CN103510130A - Trivalent hard chromium electroplating method - Google Patents

Trivalent hard chromium electroplating method Download PDF

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Publication number
CN103510130A
CN103510130A CN201210210952.7A CN201210210952A CN103510130A CN 103510130 A CN103510130 A CN 103510130A CN 201210210952 A CN201210210952 A CN 201210210952A CN 103510130 A CN103510130 A CN 103510130A
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electroplating
solution
chromium
trivalent
trivalent chromium
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CN103510130B (en
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毛祖国
李家柱
丁运虎
孙宁
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CHINA NORTH INDUSTRY NEW TECHNOLOGY PROMOTION INSTITUTE
Peking Blue Li Jiamei Chemical Science And Technology Center
WUHAN INST OF MATERIAL PROTECTION
Wuhan Research Institute of Materials Protection
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CHINA NORTH INDUSTRY NEW TECHNOLOGY PROMOTION INSTITUTE
Peking Blue Li Jiamei Chemical Science And Technology Center
WUHAN INST OF MATERIAL PROTECTION
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Priority to CN201210210952.7A priority Critical patent/CN103510130B/en
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Abstract

The present invention discloses an electroplating method for electroplating a trivalent hard chromium plating layer on iron and steel, wherein a DSA anode and a sulfuric acid system trivalent chromium solution are adopted, a temperature of about 50 DEG C and current density of 35-65 A/dm<2> are adopted, a soft starting process that change of current and a tank voltage is controlled during an electroplating process is adopted, and the pH value is maintained in the specified range (the pH value is 0.9-2.1) to obtain the trivalent chromium plating layer with a thickness of more than 80 mum, wherein the plating layer hardness achieves more than HV870, the current efficiency is more than 35%, the plating coating rate can be up to 2 mum/min, and the plating layer bonding force passes through the thermal shock test (200 DEG C heating, and salt water quenching). According to the present invention, the process method that the trivalent hard chromium electroplating replaces the sexvalent hard chromium electroplating with a characteristic of serious environment pollution is provided, and problems that the thick plating layer can not be obtained through the existing trivalent chromium electroplating technology, the plating layer and substrate bonding force is poor, and the like are solved.

Description

Trivalent chromium hard chrome electro-plating method
Technical field the present invention relates to trivalent chromium vitriol as the Technology of the durionise of main salt
Technical background
Sexavalent chrome chromium plating is one of most widely used plating in electroplating industry, have a large capacity and a wide range, in iron and steel, aluminium, plastics, copper alloy and Zinc Alloy Die Castings, all want decorative chromium plating, the electroplating parts that function is electroplated (hard chrome) comprises the manufacture, cutting tool of hydraulic cylinder and plunger, bent axle, printing plate/cylinder, internal combustion engine, mould of plastics and glass fibre workpiece etc., also for repairing the workpiece of wearing and tearing, for example reparation of cylinder, mould, cylinder and bent axle.Sexavalent chrome coating has good hardness, wear resistance, corrosion resistance nature and ornamental, not only for decorative coating, and a large amount of reparations for functional coating and workpiece etc., also can utilize tiny crack chromium layer to adopt sexavalent chrome (chromic acid) as main plating raw material as lubrication coating application (hard chrome) traditional chromium plating technology always, sexavalent chrome coating, Bai Liang, hardness are high, wear-resistant and Corrosion Protection is good, and technique is simple, easy to maintenance.But sexavalence chromium plating is the most serious, one of source of pollution of the most unmanageable electroplating industry.Chromium is one of necessary element of biological normal metabolic process, and scarce chromium will cause the metabolism such as sugar, fat chaotic, but chromium too high levels causes serious harm to biological and people's health.USEPA (EPA) is defined as sexavalent chrome one of toxicant of 17 kinds of highly dangerous.Chromium exists with trivalent and sexavalence form in water, and wherein chromic toxicity is very large, is approximately chromic 100 times, if chromic content, over the concentration of 0.1 mg/litre, will produce toxic action to human body in water.Sexavalent chrome has serious pungency to skin, can cause skin ulcer, and long-term absorption can cause the diseases such as squamous cell carcinoma, sarcoma and gland cancer.Chromic waste water, refuse can not be at nature natural degradations as the prussiate, it is in biological and human body inner accumulated, can cause the harm of chronicity, be the extremely strong strong carcinogenic substance of a kind of toxicity, is also serious corrosive medium and the material of heavily contaminated environment.China each department have a large amount of hexavalent chromium plating tank liquors, total amount is estimated more than ten million ton, the water of severe contamination China, soil and atmospheric environment, annual more than 60% is for the treatment of chromyl waste water, waste gas and refuse for administering the expense of electroplating wastewater, the Environmental Pollution Loss that hexavalent chromium plating causes, wastewater treatment expense and personnel's occupational disease are saved your breath also more than tens billion of Renminbi.
In order to replace the sexavalent chrome chromium plating of severe contamination, people have carried out much research, comprise the researchs such as low concentration chromium plating, nickel-base alloy coating and trivalent chromium plating, wherein with trivalent chromium plating, enliven the most and are hopeful most.
The chromium coating white color that trivalent chromium chrome plating obtains is bright, hardness is very high and mechanical property is good, its dispersing property and covering power are all far away higher than sexavalent chrome, and in same current density situation, its sedimentation velocity is the twice of sexavalent chrome chromium plating, and current efficiency is also higher than sexavalent chrome.But, the topmost advantage of trivalent chromium chrome plating is that its toxicity only has chromic 1/100th, in general trivalent chromium chrome plating solution the content of trivalent chromic ion only have hexavalent chromium in sexavalent chrome chromium plating tank liquor 1/7th even still less, and waste water is easy to process, be that a kind of replacement is widely used but one of promising electroplating technology of tool of the sexavalent chrome chromium plating of serious environment pollution.But, trivalent chromium plating also exists some problems, mainly because its impurity tolerance is very low, when the cumulative concentration in trivalent chromium coating bath such as the metal ion such as zinc, copper and mickel reaches 10~100ppm, chromium coating quality will decline, thereby cause its stability bad, be difficult to drop into production application.The hexavalent chromium producing at anode also can have a strong impact on the quality of coating, so that cannot produce qualified product completely.The trivalent chromium bath of selling on open market, can not plate thick chromium layer, at the aspects such as stable and maintenance of tank liquor, exists larger problem.The trivalent chromium plating Technology that various aspects of performance can substitute hexavalent chromium plating also has not seen reported.For this reason, the trivalent chromium plating technology of the stable thickness coating (namely hard chromium) of development research has great importance.
Summary of the invention
The invention provides a kind of stable trivalent chromium plating technology that can produce thickness coating (namely hard chrome), comprise the Electroplating Process Control Techniques of solution preparation and hard chromium coating.Cathode current density surpasses 30%, and coating hardness reaches 870HV, 1058HV after thermal treatment, and the white bright zero defect of Deposit appearance, neutral salt spray not corrosion in 240 hours, 300 ℃ of thermal shock tests, without cracking.
The invention provides a kind of trivalent chromium vitriol hard chrome electroplating solution and compound method thereof, mainly comprise the main salt of trivalent chromium, complexing agent, buffer reagent, catalyst component.
The main salt of trivalent chromium plating solution is chromium sulphate or potassium chromium sulfate, and the content of trivalent chromic ion is 5~40g/L,
Complexing agent is nitrilotriacetic acid(NTA), oxalic acid, oxysuccinic acid, glycine, formic acid, acetic acid or its sodium salt sylvite, and preparation plating solution, at least adopts wherein a kind of complexing agent.Content is 1~60g/L,
Buffer reagent is boric acid, Tai-Ace S 150, phthalic acid, preparation plating solution, at least adopt wherein a kind of buffer reagent, content is 50~180g/L, catalyzer is Potassium Bromide, Repone K, Neutral ammonium fluoride, Potassium monofluoride and Sodium Fluoride, preparation plating solution at least adopts wherein a kind of catalyzer 10~30g/, and conducting salt is that vitriolate of tartar or sodium sulfate are 0~80g/L.All the other are deionized water.
The pH value of described solution is 0.6~2.1, can adjust acidity with sodium carbonate or salt of wormwood and sulfuric acid, preferably 0.8~1.8.
Compound method: first the deionized water that measures 2/3rds put into container and be heated to more than 60 ℃, main salt is put into deionized water while stirring, then putting into successively complexing agent, catalyzer and buffer reagent, after all dissolving, retaining stand-by.The deionized water that is less than metering 1/3rd is put into other container and is heated to more than 60 ℃, buffer reagent is put into while stirring to the deionized water of this container, after all dissolving, pour the solution in second container into first container, be heated to 95 ℃ of left and right, insulation is more than 2 hours, and when temperature cools to technological temperature naturally, trivalent chromium bath has been prepared.
Electroplating parameter control method:
The current density range of described solution hard chrome is 25~75A/dm 2' current density is preferably controlled at 35~60A/dm 2.Current density is too little, does not reach the deposition potential of chromium; Too large, coating stress is large, easily peeling.
Within the scope of 0.8-2.1, along with pH value raises, range of current expands, and electroplating efficiency is higher simultaneously; PH value rises, and solution activation performance is inadequate, and peeling easily appears in coating, is not suitable for long-time plating; Span of control: pH value is better between being controlled at 1.2~1.6.
The temperature of electroplating solution is controlled: temperature is low, and covering power is good, and sedimentation velocity is fast, but temperature is too low, and mass transfer velocity is slower, the long-term high-end peeling that easily burns of continuous electroplating; When temperature is higher, can adopt higher current density, but the covering power of plating solution and sedimentation velocity decline; The temperature range of described solution is normal temperature~60 ℃, and the preferred range that hard chrome is electroplated is 45~55 ℃, and more preferably temperature range is 40~50 ℃.
While adopting described solution to electroplate, must carry out the pre-treatment of degreasing and rust removal and activation.
Electroplate starting method: in order to ensure that coating and substrate have good bonding force, must adopt soft-start method to electroplate.The implication of soft start of the present invention be at 1 minute in 5 minutes, the 0 ampere current density that be progressively increased to appointment of the current density applying from starting.Or from 0 volt of initial electroplating voltage, in 1 minute to 5 minutes, progressively pressure regulation, under the voltage of appointment, is carried out plating.
Cannot adopt movable cathode and solution forced-flow:
In order to ensure that coating and base metal have good bonding force, in electroplating process, electroplating cathode (namely plating workpiece) can not move, and solution can not adopt circulating filtration, mechanical stirring etc. to cause the additive method of solution forced-flow.
Anode adopts iridium tantalum coating Ti-alloy anode.
Performance test data, cathode current density surpasses 30%, coating hardness 870HV, 1058HV after thermal treatment, the white bright zero defect of Deposit appearance, neutral salt spray not corrosion in 240 hours, 300 degree thermal shock tests, without cracking.
Power supply can also can be used the pulse power with direct supply, and the sedimentation velocity of direct supply is faster, and the settled layer surface of the pulse power is finer and closely woven.
Embodiment 1 solution preparation
Adopt potassium chromium sulfate 230g/L, buffer reagent 120g/L, complexing agent 30g/L, catalyzer 20g/L, conducting salt 50g/L, as follows obtain solution.
First the deionized water that measures 2/3rds put into container and be heated to more than 60 ℃, main salt is put into deionized water while stirring, then putting into successively complexing agent, catalyzer and buffer reagent, after all dissolving, retaining stand-by; .The deionized water that is less than metering 1/3rd is put into other container and is heated to more than 60 ℃, buffer reagent is put into while stirring to the deionized water of this container, after all dissolving, pour the solution in second container into first container, be heated to 95 ℃ of left and right, be incubated more than 2 hours, when temperature cools to technological temperature naturally, adopt deionized water constant volume, trivalent chromium bath has been prepared.
No. 45 steel shaft-like parts of embodiment 2 base material (the long 200mm of diameter 30*)
Mechanical polishing---the upper hanger of pre-chemical degreasing 10min-, shield is installed, and---------------pure water is washed, and------hanger is unloaded in secondary washing---pure water is washed---to durionise (directly starting to the current density of appointment) to activation 1min to anode electrolysis degreasing 5min in secondary washing in secondary washing
Trivalent chromium coating peeling comes off.
Embodiment 3 base material 65Mn steel shaft-like parts (the long 200mm of diameter 30*, wherein in the middle of parcel plating, 50mm is long)
Mechanical polishing---the upper hanger of pre-chemical degreasing 10min-, shield is installed, and---------------pure water is washed, and------hanger is unloaded in secondary washing---pure water is washed---to durionise (mechanical stirring) to activation 1min to anode electrolysis degreasing 5min in secondary washing in secondary washing
Craze of coating.
Embodiment 4: base material 65Mn steel standard test piece (100*50*2mm)
Mechanical polishing---the upper hanger of pre-chemical degreasing 10min-, shield is installed, and---------------pure water is washed, and------hanger is unloaded in secondary washing---pure water is washed---to durionise (pneumatic blending) to activation 1min to anode electrolysis degreasing 5min in secondary washing in secondary washing
Craze of coating peeling.
No. 45 steel shaft-like parts of embodiment 5 base material (the long 200mm of diameter 30*)
Technical process:
Mechanical polishing---the upper hanger of pre-chemical degreasing 10min-, shield is installed, and------secondary washing---activates 1min---secondary washing---pure water is washed---durionise (soft start to anode electrolysis degreasing 5min, it is static that negative electrode keeps, and solution is without stirring)---secondary washing---pure water is washed---unloading hanger---dehydrogenation
Durionise condition: 50 ℃, 90A, PH=1.4, electroplates 20min, and evenly, thickness reaches 44um to coating light, and hardness reaches 880HV (1050HV after thermal treatment), and bonding force is by thermal shock test (200 ℃ of heating, salt water quick cooling).
Implement real 6: base material 65Mn steel shaft-like part (the long 200mm of diameter 30*, wherein in the middle of parcel plating, 50mm is long) technical process:
Mechanical polishing---the upper hanger of pre-chemical degreasing 10min-, shield is installed, Fei Du position insulation processing---anode electrolysis degreasing 5min---secondary washing---activation 1min---secondary washing---pure water is washed---durionise (soft start, it is static that negative electrode keeps, and solution is without stirring)---secondary washing---pure water is washed---unloading hanger---dehydrogenation
Durionise condition: 50 ℃, 22A, PH=1.4, electroplates 20min, and evenly, thickness reaches 45um to coating light, and hardness reaches 870V (1048HV after thermal treatment), and bonding force is by thermal shock test (200 ℃ of heating, salt water quick cooling).
Embodiment 7: base material 65Mn steel standard test piece (100*50*2mm)
Technical process:
Mechanical polishing---the upper hanger of pre-chemical degreasing 10min-, shield is installed, and------secondary washing---activates 1min---secondary washing---pure water is washed---durionise (soft start to anode electrolysis degreasing 5min, it is static that negative electrode keeps, and solution is without stirring)---secondary washing---pure water is washed---unloading hanger---dehydrogenation
Durionise condition: 50 ℃, 45A, PH=1.4, electroplates 20min, and evenly, mean thickness reaches 40um to coating light, and hardness reaches 890V (1030HV after thermal treatment), and bonding force is by thermal shock test (200 ℃ of heating, salt water quick cooling).

Claims (10)

1. a trivalent chromium hard chrome electroplating solution, mainly comprises trivalent chromium Liu Suanyan complexing agent, catalyzer, buffer reagent and conducting salt.
2. electroplating solution as claimed in claim 1, wherein trivalent chromium vitriol can be chromium sulphate or potassium chromium sulfate, the concentration 5~40g/L of trivalent chromic ion in solution.
3. electroplating solution as claimed in claim 1, wherein, complexing agent can be nitrilotriacetic acid(NTA), oxalic acid, oxysuccinic acid, glycine, formic acid, acetic acid or its sodium salt and sylvite, at least contain wherein a kind of complexing agent, and content is 1~60g/L.
4. electroplating solution as claimed in claim 1, wherein catalyzer can be Potassium Bromide, Potassium monofluoride, Neutral ammonium fluoride and Sodium Fluoride, at least contains wherein a kind of catalyzer, content is 5~50g/L.
5. electroplating solution as claimed in claim 1, wherein buffer reagent can be Tai-Ace S 150, boric acid, phthalic acid, at least contains wherein a kind of buffer reagent, content is 50~150g/L.
6. electroplating solution as claimed in claim 1, wherein conducting salt can be vitriolate of tartar and sodium sulfate, content is 0~80g/L.
7. the pH value of the electroplating solution as described in claim as arbitrary in right 1~6 is 0.6~2.1.
8. the pH value of the electroplating solution as described in claim as arbitrary in right 1~6 is 0.8~1.8.
9. the compound method of a trivalent chromium solutions, it is characterized in that first the deionized water that measures 2/3rds being put into container and being heated to more than 60 ℃, main salt is put into deionized water while stirring, then put into successively complexing agent, catalyzer and buffer reagent, after all dissolving, retain stand-by; The deionized water that is less than metering 1/3rd is put into other container and is heated to more than 60 ℃, buffer reagent is put into while stirring to the deionized water of this container, after all dissolving, pour the solution in second container into first container, be heated to about 95 ℃ insulations more than 2 hours, when temperature cools to technological temperature naturally, use deionized water constant volume, trivalent chromium bath has been prepared.
10. an electro-plating method for trivalent chromium hard chrome, comprises the steps:
(1) preparation trivalent chromium hard chrome electroplating solution;
(2) workpiece pre-treatment, must to workpiece carry out oil removing rust cleaning cleaning up, dilute sulphuric acid activation; ,
(3) workpiece dress is put into electroplating solution after hanging;
(4) electroplate to start and must adopt soft start, i.e. time 1-5min, current potential is progressively changed to selection of appointed by 0V; Current density is progressively changed to given current density by 0A;
(5) electroplating parameter control current density range is 25~75A/dm 2, current density is preferably controlled at 35~60A/dm 2;
(6) electroplating solution temperature control plating parameter control solution temperature is controlled as normal temperature~60 ℃, and the preferred range of hard chrome plating is 40~55 ℃, and more preferably temperature range is 45~50 ℃;
(7) in electroplating process, electroplating cathode (namely plating workpiece) can not move, and solution can not adopt circulating filtration, mechanical stirring etc. to force flow of solution method.
CN201210210952.7A 2012-06-26 2012-06-26 Trivalent hard chromium electro-plating method Expired - Fee Related CN103510130B (en)

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CN105063676A (en) * 2015-08-17 2015-11-18 内蒙古第一机械集团有限公司 Method for electroplating hard chromium by using trivalent chromium
CN105386089A (en) * 2015-12-25 2016-03-09 武汉迪赛环保新材料股份有限公司 Trivalent chromium hard chromium electroplating solution and application of trivalent chromium hard chromium electroplating solution in hard chromium electroplating
CN107675215A (en) * 2017-08-25 2018-02-09 刘建伟 A kind of gear electroplating solution
CN109371433A (en) * 2018-10-31 2019-02-22 中国人民解放军陆军装甲兵学院 A kind of preparation method of nanocrystalline trivalent chromium composite deposite plating solution and composite deposite
CN111020655A (en) * 2019-11-25 2020-04-17 厦门大学 Preparation method and application of zirconium alloy material with chromium coating
CN112609216A (en) * 2020-11-30 2021-04-06 中船重工重庆液压机电有限公司 Electroplating method for improving corrosion resistance

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103849908A (en) * 2014-02-17 2014-06-11 惠州大亚湾达志精细化工有限公司 Trivalent chromium plating liquid and method for electrically depositing chromium plating layer in trivalent chromium plating liquid
CN103849908B (en) * 2014-02-17 2016-04-20 惠州大亚湾达志精细化工有限公司 A kind of trivalent chromium bath and in trivalent chromium bath the method for electrodeposited chromium coating
CN105063676A (en) * 2015-08-17 2015-11-18 内蒙古第一机械集团有限公司 Method for electroplating hard chromium by using trivalent chromium
CN105386089A (en) * 2015-12-25 2016-03-09 武汉迪赛环保新材料股份有限公司 Trivalent chromium hard chromium electroplating solution and application of trivalent chromium hard chromium electroplating solution in hard chromium electroplating
CN107675215A (en) * 2017-08-25 2018-02-09 刘建伟 A kind of gear electroplating solution
CN109371433A (en) * 2018-10-31 2019-02-22 中国人民解放军陆军装甲兵学院 A kind of preparation method of nanocrystalline trivalent chromium composite deposite plating solution and composite deposite
CN111020655A (en) * 2019-11-25 2020-04-17 厦门大学 Preparation method and application of zirconium alloy material with chromium coating
CN112609216A (en) * 2020-11-30 2021-04-06 中船重工重庆液压机电有限公司 Electroplating method for improving corrosion resistance

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