CN108866605A - A kind of Zn-Ni-Al2O3Electroplate liquid, preparation method and application - Google Patents

A kind of Zn-Ni-Al2O3Electroplate liquid, preparation method and application Download PDF

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Publication number
CN108866605A
CN108866605A CN201811034411.7A CN201811034411A CN108866605A CN 108866605 A CN108866605 A CN 108866605A CN 201811034411 A CN201811034411 A CN 201811034411A CN 108866605 A CN108866605 A CN 108866605A
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electroplate liquid
additive
solution
acid
sodium
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冯忠宝
王琳
安茂忠
邢鹏飞
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Northeastern University China
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Northeastern University China
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating And Plating Baths Therefor (AREA)

Abstract

The invention discloses a kind of Zn-Ni-Al2O3Electroplate liquid, preparation method and application, electroplate liquid is by main complexant, auxiliary complexing agent, zinc sulfate, nickel sulfate, potassium carbonate, additive, Al2O3Nano granule suspension and water are formulated；Each component content is respectively in electroplate liquid：Main 20~400g/L of complexant, 5~300g/L of auxiliary complexing agent, 10~300g/L of zinc sulfate, 5~200g/L of nickel sulfate, 10~500g/L of potassium carbonate, 0.1~20g/L of additive, Al2O31~100ml/L of nano granule suspension；Wherein additive is formulated by ultrapure water.The present invention is optimized performance by screening and use to additive.Gained Deposit appearance is bright, and uniform ground, plated layer compact, pore-free and crackle, corrosion resistance and wearability significantly improve.

Description

A kind of Zn-Ni-Al2O3Electroplate liquid, preparation method and application
Technical field
The invention belongs to electroplating Zn-Ni-Al2O3Composite deposite technical field is related to a kind of Zn-Ni-Al2O3Electroplate liquid, system Preparation Method and application.
Background technique
It is higher and higher to the quality requirement of protective coating with the development of science and technology and modern industry.Zinc-containing alloy Coating can play a very good protection to steel substrate as anodic coating, be widely used.Currently, due to Zn-Ni- Al2O3The advantages that composite deposite has stability high, and corrosion resistance is good, and hardness is big, pollution-free, therefore it is used for protective materials, in vapour There is very big application in terms of vehicle, aerospace, electric mechanical product.
Cyanide-free electrodeposition Zn-Ni-Al at this stage2O3Composite deposite technology has been achieved for very big progress, but with traditional cyanogen Compound Zn-Ni-Al2O3Composite deposite is compared, and there are still certain gaps for performance, especially in bath stability, corrosion resistance of coating On shiny appearance, it is restricted its application.And plating can significantly be improved by adding a certain amount of additive in the plating solution Liquid and coating performance, stability and corrosion resistance all increase.Existing most of additives can be improved certain of plating solution or coating A little aspect performances, but will also result in the decline of other performances simultaneously, all properties can not be combined.Therefore, the present invention provides It is a kind of to mention high performance additive simultaneously, traditional technology can be replaced completely, make it have highly important technical application value With far-reaching historic significance.
Summary of the invention
Present invention generally provides a kind of Zn-Ni-Al2O3Electroplate liquid, preparation method and application.By the screening of additive and The features such as addition optimizes plating solution, and gained plating solution current efficiency is high, stability height, good dispersion.To obtain appearance Bright, hardness height and corrosion-resistant good composite deposite, are paid attention in industrialization.
The specific technical solution of the present invention is：
A kind of Zn-Ni-Al2O3Electroplate liquid, by main complexant, auxiliary complexing agent, zinc sulfate, nickel sulfate, potassium carbonate, addition Agent, Al2O3Nano granule suspension and water are formulated；Each component content is respectively in electroplate liquid：Main 20~400g/ of complexant L, 5~300g/L of auxiliary complexing agent, 10~300g/L of zinc sulfate, 5~200g/L of nickel sulfate, 10~500g/L of potassium carbonate, addition 0.1~20g/L of agent, Al2O31~100ml/L of nano granule suspension；The additive is alkyl hydrazine, 3- alkyl -2- ring second Alkene, amino acetamide, alkyl trimethyl ammonium bromide, adenine, guanine, cytimidine, thymidine, tetraethylenepentamine, saccharin, Gum arabic, 3- methylquinoline, 2,3- dichloro-quinoxaline, pyridine, cortex cinnamomi acetic acid, 5,6- dichloro-nicotinic acid, uric acid, Vitamin C Acid, dodecyl sodium sulfate, dodecylphenol, alkyl sulfonic acid ammonium, alkyl glycosides, dialkyl diphenylamine, sulfurized alkylphenol calcium, alkane One of base benzene sulfonic acid calcium, succinic acid, dimethyamine borane, antimony trichloride or two or more mixtures.Due to addition The addition of agent, improves wearability, the corrosion resistance of coating, shiny appearance, and coating character is obviously improved.Wherein additive is micro i.e. Changeable plating solution performance, so the concentration of additive is unsuitable excessively high.
Further, above-mentioned main complexant is one or more kinds of mixing of hydantoins or hydantoin derivatives Object.
Further, above-mentioned hydantoin derivatives are 3- methylol -5,5- diphenyl hydantoin, 5,5- diphenyl second Interior uride, the chloro- 5,5- diphenyl hydantoin of 1,3- bis-, 1- amido glycolyurea, 5,5- dimethyl hydantoin, the thio second of 2- Interior uride, the bromo- 5,5- dimethyl hydantoin of 1,3- bis-, 1,3-Dimethylol-5,5-Dimethylhydantoin or 2- thio -5, 5- dimethyl hydantoin.
Further, above-mentioned auxiliary complexing agent is dimethylamine, ethylenediamine, triethanolamine, triethylene tetramine, four ethylene five Amine, amion acetic acid, potassium tartrate, sodium potassium tartrate tetrahydrate, sodium citrate, ammonium citrate, malic acid, polyethylene glycol, hydroxy ethylidene two Phosphonic acids, sodium pyrophosphate, potassium pyrophosphate, oxalic acid, urea, sodium formate, ammonium formate, sodium acetate, ammonium acetate, sodium sulfite, sulfurous acid One or more of ammonium, potassium sulfite, sodium thiosulfate, thiocarbamide.
Above-mentioned Zn-Ni-Al2O3Liquid and preparation method thereof is electroplated, includes the following steps：
Step 1, Al is prepared2O3Nano granule suspension：
Dehydrated alcohol is added in aluminium secondary butylate reagent, reagent is sufficiently dissolved, carries out magnetic agitation, is slowly added to ultrapure The molar ratio of water, aluminium secondary butylate reagent and ultrapure water is 0.01:1.24, obtain solution A；10-20ml is added into every liter of solution A The nitric acid solution that mass concentration is 30%, makes pH value reach 3-5, there is white precipitate generation at this time；Continue to stir at 60 DEG C, directly It is dissolved to all precipitatings to get Al is arrived2O3Nano granule suspension；
Step 2, additive solution is prepared
According to the aimed concn of additive in electroplate liquid, constant volume after additive raw material is configured to clear solution with ultrapure water It saves；
Step 3, electroplate liquid is configured：
According to the target content of ingredient each in electroplate liquid, adds water to mix with zinc sulfate main complexant first, obtain No.1 Clear solution；Auxiliary complexing agent adds water to mix with nickel sulfate, obtains No. two clear solutions；Secondly, by potassium carbonate and Al2O3Nanometer Particle suspension liquid is added separately in No.1 and No. two solution and stirs；Finally, by two kinds after No.1 and No. two solution clarifications Additive solution prepared by step 2 is added in solution mixing, is uniformly mixed, obtains Zn-Ni-Al2O3Electroplate liquid.
Above-mentioned Zn-Ni-Al2O3The method that electroplate liquid prepares composite deposite, includes the following steps：Matrix carry out first oil removing, Pickling is rinsed with distilled water and ultrapure water；Then directly matrix is put into containing Zn-Ni-Al2O3The coating bath of electroplate liquid In, it is electroplated；After completing plating, sample is taken out from electroplate liquid, with ultrapure water clean the surface, cold air drying obtains coating； Current density is 1~5A/dm in electroplating process2, bath temperature is 20~60 DEG C, and pH value is between 7~11, anode cathode separation For 1~30cm, plating solution mixing speed is 0~3000rpm, and electroplating time is 10~120min.
Further, above-mentioned matrix is using piece or iron plate；Anode is Pt piece.
Beneficial effects of the present invention are：Using one or more kinds of additives in plating solution, plating solution is largely changed With the performance of coating.In electroplating Zn-Ni-Al2O3When composite deposite, electroplating process stablize, plating solution will not decompose precipitating, become The phenomenon that color.And additive plays synergistic effect in the plating solution, does not generate doping phenomenon.Coating crystallization is careful, smooth and without gas Hole and crackle, bright property increase.Meanwhile corrosion resistance and wearability are also significantly promoted, and are further improved industrialized Feasibility.
Detailed description of the invention
Fig. 1 is gained SEM figure before and after the addition additive obtained of specific embodiment 5；(a) before being added, after (b) being added.
Fig. 2 is gained Tafel figure before and after the addition additive obtained of specific embodiment 5.
Fig. 3 is gained SEM figure before and after the addition additive obtained of specific embodiment 7；(a) before being added, after (b) being added.
Fig. 4 is gained Tafel figure before and after the addition additive obtained of specific embodiment 7.
Specific embodiment
Present invention will be further explained below with reference to the attached drawings and examples.
Embodiment 1：
Implement electroplating technical conditions：Copper sheet is cathode, and Pt piece is anode, and the distance between anode and cathode is 15cm, plating bath temperature Degree is 50 DEG C, pH value 8, current density 4A/dm2, mixing speed 1100rpm, electroplating time 40min.
Embodiment 2：
Implement electroplating technical conditions：Copper sheet is cathode, and Pt piece is anode, and the distance between anode and cathode is 5cm, bath temperature It is 30 DEG C, pH value 7, current density 3A/dm2, mixing speed 700rpm, electroplating time 30min.
Embodiment 3：
Implement electroplating technical conditions：Copper sheet is cathode, and Pt piece is anode, and the distance between anode and cathode is 10cm, plating bath temperature Degree is 45 DEG C, pH value 9, current density 5A/dm2, mixing speed 800rpm, electroplating time 45min.
Embodiment 4：
Implement electroplating technical conditions：Copper sheet is cathode, and Pt piece is anode, and the distance between anode and cathode is 12cm, plating bath temperature Degree is 40 DEG C, pH value 10, current density 1A/dm2, mixing speed 900rpm, electroplating time 50min.
Embodiment 5：
Implement electroplating technical conditions：Copper sheet is cathode, and Pt piece is anode, and the distance between anode and cathode is 7cm, bath temperature It is 30 DEG C, pH value 10, current density 6A/dm2, mixing speed 900rpm, electroplating time 40min.
Embodiment 6：
Implement electroplating technical conditions：Copper sheet is cathode, and Pt piece is anode, and the distance between anode and cathode is 6cm, bath temperature It is 35 DEG C, pH value 11, current density 6A/dm2, mixing speed 900rpm, electroplating time 30min.
Embodiment 7：
Implement electroplating technical conditions：Copper sheet is cathode, and Pt piece is anode, and the distance between anode and cathode is 4cm, bath temperature It is 45 DEG C, pH value 10, current density 5A/dm2, mixing speed 1000rpm, electroplating time 55min.
Embodiment 8：
Implement electroplating technical conditions：Copper sheet is cathode, and Pt piece is anode, and the distance between anode and cathode is 5cm, bath temperature It is 55 DEG C, pH value 11, current density 7A/dm2, mixing speed 900rpm, electroplating time 30min.
Embodiment 9：
Implement electroplating technical conditions：Copper sheet is cathode, and Pt piece is anode, and the distance between anode and cathode is 6cm, bath temperature It is 50 DEG C, pH value 10, current density 8A/dm2, mixing speed 1000rpm, electroplating time 35min.
Embodiment 10：
Implement electroplating technical conditions：Copper sheet is cathode, and Pt piece is anode, and the distance between anode and cathode is 6cm, bath temperature It is 50 DEG C, pH value 9, current density 4A/dm2, mixing speed 1000rpm, electroplating time 30min.
Embodiment 11：Plating solution composition and concentration are same as Example 8, and iron plate is cathode, and Pt piece is anode, between anode and cathode Distance be 5cm, bath temperature be 55 DEG C, pH value 11, current density 7A/dm2, mixing speed 900rpm, when plating Between be 30min.
Embodiment 12：Plating solution composition and concentration are same as Example 9, and iron plate is cathode, and Pt piece is anode, between anode and cathode Distance be 6cm, bath temperature be 50 DEG C, pH value 10, current density 8A/dm2, mixing speed 1000rpm, when plating Between be 35min.
Embodiment 13：Plating solution composition and concentration are same as in Example 10, and iron plate is cathode, and Pt piece is anode, anode and cathode it Between distance be 6cm, bath temperature be 50 DEG C, pH value 9, current density 4A/dm2, mixing speed 1000rpm, plating Time is 30min.
Gained Deposit appearance is bright, and uniform ground, plated layer compact, pore-free and crackle, corrosion resistance and wearability are significant It improves.

Claims (7)

1. a kind of Zn-Ni-Al2O3Electroplate liquid, which is characterized in that by main complexant, auxiliary complexing agent, zinc sulfate, nickel sulfate, carbon Sour potassium, additive, Al2O3Nano granule suspension and water are formulated；Each component content is respectively in electroplate liquid：Main complexant 20~400g/L, 5~300g/L of auxiliary complexing agent, 10~300g/L of zinc sulfate, 5~200g/L of nickel sulfate, potassium carbonate 10~ 500g/L, 0.1~20g/L of additive, Al2O31~100ml/L of nano granule suspension；The additive is alkyl hydrazine, 3- Alkyl -2- cyclic ethylene, amino acetamide, alkyl trimethyl ammonium bromide, adenine, guanine, cytimidine, thymidine, tetrem Five amine of alkene, saccharin, gum arabic, 3- methylquinoline, 2,3- dichloro-quinoxaline, pyridine, cortex cinnamomi acetic acid, 5,6- dichloro-nicotinic acid, Uric acid, ascorbic acid, dodecyl sodium sulfate, dodecylphenol, alkyl sulfonic acid ammonium, alkyl glycosides, dialkyl diphenylamine, vulcanization One of alkyl phenol calcium, alkyl benzene calcium sulfonate, succinic acid, dimethyamine borane, antimony trichloride or two or more mixing Object.
2. electroplate liquid according to claim 1, which is characterized in that the main complexant is that hydantoins or hydantoins spread out One or more kinds of mixtures of biology.
3. electroplate liquid according to claim 2, which is characterized in that the hydantoin derivatives are 3- methylol -5,5- Diphenyl hydantoin, 5,5- diphenyl hydantoin, the chloro- 5,5- diphenyl hydantoin of 1,3- bis-, 1- amido glycolyurea, 5,5- dimethyl hydantoin, 2- thio-hydantoin, the bromo- 5,5- dimethyl hydantoin of 1,3- bis-, dihydroxymethyl -5 1,3-, 5- dimethyl hydantoin or the thio -5,5- dimethyl hydantoin of 2-.
4. electroplate liquid according to claim 1 or 2 or 3, which is characterized in that the auxiliary complexing agent is dimethylamine, second two Amine, triethanolamine, triethylene tetramine, tetraethylenepentamine, amion acetic acid, potassium tartrate, sodium potassium tartrate tetrahydrate, sodium citrate, lemon Sour ammonium, malic acid, polyethylene glycol, 1-hydroxy ethylidene-1,1-diphosphonic acid, sodium pyrophosphate, potassium pyrophosphate, oxalic acid, urea, sodium formate, formic acid One or both of ammonium, sodium acetate, ammonium acetate, sodium sulfite, ammonium sulfite, potassium sulfite, sodium thiosulfate, thiocarbamide with On.
5. any Zn-Ni-Al of Claims 1 to 42O3Liquid and preparation method thereof is electroplated, which is characterized in that include the following steps：
Step 1, Al is prepared2O3Nano granule suspension：
Dehydrated alcohol is added in aluminium secondary butylate reagent, reagent is sufficiently dissolved, carries out magnetic agitation, is slowly added to ultrapure water, The molar ratio of aluminium secondary butylate reagent and ultrapure water is 0.01:1.24, obtain solution A；10-20ml matter is added into every liter of solution A The nitric acid solution that concentration is 30% is measured, so that pH value is reached 3-5, there is white precipitate generation at this time；Continue to stir at 60 DEG C, until All precipitatings dissolve to arrive Al2O3Nano granule suspension；
Step 2, additive solution is prepared
According to the aimed concn of additive in electroplate liquid, constant volume is protected after additive raw material is configured to clear solution with ultrapure water It deposits；
Step 3, electroplate liquid is configured：
According to the target content of ingredient each in electroplate liquid, add water to mix with zinc sulfate main complexant first, obtains No.1 clarification Solution；Auxiliary complexing agent adds water to mix with nickel sulfate, obtains No. two clear solutions；Secondly, by potassium carbonate and Al2O3Nano particle Suspension is added separately in No.1 and No. two solution and stirs；Finally, by two kinds of solution after No.1 and No. two solution clarifications Additive solution prepared by step 2 is added in mixing, is uniformly mixed, obtains Zn-Ni-Al2O3Electroplate liquid.
6. applying any Zn-Ni-Al of Claims 1 to 42O3The method that electroplate liquid prepares composite deposite, including walk as follows Suddenly：Matrix carries out oil removing, pickling first, is rinsed with distilled water and ultrapure water；Then directly matrix is put into containing Zn- Ni-Al2O3In the coating bath of electroplate liquid, it is electroplated；After completing plating, sample is taken out from electroplate liquid, cleans table with ultrapure water Face, cold air drying obtain coating；It is characterized in that, current density is 1~5A/dm in electroplating process2, bath temperature be 20~ 60 DEG C, for pH value between 7~11, anode cathode separation is 1~30cm, and plating solution mixing speed is 0~3000rpm, electroplating time For 10~120min.
7. according to the method described in claim 6, it is characterized in that, matrix is using piece or iron plate；Anode is Pt piece.
CN201811034411.7A 2018-09-06 2018-09-06 A kind of Zn-Ni-Al2O3Electroplate liquid, preparation method and application Pending CN108866605A (en)

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CN109594110A (en) * 2018-12-13 2019-04-09 江苏师范大学 A kind of localization repairs the device and method of high-speed blanking press Large Copper Screw Nut abrasion
CN109735891A (en) * 2018-12-13 2019-05-10 江苏师范大学 A method of for improving microparticle jetting electrodeposited composite coatings mechanical property
CN110004471A (en) * 2019-05-21 2019-07-12 武汉奥邦表面技术有限公司 A kind of preparation method of green alkaline admiro complexing agent
CN110983309A (en) * 2019-12-26 2020-04-10 广东东硕科技有限公司 Application of 2-thiohydantoin compound or salt thereof
CN111593378A (en) * 2020-04-20 2020-08-28 常州新纪元材料科技有限公司 Preparation of high corrosion-resistant alkaline zinc-nickel alloy electroplating solution and components of additive
CN113249766A (en) * 2021-04-29 2021-08-13 江苏师范大学 High-strength coating for repairing metal parts and preparation method thereof

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109594110A (en) * 2018-12-13 2019-04-09 江苏师范大学 A kind of localization repairs the device and method of high-speed blanking press Large Copper Screw Nut abrasion
CN109735891A (en) * 2018-12-13 2019-05-10 江苏师范大学 A method of for improving microparticle jetting electrodeposited composite coatings mechanical property
CN110004471A (en) * 2019-05-21 2019-07-12 武汉奥邦表面技术有限公司 A kind of preparation method of green alkaline admiro complexing agent
CN110983309A (en) * 2019-12-26 2020-04-10 广东东硕科技有限公司 Application of 2-thiohydantoin compound or salt thereof
CN110983309B (en) * 2019-12-26 2023-01-03 广东东硕科技有限公司 Application of 2-thiohydantoin compound or salt thereof
CN111593378A (en) * 2020-04-20 2020-08-28 常州新纪元材料科技有限公司 Preparation of high corrosion-resistant alkaline zinc-nickel alloy electroplating solution and components of additive
CN113249766A (en) * 2021-04-29 2021-08-13 江苏师范大学 High-strength coating for repairing metal parts and preparation method thereof

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