲电沉积铬-镍-铁合金的平均沉积速度可以达到3μm·min~(-1)，电流效率为50％以上。对直流电沉积和脉冲电沉积纳米晶铬和纳米晶铬-镍-铁合金的电流效率、晶体结构、物理和化学性能等进行了比较，结果表明脉冲电沉积获得的纳米晶较直流电沉积获得的纳米晶在各方面都优秀。
通过动电位扫描、计时电流等电化学方法，详细研究了纳米晶铬、纳米晶铁-镍-铬合金箔、纳米晶铬-镍-铁合金在10％H_2SO_4、10％NaOH、3.5％NaCl中的电
中南大学博士学位论文
摘要
化学行为，还用在空气中放置的方法研究了其在空气中的耐蚀性能，并与文献报
道的非晶态铬一镍一铁合金的耐蚀性进行了比较，结果表明本文所获得的纳米晶镀
层具有优良的耐蚀性，并且具有优良的电催化析氢性能;通过对纳米晶镀层的电
阻率和磁饱和度测定，表明纳米晶铁一镍一铬合金箔以及铬一镍一铁镀层具有比常规
合金更高的电阻率和磁饱和度，是很好的电磁材料;通过扫描电镜(S EM)对镀
层表面形貌的研究，表明镀层结晶细致均匀，镀层光亮，无针孔和微裂纹，晶粒
尺寸小于IOOnln，具有很长的晶界，因而耐蚀性优异;由于晶粒尺寸在纳米范围
内，因而电阻率和磁饱和度随晶粒尺寸的减小而大幅度提高;通过X一衍射结构
分析表明纳米晶具有介于非晶态和晶态的结构，是易于氢析出的(111)织构，
而非常规的(220)织构，因此具有较好的电催化析氢能力。
通过电化学方法和光谱方法研究了铬一镍一铁合金镀液的陈化和稳定性，cr3份
的配合形态以及电沉积过程中CrZ‘对电沉积的影响结果:通过电位分析研究表明
添加剂和稳定剂可以提高合金镀液的缓冲能力;发现在没有稳定剂和添加剂存在
的条件下，很难获得质量好的厚铬或厚铬合金镀层，电解液的缓冲能力也很差。
稳态极化曲线研究也表明合适的稳定剂和添加剂使得铬、镍、铁合金电沉积
成为可能:用交流阻抗法研究了镍、镍一铁、铬一镍一铁在水心MF溶液中沉积的电
化学过程，分析表明镍、镍一铁和?
Though having disadvantage such as low current efficiency and toxicity, the electrodeposition of traditional chromium or chromium alloy had been employed from heaxvalent chromium electrolyte since the first use of the process. With the more and more attention having been paid to the pollution control and economical efficiency at the present time, it has been hoped to substitute by nontoxicity trivalent chromium electrolyte little by little. While high quality deposition from trivalent chromium electrolyte could only be sustained for short periods and thin deposits obtained of decorative value only, it is difficult to substitute heaxvalent chromium plating in engineering electrodeposits by trivalent chromium plating at all. In order to resolve the problem of substitution for heaxvalent chromium electrodeposits, the technology and mechanism of pulse plating nanocrystalline chromium, chromium-nickel-iron alloys from trivalent chromium electrolyte have been investigated based on the electroplating nanocrystallin
e iron-nickel alloy foil.
In this dissertation, methods of plating nanocrystalline iron-nickel alloy foil and iron-nickel-chromium alloy foil, which are used in electromagnet fields, have been studied for the first time based on the electroplating nanocrystalline iron-nickel alloy. The technological parameters, which affect the alloy composition and current efficiency, have also been studied systemically. The optimum technology of iron-nickel alloy foil plating is followed as that: 52g l-11 FeSO4 7H2O,about 3.5 of the concentration ratio of Fe2+ and Ni2+ , 29~34g l-1 stabilizer I , 10g l-1 stabilizer II. with 5 A dm-2 current density ,at 48-52C temperature in the solution of pH restricted between 1.75 and 2.25. The optimum technology of iron-nickel-chromium alloy foil plating is followed as that: 20 g l-1 CrCl3 6H2O,65~70 g l-1 FeSO4 7H2O,180 g l-1 NiSO4 6H2O,45 g l-1 NiCl2 6H2O,45 g l-1 H3BO3, 25~30 g l-1 stabilizer I , and 10g l-1 stabilizer II, 1-5 g l-1brighteners ,0.2-0.5 g l-1 addictives with 10-12 A 玠m" current density
,at 58~65C temperature in the solution of pH from2.0 to 2.50. The thickness of alloy foils are up to 50 u m with a mirror-like appearance , uniform composition and delicate grain. The iron-nickel alloy foil contains 46%~48%Ni, 50%~52%%Fe, and a little other elements such as Cr, S, B, C and P, while the iron-nickel-chromium alloy foil contains 65%~70%Fe, 30%~35%Ni, l%~2%Cr% and a little other elements such as S, B, C, O and P. The experiment proved that it is difficult to obtain thick deposits with >2% Cr from aqueous solution by direct current plating.
For the first time, some new methods of pulse plating nanocrystalline chromium, and chromium-nickel-iron alloy deposits from trivalent chromium chloride -N, N-dimethylformamide (DMF) solution have been studied systemically. The effects on electrodeposit rate, current efficiency, alloy composition, surface appearance and grainsize by pulse plating periods, duty cycle, concentration of different metal ions, cathodic average current density, pH of electrolyte, operation temperature, stirring velocity and plating time from chloride-N, N-dimethylformamide solution have been studied systemically for the first time. All the nanocrystalline deposits have been
obtained at room temperature with a mirror like appearance. The thickness of nanocrystalline chromium-nickel-iron alloy deposit was up to 80 um. Nanocrystalline chromium-nickel-iron alloy deposits contain 40%~60%Cr, 10%~40%Ni, 10%~30%Fe and a little other elements such as S, B, C, O and H. The optimum technology of bright nanocrystalline chromium plating is followed as that:0.8~l ,2mol l-1 CrCl3 6H2O ,period is 100ms,duty cycle is from 0.3-0.5,average current density is from 18-20A ?dm'2 ,at temperature about 30C in the solution of pH restricted at 0.9. The optimum technology of bright nanocrystalline chromium-nickel-iron alloy plating is followed as that: period is 100ms,duty cycle is from 0.3-0.5,average current density is from 18-20A dm-2 ,at temperature about of 30C in the
本文首次研究了制备用于电磁屏蔽等领域的电沉积铁-镍纳米晶合金箔和铁-镍-铬纳米晶合金箔的方法；系统研究了各工艺条件对合金成分和电流效率的影响；确定了获得铁-镍合金箔的最优工艺条件为：FeSO_4·7H_2O为52g·l~(-1)，镍铁离子浓度摩尔比为4.7～5左右，H_3BO_345g·l~(-1)，稳定剂Ⅰ的浓度控制在29～34g·l~(-1)，稳定剂Ⅱ浓度为10g·l~(-1)，阴极电流密度为5A·dm~(-2)，温度控制在48～52℃，pH值控制在1.75～2.25；确定了获得电沉积高电阻率铁-镍-铬合金箔的最佳工艺配方为：CrCl_3·6H_2O 20g·l~(-1)，FeSO_4·7H_2O 65～70g·l~(-1)，NiSO_4·6H_2O180 g·l~(-1)，NiCl_2·6H_2O 45g·l~(-1)，H_3BO_345g·l~(-1)，稳定剂Ⅰ25～30 g·l~(-1)，稳定剂Ⅱ 10 g·l~(-1)，光亮剂1～5 g·l~(-1)，润湿剂0.2～0.5g·l~(-1)。电流密度10～12 A·dm~(-2)，温度58~65℃，溶液pH值2.20～2.50，在上述条件下获得的合金箔厚度在50μm左右，成分均匀、结晶细致、镀层光亮；其中铁-镍合金箔成分为48％～50％Ni，50％～52％Fe，微量的Cr，P与S，B，C；铁-镍-铬合金箔成分为65％～70％Ni，30％～35％Fe，1％～2％Cr和微量的P与S，B，C。实验证明在直流电沉积条件下从水溶液中获得质量优良含Cr量＞2％的三元合金镀层是比较困难的。
本文首次系统的研究了从含Cr~(3+)的水／N，N-二甲基甲酰胺(DMF)溶液或含镍、铁、铬离子的合金水／DMF溶液中脉冲电沉积纳米晶铬和铬-镍-铁合金纳米晶厚镀层的方法；系统研究了脉冲电沉积条件下脉冲周期、脉冲工作比、溶液中各主盐浓度、溶液的pH值、电沉积时间等工艺条件对电沉积铬和铬-镍-铁合金的沉积速度、电流效率、合金成分、表面形貌、晶粒尺寸等的影响；电沉积获得纳米晶铬以及纳米晶铬-镍-铁合金镀层都具有镜面光亮的外观，其中的铬-镍-铁合金镀层最厚可以达到80μm以上，较文献报道的厚度要厚；铬-镍-铁合金镀层的成分分别为Cr40％～60％，Ni10％～40％，Fe10％～30％，以及其他一些元素，如S，B，C，O，H等。确定脉冲电沉积获得纳米晶铬镀层的最佳工艺为CrCl_3·6H_2O含量为0.8～1.2mol·l~(-1)，脉冲周期为100ms，占空比0.3-0.5，电流密度18～20 A·dm~(-2)，温度为30℃左右，溶液pH值为1.0左右，溶液循环速度保持在1.36～1.98ml·min~(-1)；获得铬-镍-铁合金纳米晶的最佳工艺条件为脉冲周期为100ms，工作比为0.3～0.5，平均电流密度为18～20A·dm~(-2)，镀液温度30℃左右，pH值控制在0.9～1.5，在这种条件下脉冲电沉积铬-镍-铁合金的平均沉积速度可以达到3μm·min~(-1)，电流效率为50％以上。对直流电沉积和脉冲电沉积纳米晶铬和纳米晶铬-镍-铁合金的电流效率、晶体结构、物理和化学性能等进行了比较，结果表明脉冲电沉积获得的纳米晶较直流电沉积获得的纳米晶在各方面都优秀。
通过动电位扫描、计时电流等电化学方法，详细研究了纳米晶铬、纳米晶铁-镍-铬合金箔、纳米晶铬-镍-铁合金在10％H_2SO_4、10％NaOH、3.5％NaCl中的电
中南大学博士学位论文
摘要
化学行为，还用在空气中放置的方法研究了其在空气中的耐蚀性能，并与文献报
道的非晶态铬一镍一铁合金的耐蚀性进行了比较，结果表明本文所获得的纳米晶镀
层具有优良的耐蚀性，并且具有优良的电催化析氢性能;通过对纳米晶镀层的电
阻率和磁饱和度测定，表明纳米晶铁一镍一铬合金箔以及铬一镍一铁镀层具有比常规
合金更高的电阻率和磁饱和度，是很好的电磁材料;通过扫描电镜(S EM)对镀
层表面形貌的研究，表明镀层结晶细致均匀，镀层光亮，无针孔和微裂纹，晶粒
尺寸小于IOOnln，具有很长的晶界，因而耐蚀性优异;由于晶粒尺寸在纳米范围
内，因而电阻率和磁饱和度随晶粒尺寸的减小而大幅度提高;通过X一衍射结构
分析表明纳米晶具有介于非晶态和晶态的结构，是易于氢析出的(111)织构，
而非常规的(220)织构，因此具有较好的电催化析氢能力。
通过电化学方法和光谱方法研究了铬一镍一铁合金镀液的陈化和稳定性，cr3份
的配合形态以及电沉积过程中CrZ‘对电沉积的影响结果:通过电位分析研究表明
添加剂和稳定剂可以提高合金镀液的缓冲能力;发现在没有稳定剂和添加剂存在
的条件下，很难获得质量好的厚铬或厚铬合金镀层，电解液的缓冲能力也很差。
稳态极化曲线研究也表明合适的稳定剂和添加剂使得铬、镍、铁合金电沉积
成为可能:用交流阻抗法研究了镍、镍一铁、铬一镍一铁在水心MF溶液中沉积的电
化学过程，分析表明镍、镍一铁和?
Though having disadvantage such as low current efficiency and toxicity, the electrodeposition of traditional chromium or chromium alloy had been employed from heaxvalent chromium electrolyte since the first use of the process. With the more and more attention having been paid to the pollution control and economical efficiency at the present time, it has been hoped to substitute by nontoxicity trivalent chromium electrolyte little by little. While high quality deposition from trivalent chromium electrolyte could only be sustained for short periods and thin deposits obtained of decorative value only, it is difficult to substitute heaxvalent chromium plating in engineering electrodeposits by trivalent chromium plating at all. In order to resolve the problem of substitution for heaxvalent chromium electrodeposits, the technology and mechanism of pulse plating nanocrystalline chromium, chromium-nickel-iron alloys from trivalent chromium electrolyte have been investigated based on the electroplating nanocrystallin
e iron-nickel alloy foil.
In this dissertation, methods of plating nanocrystalline iron-nickel alloy foil and iron-nickel-chromium alloy foil, which are used in electromagnet fields, have been studied for the first time based on the electroplating nanocrystalline iron-nickel alloy. The technological parameters, which affect the alloy composition and current efficiency, have also been studied systemically. The optimum technology of iron-nickel alloy foil plating is followed as that: 52g l-11 FeSO4 7H2O,about 3.5 of the concentration ratio of Fe2+ and Ni2+ , 29~34g l-1 stabilizer I , 10g l-1 stabilizer II. with 5 A dm-2 current density ,at 48-52C temperature in the solution of pH restricted between 1.75 and 2.25. The optimum technology of iron-nickel-chromium alloy foil plating is followed as that: 20 g l-1 CrCl3 6H2O,65~70 g l-1 FeSO4 7H2O,180 g l-1 NiSO4 6H2O,45 g l-1 NiCl2 6H2O,45 g l-1 H3BO3, 25~30 g l-1 stabilizer I , and 10g l-1 stabilizer II, 1-5 g l-1brighteners ,0.2-0.5 g l-1 addictives with 10-12 A 玠m" current density
,at 58~65C temperature in the solution of pH from2.0 to 2.50. The thickness of alloy foils are up to 50 u m with a mirror-like appearance , uniform composition and delicate grain. The iron-nickel alloy foil contains 46%~48%Ni, 50%~52%%Fe, and a little other elements such as Cr, S, B, C and P, while the iron-nickel-chromium alloy foil contains 65%~70%Fe, 30%~35%Ni, l%~2%Cr% and a little other elements such as S, B, C, O and P. The experiment proved that it is difficult to obtain thick deposits with >2% Cr from aqueous solution by direct current plating.
For the first time, some new methods of pulse plating nanocrystalline chromium, and chromium-nickel-iron alloy deposits from trivalent chromium chloride -N, N-dimethylformamide (DMF) solution have been studied systemically. The effects on electrodeposit rate, current efficiency, alloy composition, surface appearance and grainsize by pulse plating periods, duty cycle, concentration of different metal ions, cathodic average current density, pH of electrolyte, operation temperature, stirring velocity and plating time from chloride-N, N-dimethylformamide solution have been studied systemically for the first time. All the nanocrystalline deposits have been
obtained at room temperature with a mirror like appearance. The thickness of nanocrystalline chromium-nickel-iron alloy deposit was up to 80 um. Nanocrystalline chromium-nickel-iron alloy deposits contain 40%~60%Cr, 10%~40%Ni, 10%~30%Fe and a little other elements such as S, B, C, O and H. The optimum technology of bright nanocrystalline chromium plating is followed as that:0.8~l ,2mol l-1 CrCl3 6H2O ,period is 100ms,duty cycle is from 0.3-0.5,average current density is from 18-20A ?dm'2 ,at temperature about 30C in the solution of pH restricted at 0.9. The optimum technology of bright nanocrystalline chromium-nickel-iron alloy plating is followed as that: period is 100ms,duty cycle is from 0.3-0.5,average current density is from 18-20A dm-2 ,at temperature about of 30C in the
引文
[1] 罗勤慧，沈孟生，丁益，等，三价铬离子的水解聚合作用的研究，化学学报，1982，40(2)：125～132。
[2] Liebreich E,German Patent,1924,448526,GB.Patent 1924,243046.
[3] O.Bornhauser, Societe, D'Electro-chimine D'Electro-Metallurgoe Et.Des.Acieries Electriques D' ugine,German Patent,608757(17.1.35).
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