CN105887056A - Chemical nickel plating method for surface of magnesium alloy - Google Patents
Chemical nickel plating method for surface of magnesium alloy Download PDFInfo
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- CN105887056A CN105887056A CN201610259218.8A CN201610259218A CN105887056A CN 105887056 A CN105887056 A CN 105887056A CN 201610259218 A CN201610259218 A CN 201610259218A CN 105887056 A CN105887056 A CN 105887056A
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- magnesium alloy
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1806—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by mechanical pretreatment, e.g. grinding, sanding
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1837—Multistep pretreatment
Abstract
The invention discloses a chemical nickel plating method for the surface of a magnesium alloy. The method includes the following specific steps that the magnesium alloy is subjected to mechanical polishing, oil removal, oxidation film removal and activation and then put into a chemical plating solution, the temperature of the plating solution ranges from 80 DEG C to 90 DEG C, the pH value of the plating solution is adjusted with ammonia water to range from 5.0 to 6.5, and the plating time ranges from 30 min to 90 min; and the chemical plating solution comprises 10-25 g/L of nickel sulfate, 10-25 g/L of sodium hypophosphite, 5-20 g/L of ammonium bifluoride, 10-30 mL/L of hydrofluoric acid, 5-20 g/L of a complexing agent and 0.01-0.2 g/L of a stabilizing agent. The magnesium alloy is put into a passivation solution to be soaked for 1 minute to 3 minutes at the room temperature; and then the magnesium alloy is washed and dried and is subjected to heat treatment for 1 hour to 3 hours at the temperature of 250 DEG C to 350 DEG C, and a plating layer with the metallic luster is obtained on the surface of the magnesium alloy. The plating layer obtained through the chemical nickel plating method has the excellent corrosion resistance, the self-corrosion potential is increased greatly relative to that of a base body, and the self-corrosion current is lowered remarkably.
Description
Technical field
The invention belongs to field of metal surface treatment technology, a kind of method relating to magnesium alloy surface chemical nickel plating.
Background technology
Magnesium and magnesium alloy are metals the lightest in structural material, have light weight, specific strength is high, thermal diffusivity is good, electromagnetic wave shielding is good, excellent shock resistance and the characteristic such as be easily recycled, and is widely used in military project and civilian production field.Magnesium alloy have higher heat conductivity and diamagnetic interference, can die casting thin-wall part and the advantage such as be easily recycled, thus people wait in expectation and are applied to automobile mechanical and electronic product with magnesium alloy as light material, alleviate product weight with expectation, save the energy, reduction pollution and improve environment.Exploitation magnesium alloy, China not only has huge resources advantage, the hugest market demand.Developed country also greatly develops the application of magnesium alloy materials.
But the chemical property of magnesium and magnesium alloy is active; at room temperature can oxidation by air; the oxide-film generated is loose, porous; the corrosion resistance causing magnesium and magnesium alloy is excessively poor; cannot play a good protection matrix, corrosion resistance difference determines it and could have to enter in industry-by-industry after being first processed.
Chemical nickel plating is possible not only to obtain coating in uniform thickness on baroque workpiece, it is also possible to obtain the coating of high corrosion resistance and wearability.Requiring that surface has the occasion of electric conductivity, heat conductivity, soldering for those, chemical nickel plating process on magnesium alloy is a kind of method that surface that cannot substitute processes, and is also one of maximally effective safeguard procedures of corrosion resisting property improving Mg alloy surface.Traditional handicraft is leaching zinc after oil removing, re-plating copper, last chemical nickel plating.This complex process efficiency is low.Technique after improving now is chromic acid dipping and hydrofluoric acid treatment after alkaline degreasing, finally carries out chemical nickel plating.
Summary of the invention
A kind of method that it is an object of the invention to provide magnesium alloy surface chemical nickel plating, thus improve the corrosion resisting property of magnesium alloy.
A kind of method of magnesium alloy surface chemical nickel plating, it is characterised in that specifically comprising the following steps that of the method
A. magnesium alloy is carried out mechanical grinding, mechanical polishing, then ultrasonic waves for cleaning；
B. with heat alkali liquid, magnesium alloy is carried out oil removing；Temperature controls at 55-65 DEG C, time 10-20min；
C. chemical deoxidization film: clean magnesium alloy by acid solution, temperature is room temperature, time 3-10min；
D. magnesium alloy is activated in a solution of hydrofluoric acid, soak；Temperature is room temperature, time 5-15 min；
E. chemical plating: put in chemical plating fluid by above-mentioned treated magnesium alloy, temperature 80-90 DEG C of plating solution, the pH value ammonia of plating solution is adjusted to 5.0-6.5, and plating time is 30-90min；Component and content thereof that described chemical plating fluid is comprised is: nickel sulfate 10-25g/L, sodium hypophosphite 10-25g/L, ammonium acid fluoride 5-20g/L, Fluohydric acid. 10-30mL/L, chelating agent 5-20g/L, stabilizer 0.01-0.2g/L；
F. being put into by magnesium alloy in passivating solution and soak, temperature is room temperature, soaks 1-3 minute；Then carrying out washing to dry, 250 ~ 350 DEG C of heat treatments 1-3 hour, Mg alloy surface obtained the coating with metallic luster.
Described mechanical grinding successively with 800,1000, the carborundum paper of 1500# polishes.
Described mechanical polishing is polished with dehydrated alcohol on polishing cloth.
Component and content thereof that described heat alkali liquid is comprised is: sodium hydroxide 30-50g/L, sodium phosphate 5-20g/L.
Component and content thereof that described acid solution is comprised is: phosphatase 11 0-20mL/L, acetic acid 10-30mL/L.
One or more in tartaric acid, malic acid, citric acid and sodium citrate chosen by described chelating agent.
One or more in sodium lauryl sulphate, dodecyl sodium sulfate and thiourea chosen by described stabilizer.
Containing Fluohydric acid. 200-400mL/L in described hydrofluoric acid solution.
Described passivating solution be mass concentration be chromic acid and the phosphorus aqueous acid of 1-10%.
It is an advantage of the current invention that: chemical plating fluid composition is simple, preparation is convenient, and solution composition good stability is easy to operate.Surface pretreatment process is simple, and after using pre-treating technology to process magnesium alloy, the corrosion resistance of coating of gained is excellent, and corrosion potential is greatly improved relative to matrix, and corrosion current significantly reduces.Coating surface light is smooth, and thickness is uniform, has good corrosion resistance.This technology can be applicable in automobile, weaponry lightweight.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the embodiment of the present invention 1 gained magnesium alloy chemical coating.
Fig. 2 is the elementary analysis figure of the embodiment of the present invention 1 gained magnesium alloy chemical coating.
Fig. 3 is the embodiment of the present invention 1 gained magnesium alloy chemical coating electrochemical tests figure in the NaCl solution that mass fraction is 3.5%.
Detailed description of the invention
Embodiment 1
Magnesium alloy materials is as cast condition AZ91D alloy, and sample size is 25m × 15mm × 3mm.
A. mechanical grinding polishing, ultrasonic waves for cleaning
Successively with 800,1000, the carborundum paper of 1500# polishes, to ensure that matrix has identical surface roughness；Polishing cloth is polished with dehydrated alcohol, matrix over oxidation can be avoided；Carry out ultrasonic waves for cleaning in acetone, control time: 10min.
B. alkali cleaning, solution preparation and operating condition are as follows:
Sodium hydroxide 45g/L, sodium phosphate 10g/L, temperature 55 DEG C, time 15min.
C. pickling, solution preparation and operating condition are as follows:
Phosphatase 11 5mL/L, acetic acid 20mL/L, room temperature, time 5min.
D. activating, solution preparation and operating condition are as follows:
Fluohydric acid. 350mL/L, room temperature, the time 10
min。
E. chemical composition and the formulation by weight thereof of preparing this plating solution are as follows: nickel sulfate 20g/L, sodium hypophosphite 20g/L, ammonium acid fluoride 10g/L, sodium citrate 10g/L, Fluohydric acid. 20mL/L, dodecyl sodium sulfate 0.1g/L
F. subsequently into chemical plating process program, putting in above-mentioned plating solution by above-mentioned treated magnesium alloy sample, it is 6.5 that temperature controls at the pH value of 85 DEG C of solution, and plating time is 60 minutes.
The most then magnesium alloy is put in passivating solution and soak.
The most then wash, and heat treatment 2 hours at a temperature of 300 DEG C；Thickness of coating is 20 microns.The corrosion potential of AZ91D magnesium alloy raises, and corrosion current reduces, and anti-corrosion capability is obviously enhanced.
Embodiment 2
Magnesium alloy materials is as cast condition AZ91D alloy, and sample size is 25m × 15mm × 3mm.
A. mechanical grinding polishing, ultrasonic waves for cleaning
Successively with 800,1000, the carborundum paper of 1500# first polishes；Then it is polished with dehydrated alcohol on polishing cloth；Carry out ultrasonic waves for cleaning in acetone, control time: 10min.
B. alkali cleaning, solution preparation and operating condition are as follows:
Sodium hydroxide 45g/L, sodium phosphate 10g/L, temperature 65 DEG C, time 15min.
C. pickling, solution preparation and operating condition are as follows:
Phosphatase 11 5mL/L, acetic acid 20mL/L, room temperature, time 1min.
D. activating, solution preparation and operating condition are as follows:
Fluohydric acid. 300mL/L, room temperature, time 8min.
E. chemical plating solution is prepared: nickel sulfate 20g/L, sodium hypophosphite 15g/L, ammonium acid fluoride 10g/L, sodium citrate 10g/L, Fluohydric acid. 12mL/L, tartaric acid 2.5g/L, thiourea 0.01g/L.
F. subsequently into chemical plating process program, putting in above-mentioned plating solution by above-mentioned treated magnesium alloy sample, it is 6.5 that temperature controls at the pH value of 85 DEG C of solution, and plating time is 60 minutes.
The most then magnesium alloy is put in passivating solution and soak.
The most then wash, and heat treatment 1 hour at a temperature of 300 DEG C；Coating surface bright in color, thickness is uniform.The corrosion potential of AZ91D magnesium alloy raises, and corrosion current reduces, and anti-corrosion capability is obviously enhanced.
Embodiment 3
Magnesium alloy materials is as cast condition AZ91D alloy, and sample size is 25m × 15mm × 3mm.
A. mechanical grinding polishing, ultrasonic waves for cleaning
Successively with 800,1000, the carborundum paper of 1500# first polishes；Then it is polished with dehydrated alcohol on polishing cloth；Carry out ultrasonic waves for cleaning in acetone, control time: 10min.
B. alkali cleaning, solution preparation and operating condition are as follows:
Sodium hydroxide 45g/L, sodium phosphate 10g/L, temperature 65 DEG C, time 15min.
C. pickling, solution preparation and operating condition are as follows:
Phosphatase 11 5mL/L, acetic acid 20mL/L, room temperature, time 2min.
D. activating, solution preparation and operating condition are as follows:
Fluohydric acid. 350mL/L, room temperature, time 5 min.
E. chemical plating solution is prepared: nickel sulfate 20g/L, sodium hypophosphite 15g/L, ammonium acid fluoride 10g/L, citric acid 10g/L, malic acid 2g/L, Fluohydric acid. 10mL/L, thiourea 0.01g/L,
F. subsequently into chemical plating process program, putting in above-mentioned plating solution by above-mentioned treated magnesium alloy sample, it is 6.5 that temperature controls at the pH value of 90 DEG C of solution, and plating time is 90 minutes.
The most then magnesium alloy is put in passivating solution and soak.
The most then wash, and heat treatment 1 hour at a temperature of 300 DEG C；Last coating surface bright in color, thickness is uniform.The corrosion potential of AZ91D magnesium alloy raises, and corrosion current reduces, and anti-corrosion capability is obviously enhanced.
Embodiment 4
Magnesium alloy materials is as cast condition AZ91D alloy, and sample size is 25m × 15mm × 3mm.
A. mechanical grinding polishing, ultrasonic waves for cleaning
Successively with 800,1000, the carborundum paper of 1500# first polishes；Then it is polished with dehydrated alcohol on polishing cloth；Carry out ultrasonic waves for cleaning in acetone, control time: 10min.
B. alkali cleaning, solution preparation and operating condition are as follows:
Sodium hydroxide 45g/L, sodium phosphate 10g/L, temperature 55 DEG C, time 15min.
C. pickling, solution preparation and operating condition are as follows:
Phosphatase 11 5mL/L, acetic acid 20mL/L, room temperature, 40 seconds time.
D activates, and solution preparation and operating condition are as follows:
Fluohydric acid. 220mL/L, room temperature, the time 10
min。
E. chemical plating solution is prepared: nickel sulfate 15g/L, sodium hypophosphite 14g/L, ammonium acid fluoride 10g/L, sodium citrate 5g/L, citric acid 5g/L, Fluohydric acid. 10mL/L, sodium lauryl sulphate 0.01g/L.
F. subsequently into chemical plating process program, putting in above-mentioned plating solution by above-mentioned treated magnesium alloy sample, it is 6.5 that temperature controls at the pH value of 90 DEG C of solution, and plating time is 60 minutes.
The most then magnesium alloy is put in passivating solution and soak.
The most then wash, and heat treatment 2 hours at a temperature of 300 DEG C；Last coating surface bright in color, thickness is uniform.The corrosion potential of AZ91D magnesium alloy raises, and corrosion current reduces, and anti-corrosion capability is obviously enhanced.
Claims (9)
1. the method for a magnesium alloy surface chemical nickel plating, it is characterised in that specifically comprising the following steps that of the method
A. magnesium alloy is carried out mechanical grinding, mechanical polishing, then ultrasonic waves for cleaning；
B. with heat alkali liquid, magnesium alloy is carried out oil removing；Temperature controls at 55-65 DEG C, time 10-20min；
C. chemical deoxidization film: clean magnesium alloy by acid solution, temperature is room temperature, time 3-10min；
D. magnesium alloy is activated in a solution of hydrofluoric acid, soak；Temperature is room temperature, time 5-15 min；
E. chemical plating: put in chemical plating fluid by above-mentioned treated magnesium alloy, temperature 80-90 DEG C of plating solution, the pH value ammonia of plating solution is adjusted to 5.0-6.5, and plating time is 30-90min；Component and content thereof that described chemical plating fluid is comprised is: nickel sulfate 10-25g/L, sodium hypophosphite 10-25g/L, ammonium acid fluoride 5-20g/L, Fluohydric acid. 10-30mL/L, chelating agent 5-20g/L, stabilizer 0.01-0.2g/L；
F. being put into by magnesium alloy in passivating solution and soak, temperature is room temperature, soaks 1-3 minute；Then carrying out washing to dry, 250 ~ 350 DEG C of heat treatments 1-3 hour, Mg alloy surface obtained the coating with metallic luster.
2. the method for claim 1, it is characterised in that described mechanical grinding successively with 800,1000, the carborundum paper of 1500# polishes.
3. the method for claim 1, it is characterised in that described mechanical polishing is polished with dehydrated alcohol on polishing cloth.
4. the method for claim 1, it is characterised in that component and content thereof that described heat alkali liquid is comprised is: sodium hydroxide 30-50g/L, sodium phosphate 5-20g/L.
5. the method for claim 1, it is characterised in that component and content thereof that described acid solution is comprised is: phosphatase 11 0-20mL/L, acetic acid 10-30mL/L.
6. the method for claim 1, it is characterised in that one or more in tartaric acid, malic acid, citric acid and sodium citrate chosen by described chelating agent.
7. the method for claim 1, it is characterised in that one or more in sodium lauryl sulphate, dodecyl sodium sulfate and thiourea chosen by described stabilizer.
8. the method for claim 1, it is characterised in that containing Fluohydric acid. 200-400mL/L in described hydrofluoric acid solution.
9. the method for claim 1, it is characterised in that described passivating solution be mass concentration be chromic acid and the phosphorus aqueous acid of 1-10%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610259218.8A CN105887056A (en) | 2016-04-25 | 2016-04-25 | Chemical nickel plating method for surface of magnesium alloy |
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| CN201610259218.8A CN105887056A (en) | 2016-04-25 | 2016-04-25 | Chemical nickel plating method for surface of magnesium alloy |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107779942A (en) * | 2016-08-30 | 2018-03-09 | 昆山汉鼎精密金属有限公司 | Mg alloy surface electrochemical polish liquid and its processing method |
| CN107985608A (en) * | 2017-11-21 | 2018-05-04 | 武汉航空仪表有限责任公司 | A kind of method for preventing icing detector probe corrosion |
| CN108277512A (en) * | 2018-03-15 | 2018-07-13 | 新乡学院 | A kind of magnesium alloy surface activating process |
| CN111690931A (en) * | 2020-06-05 | 2020-09-22 | 中国科学院金属研究所 | Aluminum alloy surface multilayer composite coating and preparation method thereof |
| CN112725773A (en) * | 2020-12-21 | 2021-04-30 | 中国航天科工集团八五一一研究所 | Direct chemical nickel plating method universally used for AZ91D and ZK61M magnesium alloys |
| CN114774894A (en) * | 2022-03-30 | 2022-07-22 | 美诺精密汽车零部件(南通)有限公司 | Die casting surface treatment process based on image monitoring |
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| CN101760732A (en) * | 2009-11-16 | 2010-06-30 | 海洋王照明科技股份有限公司 | Chemical nickel plating process for surface of magnesium alloy and chemical nickel plating solution |
| CN105220133A (en) * | 2015-10-29 | 2016-01-06 | 无锡桥阳机械制造有限公司 | A kind of steel surface treatment process |
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2016
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Patent Citations (2)
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| CN101760732A (en) * | 2009-11-16 | 2010-06-30 | 海洋王照明科技股份有限公司 | Chemical nickel plating process for surface of magnesium alloy and chemical nickel plating solution |
| CN105220133A (en) * | 2015-10-29 | 2016-01-06 | 无锡桥阳机械制造有限公司 | A kind of steel surface treatment process |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107779942A (en) * | 2016-08-30 | 2018-03-09 | 昆山汉鼎精密金属有限公司 | Mg alloy surface electrochemical polish liquid and its processing method |
| CN107985608A (en) * | 2017-11-21 | 2018-05-04 | 武汉航空仪表有限责任公司 | A kind of method for preventing icing detector probe corrosion |
| CN108277512A (en) * | 2018-03-15 | 2018-07-13 | 新乡学院 | A kind of magnesium alloy surface activating process |
| CN111690931A (en) * | 2020-06-05 | 2020-09-22 | 中国科学院金属研究所 | Aluminum alloy surface multilayer composite coating and preparation method thereof |
| CN112725773A (en) * | 2020-12-21 | 2021-04-30 | 中国航天科工集团八五一一研究所 | Direct chemical nickel plating method universally used for AZ91D and ZK61M magnesium alloys |
| CN114774894A (en) * | 2022-03-30 | 2022-07-22 | 美诺精密汽车零部件(南通)有限公司 | Die casting surface treatment process based on image monitoring |
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