CN105803431A - Magnesium alloy chemical nickel plating solution and preparation method thereof, and nickel plating method - Google Patents
Magnesium alloy chemical nickel plating solution and preparation method thereof, and nickel plating method Download PDFInfo
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- CN105803431A CN105803431A CN201410852753.5A CN201410852753A CN105803431A CN 105803431 A CN105803431 A CN 105803431A CN 201410852753 A CN201410852753 A CN 201410852753A CN 105803431 A CN105803431 A CN 105803431A
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Abstract
The invention provides a magnesium alloy chemical nickel plating solution; the nickel plating solution contains a soluble nickel salt, a complexing agent, a buffering agent, a corrosion inhibitor, a reducing agent, a stabilizer and salicylaldehyde. The invention also provides a preparation method of the nickel plating solution and a magnesium alloy surface nickel plating method. Salicylaldehyde contained in the nickel plating solution can effectively reduce corrosion of a magnesium alloy zinc-dipping layer in the chemical nickel plating solution, promotes a reaction to be gently carried out, and is beneficial to deposition of a nickel layer, so as to improve plating layer density and solve the problems of pinholes and plating leakage. At the same time, with the addition of salicylaldehyde, the usage times of the nickel plating solution can be further prolonged.
Description
Technical field
The present invention relates to electroplating technology field, particularly relate to a kind of magnesium alloy surface chemical nickel plating liquid, preparation method and nickel plating process thereof.
Background technology
Magnesium alloy is constantly subjected to extensive concern because of performance and the rich in natural resources of its uniqueness, is taken as ep-type material again in this century and extremely praises highly.But owing to magnesium alloy plating technique is still immature, the problem of corrosion resistance difference becomes the major obstacle playing its superiority, thus greatly limit its larger range of popularization and application.
Therefore, Mg alloy surface carrying out effectively decoration anticorrosion is particularly important, existing conventional treatment technology has a plating, and magnesium alloy is in conventional bath solution and unstable, it is necessary to its surface carries out pretreatment so that it is adapt to routine plating environment.It is applicable to industrial pre-treating technology at present and has two big classes: heavy zinc method and direct electroless nickel method.Both approaches is all released by DowChemical company of the U.S. the earliest, and each used producer in practical probation process later, has carried out improvement in various degree all based on this, has developed into similar multiple way.What be seen in report has NorskHydro technique and WCM technique etc..
Heavy zinc method in order that dissolve the oxide of magnesium;Form hydroxide one layer thin at Mg alloy surface simultaneously, prevent the further oxidation of magnesium.Present specification is based on heavy zinc method, technical process therein is improved.The common technological process of heavy zinc method is: oil removing scale removal → activation → sink zinc → chemical nickel plating → electro-coppering/ni cr etc..
Under normal circumstances; magnesium alloy can with the acid/base solution vigorous reaction in process; nickel-plating liquid also can occur same vigorous reaction; but this is also unfavorable for nickel dam deposition on substrate surface; pin hole, plating leakage usually can be caused present; also make the adhesion of coating can not get ensureing simultaneously, bubble easily occurs, come off problem.
Summary of the invention
The present invention provides the chemical nickel-plating liquid of a kind of magnesium alloy, can relax magnesium alloy substrates reaction in nickel-plating liquid, makes reaction carry out gently, reaches better nickel plating effect, solves the phenomenon such as pin hole, plating leakage further.Meanwhile, nickel-plating liquid provided by the invention has longer life cycle.
A kind of chemically coating nickel by magnesium-alloy liquid of the present invention includes following component: soluble nickel salt, chelating agent, buffer agent, resist, reducing agent, stabilizer and salicylide.
The preparation method that present invention also offers a kind of chemically coating nickel by magnesium-alloy liquid, described method is add chelating agent, stabilizer, buffer agent and reducing agent in the aqueous solution of soluble nickel salt；Add resist and salicylide.
A kind of method that present invention also offers magnesium alloy surface chemical nickel plating, contacts with nickel-plating liquid including by the magnesium alloy through pre-treatment, must arrive surface and have the magnesium alloy substrates of nickel dam；Wherein, described nickel-plating liquid is magnesium alloy nickel-plating liquid of the present invention.
Containing salicylide in the chemically coating nickel by magnesium-alloy liquid of the present invention.Owing to magnesium alloy zinc-impregnating layer is at chemical nickel plating also middle meeting vigorous reaction, thus causing that nickel coating has the problems such as uneven or plating leakage.And salicylide contained in the nickel-plating liquid of the present invention can effectively reduce the corrosion in chemical nickel-plating liquid of the magnesium alloy zinc-impregnating layer, promote carrying out gently of reaction, thus ensureing plated layer compact degree, preventing pin hole and plating leakage phenomenon.Meanwhile, the salicylide of addition can extend nickel-plating liquid service life further.
Detailed description of the invention
Technical scheme relates to a kind of chemically coating nickel by magnesium-alloy liquid, and described nickel-plating liquid comprises following component: soluble nickel salt, chelating agent, buffer agent, resist, reducing agent, stabilizer and salicylide.
According to chemical nickel-plating liquid provided by the present invention, it is preferable that soluble nickel salt 15-25g/L, chelating agent 20-65g/L, buffer agent 10-20g/L, resist 10-30g/L, reducing agent 20-30g/L, stabilizer 0.001-0.003g/L and salicylide 2-7g/L.
According to chemical nickel-plating liquid provided by the present invention, it is preferable that described soluble nickel salt is one or more in nickel sulfate, Nickel dichloride.；Described chelating agent is one or more in ammonium citrate, ethylenediamine, sodium acetate, lactic acid, malic acid, citric acid, succinic acid, propanoic acid；Described buffer agent is boric acid；Described resist is one or more in Fluohydric acid., ammonium acid fluoride, sodium fluoride, potassium fluoride; when nickel-plating liquid adds appropriate fluoride resist; magnesium alloy substrates surface can be protected in nickel process; prevent excessive corrosion; especially can produce synergism with salicylide, reduce the corrosion in chemical nickel of the magnesium alloy zinc-impregnating layer further, it is ensured that the adhesion of coating; reduce coating to bubble, the probability come off；Described reducing agent is one or more in sodium hypophosphite, sodium borohydride, borine, hydrazine；Described stabilizer is one or more in thiourea, potassium thiocyanate, carbamide.
According to chemical nickel-plating liquid provided by the present invention, it is preferable that described chelating agent is one or more in ammonium citrate, ethylenediamine, sodium acetate, lactic acid.
According to chemical nickel-plating liquid provided by the present invention, it is preferable that the pH value of described nickel-plating liquid is 8-9.
The preparation method that present invention also offers a kind of chemically coating nickel by magnesium-alloy liquid, method described in described method is add chelating agent, stabilizer, buffer agent and reducing agent in the aqueous solution of soluble nickel salt；Add resist and salicylide.
According to preparation method provided by the present invention, it is preferable that described soluble nickel salt 15-25g/L, chelating agent 20-65g/L, buffer agent 10-20g/L, resist 10-30g/L, reducing agent 20-30g/L, stabilizer 0.001-0.003g/L and salicylide 2-7g/L.
According to preparation method provided by the present invention, it is preferable that described soluble nickel salt is one or more in nickel sulfate, Nickel dichloride.；Described chelating agent is one or more in ammonium citrate, ethylenediamine, sodium acetate, lactic acid, malic acid, citric acid, succinic acid, propanoic acid；Described buffer agent is boric acid；Described resist is one or more in Fluohydric acid., ammonium acid fluoride, sodium fluoride, potassium fluoride；Described reducing agent is one or more in sodium hypophosphite, sodium borohydride, borine, hydrazine；Described stabilizer is one or more in thiourea, potassium thiocyanate, carbamide.
According to preparation method provided by the present invention, it is preferable that finally use ammonia to regulate pH value between 8-9.
A kind of method that present invention also offers magnesium alloy surface chemical nickel plating, contacts with nickel-plating liquid including by the magnesium alloy through pre-treatment, must arrive surface and have the magnesium alloy substrates of nickel dam；It is characterized in that, described nickel-plating liquid is magnesium alloy nickel-plating liquid of the present invention.
Below in conjunction with embodiment, the present invention is further described in detail, but is not limited to this.
All raw materials in heretofore described embodiment are such as non-to be refered in particular to, and is commercially available prod.
Embodiment 1
1, chemically coating nickel by magnesium-alloy liquid is prepared
The aqueous solution of nickel sulfate adds ammonium citrate, ethylenediamine, sodium acetate, lactic acid, and thiourea, boric acid and sodium hypophosphite stir；Adding Fluohydric acid., ammonium acid fluoride and salicylide, finally using ammonia to regulate pH value is 8, can obtain nickel-plating liquid A1.Wherein, nickel sulfate 20g/L, ammonium citrate 25g/L, ethylenediamine 3g/L, sodium acetate 7g/L, lactic acid 10g/L, thiourea 0.002g/L, boric acid 15g/L, sodium hypophosphite 25g/L, Fluohydric acid. 8g/L, ammonium acid fluoride 10g/L and salicylide 4g/L.
2, Mg alloy surface nickel plating
1) base material pretreatment: selecting the trade mark is that the magnesium alloy of AZ91D is as base material, base material is put into (formula: sodium carbonate 20g/L in degreasing fluid, sodium phosphate 20g/L, sodium citrate 10g/L, sodium lauryl sulphate 1g/L), embathe at 20-30 DEG C 10 minutes, clean with tap water after taking-up, then with the phosphoric acid pickling of 300g/L.
2) activation: the magnesium alloy substrates after step 1 being processed immerses in activating solution (formula: phosphatase 11 80g/L, ammonium acid fluoride 90g/L), embathes 60 seconds, clean with tap water after taking-up at 20-30 DEG C.
3) heavy zinc: the magnesium alloy substrates obtained in step 2 is immersed in heavy zinc liquid (formula: zinc sulfate 30g/l, sodium pyrophosphate 120g/L, sodium carbonate 6g/L, potassium fluoride 2g/L, nickel sulfate 0.5g/L), embathes at 50 DEG C 10 minutes, clean with tap water after taking-up.
4) chemical nickel plating: being put into by the magnesium alloy substrates crossed through 1-3 step process in nickel-plating liquid A1, nickel-plating liquid temperature is 40 DEG C, takes out after soaking 20 minutes, obtains plating piece Y1 after cleaning with tap water.
Embodiment 2
The aqueous solution of nickel sulfate adds ammonium citrate, ethylenediamine, sodium acetate, lactic acid, and thiourea, boric acid and sodium hypophosphite stir；Adding Fluohydric acid., ammonium acid fluoride and salicylide, finally using ammonia to regulate pH value is 8.5, can obtain nickel-plating liquid A2.Wherein, nickel sulfate 18g/L, ammonium citrate 22g/L, ethylenediamine 2g/L, sodium acetate 6g/L, lactic acid 8g/L, thiourea 0.001g/L, boric acid 12g/L, sodium hypophosphite 22g/L, Fluohydric acid. 7g/L, ammonium acid fluoride 9g/L and salicylide 4g/L.
According to the method for embodiment 1, adopt nickel-plating liquid A2 that magnesium alloy is carried out nickel plating, obtain plating piece Y2.
Embodiment 3
Configure nickel-plating liquid A3 according to the method for embodiment 1, be distinctive in that: ammonium citrate 35g/L, simultaneously without ethylenediamine, sodium acetate and lactic acid.
According to the method for embodiment 1, adopt nickel-plating liquid A3 that magnesium alloy is carried out nickel plating, obtain plating piece Y3.
Embodiment 4
Configure nickel-plating liquid A4 according to the method for embodiment 1, be distinctive in that: with the malic acid of 10g/L, the succinic acid of 15g/L replaces the ethylenediamine in A1, sodium acetate, lactic acid.
According to the method for embodiment 1, adopt nickel-plating liquid A4 that magnesium alloy is carried out nickel plating, obtain plating piece Y4.
Embodiment 5
Configure nickel-plating liquid A5 according to the method for embodiment 1, be distinctive in that: substitute the ammonium hydrogen fluoride solution in A1 with sodium fluoride 10g/L.
According to the method for embodiment 1, adopt nickel-plating liquid A5 that magnesium alloy is carried out nickel plating, obtain plating piece Y5.
Comparative example 1
Except without salicylide, all the other are identical with embodiment 1.
Performance test and result
1, the mild response time is entered
Observe after nickel-plating liquid put into by base material and how long can enter mild reaction.
2, the nickel-plating liquid life-span
Observe and whether the nickel-plating liquid after using occurs precipitation.
3, nickel plating outward appearance
Whether coating is uniform to observe the magnesium alloy substrates outward appearance after nickel plating, if having the phenomenon such as pin hole, plating leakage.
4, test result
| Test event | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Comparative example 1 |
| Enter the time of mild reaction | In 60S | In 60S | In 60S | In 60S | In 60S | More than 120S |
| Outward appearance after nickel plating | Flat appearance is fine and close, free of pinholes, plating leakage, | Flat appearance is fine and close, free of pinholes, plating leakage, | Outward appearance is more smooth, free of pinholes, plating leakage, | Flat appearance is fine and close, free of pinholes, plating leakage, | Flat appearance is fine and close, free of pinholes, plating leakage, | Outward appearance is more smooth, occasionally has pin hole, plating leakage phenomenon |
| The nickel-plating liquid life-span | Without precipitation after using 10 times, deposit without nickel | Without precipitation after using 10 times, deposit without nickel | Without precipitation after using 10 times, nickel is had to deposit | Without precipitation after using 10 times, deposit without nickel | Without precipitation after using 10 times, deposit without nickel | Occurring precipitation after using 6 times, nickel deposits |
From above-mentioned test result: salicylide can effectively stop vigorous reaction, improve plated layer compact degree, prevent pin hole and plating leakage phenomenon.Meanwhile, salicylide absorption magnesium alloy dissolved impurity ion in nickel-plating liquid of addition, the nickel-plating liquid life-span can be extended further.
Obviously, above-described embodiment is only for clearly demonstrating example, and is not the restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here without also giving exhaustive to all of embodiment, and the apparent change thus extended out or variation are still among the invention scope of the claims.
Claims (10)
1. a chemically coating nickel by magnesium-alloy liquid, it is characterised in that containing, for example lower component in described nickel-plating liquid: soluble nickel salt, chelating agent, buffer agent, resist, reducing agent, stabilizer and salicylide.
2. chemical nickel-plating liquid according to claim 1, it is characterized in that, described soluble nickel salt 15-25g/L, chelating agent 20-65g/L, buffer agent 10-20g/L, resist 10-30g/L, reducing agent 20-30g/L, stabilizer 0.001-0.003g/L and salicylide 2-7g/L.
3. chemical nickel-plating liquid according to claim 1, it is characterised in that described soluble nickel salt is one or more in nickel sulfate, Nickel dichloride.；
Described chelating agent is one or more in ammonium citrate, ethylenediamine, sodium acetate, lactic acid, malic acid, citric acid, succinic acid, propanoic acid；
Described buffer agent is boric acid；
Described resist is one or more in Fluohydric acid., ammonium acid fluoride, sodium fluoride, potassium fluoride；
Described reducing agent is one or more in hypophosphite, sodium borohydride, borine, hydrazine；
Described stabilizer is one or more in thiourea, potassium thiocyanate, carbamide.
4. chemical nickel-plating liquid according to claim 3, it is characterised in that described chelating agent is one or more in ammonium citrate, ethylenediamine, sodium acetate, lactic acid.
5. chemical nickel-plating liquid according to claim 1, it is characterised in that the pH value of described nickel-plating liquid is 8-9.
6. the preparation method of a chemically coating nickel by magnesium-alloy liquid, it is characterised in that described method is add chelating agent, stabilizer, buffer agent and reducing agent in the aqueous solution of soluble nickel salt；Add resist and salicylide.
7. preparation method according to claim 6, it is characterised in that the pH value of described nickel-plating liquid is at 8-9.
8. preparation method according to claim 6, it is characterized in that, described soluble nickel salt 15-25g/L, chelating agent 20-65g/L, buffer agent 10-20g/L, resist 10-30g/L, reducing agent 20-30g/L, stabilizer 0.001-0.003g/L and salicylide 2-7g/L.
9. preparation method according to claim 6, it is characterised in that described soluble nickel salt is one or more in nickel sulfate, Nickel dichloride.；
Described chelating agent is one or more in ammonium citrate, ethylenediamine, sodium acetate, lactic acid, malic acid, citric acid, succinic acid, propanoic acid；
Described buffer agent is boric acid；
Described resist is one or more in Fluohydric acid., ammonium acid fluoride, sodium fluoride, potassium fluoride；
Described reducing agent is one or more in sodium hypophosphite, sodium borohydride, borine, hydrazine；
Described stabilizer is one or more in thiourea, potassium thiocyanate, carbamide.
10. a method for magnesium alloy surface chemical nickel plating, contacts with nickel-plating liquid including by the magnesium alloy through pre-treatment, must arrive surface and have the magnesium alloy substrates of nickel dam；It is characterized in that, described nickel-plating liquid is the magnesium alloy nickel-plating liquid described in any one of claim 1-5.
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| CN201410852753.5A CN105803431B (en) | 2014-12-31 | 2014-12-31 | A kind of chemically coating nickel by magnesium-alloy liquid, preparation method and its nickel plating process |
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| CN201410852753.5A CN105803431B (en) | 2014-12-31 | 2014-12-31 | A kind of chemically coating nickel by magnesium-alloy liquid, preparation method and its nickel plating process |
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| CN105803431B CN105803431B (en) | 2019-02-26 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109881144A (en) * | 2019-01-31 | 2019-06-14 | 安徽省鑫矿液压机械有限责任公司 | A kind of surface nitrocarburizing heat treatment process of coal mine machinery bearing steel material |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07173640A (en) * | 1993-12-17 | 1995-07-11 | Sumitomo Metal Mining Co Ltd | Electroless nickel plating solution |
| CN101435077A (en) * | 2007-11-12 | 2009-05-20 | 比亚迪股份有限公司 | Magnesium alloy chemical nickel plating solution and electroplating pretreatment method |
| CN102286735A (en) * | 2010-06-19 | 2011-12-21 | 比亚迪股份有限公司 | Chemical nickel plating solution |
| CN102994988A (en) * | 2012-11-26 | 2013-03-27 | 中国科学院金属研究所 | Direct chemical nickel-phosphate plating solution and chemical nickel-phosphate plating coating process for magnesium alloy |
-
2014
- 2014-12-31 CN CN201410852753.5A patent/CN105803431B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07173640A (en) * | 1993-12-17 | 1995-07-11 | Sumitomo Metal Mining Co Ltd | Electroless nickel plating solution |
| CN101435077A (en) * | 2007-11-12 | 2009-05-20 | 比亚迪股份有限公司 | Magnesium alloy chemical nickel plating solution and electroplating pretreatment method |
| CN102286735A (en) * | 2010-06-19 | 2011-12-21 | 比亚迪股份有限公司 | Chemical nickel plating solution |
| CN102994988A (en) * | 2012-11-26 | 2013-03-27 | 中国科学院金属研究所 | Direct chemical nickel-phosphate plating solution and chemical nickel-phosphate plating coating process for magnesium alloy |
Non-Patent Citations (2)
| Title |
|---|
| 《化工百科全书》编辑委员会等: "《化工百科全书》", 28 February 1997, 化学工业出版社 * |
| 胡林林等: "《汽车防锈技术》", 31 March 2004, 化学工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109881144A (en) * | 2019-01-31 | 2019-06-14 | 安徽省鑫矿液压机械有限责任公司 | A kind of surface nitrocarburizing heat treatment process of coal mine machinery bearing steel material |
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