CN1178259A - Solution and coating method for chemically plating amorphous nickel, chromium and phosphur alloys - Google Patents
Solution and coating method for chemically plating amorphous nickel, chromium and phosphur alloys Download PDFInfo
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- CN1178259A CN1178259A CN 97115250 CN97115250A CN1178259A CN 1178259 A CN1178259 A CN 1178259A CN 97115250 CN97115250 CN 97115250 CN 97115250 A CN97115250 A CN 97115250A CN 1178259 A CN1178259 A CN 1178259A
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Abstract
The present invention relates to a plating liquid for chemically plating Ni-Cr-P alloy and method thereof. When the chemical plating takes place in a plating liquid containing nickel salt, chromium chloride, sodium hypophosphite, main complexing agent, auxiliary complexing agent, fluoride, stabilizer, surfactant and buffering agent, Ni-Cr-P alloy can be deposited, which contains Cr (7.0-8.7 Wt.%) and P (10-15 Wt.%). Its advantages include high stability and less corrosion of plating liquid, quick dissolving speed of Cr salt, and high anticorrosion nature of plated layer.
Description
The invention belongs to the surface modification and the surface strengthening technology field of metallic substance, relate to used plating bath of electroless plating plating nickel chromium triangle phosphor alloy coating and electroless plating plating nickel chromium triangle phosphor alloy coating method thereof specifically.
Though the chemical nickel phosphorus plating base binary alloy plating has solidity to corrosion preferably, but still can not satisfy the requirement that the industrial antisepsis erosion is used.After adding the chromic salts class on the nickel phosphorus binary alloy plating bath basis, the nickel chromium triangle phosphorus ternary alloy coating that deposits has higher solidity to corrosion than nickel phosphorus binary alloy.Preparation nickel chromium triangle phosphorus ternary alloy coating is relevant with the pH value of plating bath and the kind of the chromic salts in the adding plating bath etc.In the prior art, in Japanese Patent JP45-16562 (1970), russian patent SU768853 (1981), chromic salts is main a spot of chromium trichloride that adds again with the chromium trifluoride; Some prior art is also used chromous organic coordination compound, and as U.S. Pat 3627545 (1971), US4028116 (1977), above-mentioned plating bath uses under alkaline condition, and service temperature is at the temperature range limit near chemical nickel plating.
The bath system of prior art has following shortcoming: used chromium trifluoride has severe corrosive and dissolution rate is slow, and divalence chromium is reduced by the Hypophosporous Acid, 50 root than trivalent chromium is more difficult; The coating phosphorus content that obtains in the alkali plating solution system is low; The content of chromium is generally lower in the coating, and the solidity to corrosion of coating is relevant with chromium content in the coating, and chromium content is high more, and then solidity to corrosion is good more; The plating temperature height of plating bath, the poor stability of plating bath.Owing to above reason, the chemically plating amorphous nickel, chromium and phosphur ternary alloy coating does not also obtain industrial application.
The purpose of this invention is to provide a kind of new used plating bath of chemically plating amorphous nickel, chromium and phosphur amorphous alloy coating, this plating bath is a kind of acid chemical plating nickel chromium triangle phosphor bath system that contains chromium trichloride, plating bath can use in the stable operating temperature range of chemical plating bath, the good stability of plating bath, no severe corrosive and chromic salts dissolution rate are fast.
Another object of the present invention provides a kind of method of electroless plating plating nickel chromium triangle phosphor alloy coating, this method is used acid chemical plating nickel chromium triangle phosphor bath system of the present invention, the electroless plating operating process can be carried out under lower plating temperature, can guarantee that chromium content can be kept suitable sedimentation velocity again than higher in the coating.
A further object of the present invention provides a kind of method of preparing and adjusting the acid chemical plating liquid of chemically plating amorphous nickel, chromium and phosphur alloy of the present invention, adopts this method all to obtain the high nickel chromium triangle phosphor alloy coating of chrome content in whole plating process, and the coating dense non-porous.
The used acid chemical plating plating bath of chemically plating amorphous nickel, chromium and phosphur amorphous alloy coating of the present invention contains nickel salt, chromium chloride, sodium hypophosphite, main complexing agent, auxiliary complex-former, can also add fluorochemical, stablizer, tensio-active agent and buffer reagent, the consisting of of plating bath:
Components and concentration (mol)
NiSO
4·7H
2O 0.05～0.20
CrCl
3·6H
2O 0.01～0.15
NaH
2PO
2·H
2O 0.20～0.80
Main complexing agent 0.05～0.20
Auxiliary complex-former 0.05～0.20 can also add following composition except that mentioned component:
Fluorochemical 0.12～0.48
Stablizer 1～2ppm
Tensio-active agent 1～10ppm
Sodium-acetate 0.1～0.2
PH value 4.1～5.1
Main salt is single nickel salt in the acidic bath of chemically plating amorphous nickel, chromium and phosphur of the present invention, and its used concentration range is 0.05～0.20 (mol).Concentration crosses that low then sedimentation velocity is too slow, and it is muddy and chrome content is low that excessive concentration then easily produces plating bath.
The chromic salts that uses in the acidic bath of chemically plating amorphous nickel, chromium and phosphur of the present invention is chromium trichloride, in order to remedy the deficiency of not using chromium fluoride, also contains the sylvite or the sodium salt of a spot of fluorochemical in the plating bath, as Sodium Fluoride, Potassium monofluoride.
The acidic bath of chemically plating amorphous nickel, chromium and phosphur of the present invention uses two kinds of organic carboxyl acid class complexing agents simultaneously, makes nickel and chromium two metal ion species all can keep suitable sedimentation velocity effect again by stable existence to reach.Wherein a kind of main complexing agent is citric acid or tartrate and their sodium or sylvite; Another kind of auxiliary complex-former is that carbonatoms is monocarboxylic acid or the di-carboxylic acid of 1-4, is wherein replaced by alkyl, hydroxyl, hydroxyalkyl, amino, carboxyl, alkoxy base 1 or 2, as oxyacetic acid, Padil, lactic acid, propanedioic acid, Succinic Acid etc.
The acidic bath of chemically plating amorphous nickel, chromium and phosphur of the present invention can also add an amount of stablizer, and as using used as stabilizers such as Sodium orthomolybdate, 2-mercapto benzothiazole, fumaric acid, amount ranges is that the stabiliser content in the plating bath reaches 1ppm.But do not use Hg
2+, Pb
2+, Cd
2+, Te
4+Deng the toxic heavy metal salt, do not use to contain Se, Te organism yet.These stablizers that the present invention uses are nontoxic, and not obvious reduction sedimentation velocity does not have tangible detrimentally affect to corrosion resistance of coating.
Can add an amount of tensio-active agent in the acidic bath plating bath of chemically plating amorphous nickel, chromium and phosphur of the present invention, it can be sodium lauryl sulphate, sodium laurylsulfonate, OP class tensio-active agent etc., other surface chemistry agent that does not influence plating bath chemical stability, sedimentation velocity, quality of coating all can be used, as aniorfic surfactant, cationic surfactant and amphoterics.Amount ranges is that the surfactant content in the plating bath reaches 1～10ppm.These tensio-active agents can reduce the surface tension of plating bath, help plating bath and fully contact with the metallic surface, help separating out of byproduct of reaction hydrogen, reduce the coating pin hole, improve quality of coating, also can reduce the possibility of plating piece hydrogen embrittlement.
Can add an amount of buffer reagent in the acidic bath of chemically plating amorphous nickel, chromium and phosphur of the present invention, be 0.1～0.2 (mol) as the sodium-acetate amount ranges, reaches in pH value 4.1～5.1 scopes of keeping bath system.
The method of electroless plating plating nickel chromium triangle phosphor alloy coating of the present invention is: adopting above-mentioned plating bath of the present invention, is plating under 80～95 ℃ the temperature in temperature.Temperature is low excessively, and sedimentation velocity is very slow; Temperature is too high, and bath stability is poor.The pH value of plating bath maintains the pH value of acetate buffer system in 4.1～5.1 scopes.
The acidic bath compound method of chemically plating amorphous nickel, chromium and phosphur of the present invention is that first chromium chloride with weighing in advance dissolves with complexing agent, and other composition that adds plating bath of the present invention then is mixed with complete plating bath.
Plating bath of the present invention can be adjusted pH in 4.1～5.1 scopes with 10% (weight) NaOH in the plating process, nickel salt and sodium hypophosphite consumption are added by 1: 2.4 mol ratio.
The acidic bath of chemically plating amorphous nickel, chromium and phosphur of the present invention has bath stability height, long service life; No severe corrosive and the fast advantage of chromic salts dissolution rate.Adopt acidic bath of the present invention to carry out, and in the plating process, can adjust the pH value and the composition of plating bath easily in lower plating temperature scope.
Use the method for electroless plating plating nickel chromium triangle phosphor alloy coating of the present invention, above-mentioned plating bath form and the operational condition scope in carry out, the coating of the Huo Deing metalluster that is silvery white in color then, coating hardness is about 500Hv under plated state.The nickel chromium triangle phosphor alloy coating that obtains is measured by analysis and is contained chromium 7.0～8.7wt%, phosphorus 10～15wt%.
Gained nickel chromium triangle phosphor alloy coating of the present invention adopts the concentrated nitric acid accelerated corrosion test of standard to test, and etching time was greater than 900 seconds.Test-results shows resulting chemically plating amorphous nickel, chromium and phosphur alloy layer solidity to corrosion height, and solidity to corrosion is higher than the nickel phosphorus base binary alloy plating of close phosphorus content in acid, alkali, brine corrosion medium, and the performance of coating meets and exceeds national standard.
Therefore the acidic bath of chemically plating amorphous nickel, chromium and phosphur of the present invention and solution and coating method thereof, plating bath inflation method have overcome the defective of prior art, make the chemically plating amorphous nickel, chromium and phosphur amorphous alloy coating realize industrial applications.
The invention will be further described below by embodiment.Should be understood that these embodiment just to the present invention is illustrated, do not mean to constitute to limit the invention.Embodiment 1
In the present embodiment the straight carbon steel base material is carried out nickel chromium triangle phosphorus alloy electroless plating.The straight carbon steel base material carries out plating after grinding, alkali cleaning oil removing, pickling, activation.Base materials such as copper need to carry out plating behind the first flash nickel.Main complexing agent citric acid in the used plating bath, auxiliary complex-former oxyacetic acid, stablizer Sodium orthomolybdate, tensio-active agent sodium lauryl sulphate.This is suitable executes that plating bath that example adopted is formed and operational condition is as follows:
Components and concentration (mol)
NiSO
4·7H
2O 0.05
CrCl
3·6H
2O 0.03
NaH
2PO
2·H
2O 0.30
Citric acid 0.10
Oxyacetic acid 0.20
NaF 0.12
Na
2MoO
3 1ppm
Sodium lauryl sulphate 10ppm
Sodium-acetate 0.2
pH 4.6
90 ℃ of temperature
Coating deposition rate is 3 * 10
-3G cm
-2h
-1About.
The nickel chromium triangle phosphor alloy coating that the obtains metalluster that is silvery white in color, coating hardness is about 550Hv.
The nickel chromium triangle phosphor alloy coating that obtains is measured by analysis and is contained chromium 7.0～8.0wt%, phosphorus 14～15wt%.
The concentrated nitric acid accelerated corrosion test test gained nickel chromium triangle phosphor alloy coating of employing standard, etching time is 950 seconds.Test-results shows resulting chemically plating amorphous nickel, chromium and phosphur alloy layer solidity to corrosion height.Solidity to corrosion is higher than the nickel phosphorus base binary alloy plating of close phosphorus content in acid, alkali, brine corrosion medium, and the performance of coating meets and exceeds national standard.Embodiment 2
In the present embodiment copper coin is carried out nickel chromium triangle phosphorus alloy electroless plating.Copper coin carries out plating behind grinding, alkali cleaning oil removing, acid-wash activation.Copper material needs to carry out plating behind the first flash nickel.Main complexing agent citric acid in the used plating bath, auxiliary complex-former lactic acid, stablizer fumaric acid, tensio-active agent OP-10.Plating bath composition and operational condition that present embodiment adopted are as follows:
Components and concentration (mol)
NiSO
4·7H
2O 0.15
CrCl
3·6H
2O 0.10
NaH
2PO
2·H
2O 0.50
Citric acid 0.15
Lactic acid 0.20
NaF 0.45
Fumaric acid 1ppm
OP-10 1ppm
Sodium-acetate 0.2
pH 4.8
85 ℃ of temperature
Coating deposition rate is 3.5 * 10
-3G cm
-2h
-1About.
The nickel chromium triangle phosphor alloy coating that the obtains metalluster that is silvery white in color, coating hardness is about 500Hv.
The nickel chromium triangle phosphor alloy coating that obtains is measured by analysis and is contained chromium 7.5～8.0wt%, phosphorus 10～13wt%.
The concentrated nitric acid accelerated corrosion test test gained nickel chromium triangle phosphor alloy coating of employing standard, etching time is 930 seconds.Embodiment 3
In the present embodiment cast iron base material is carried out nickel chromium triangle phosphorus alloy electroless plating.Cast iron base material is carried out plating behind grinding, alkali cleaning oil removing, pickling, activation, flash nickel.Main complexing agent tartrate in the used plating bath, auxiliary complex-former Padil, stablizer 2-mercapto benzothiazole, tensio-active agent Sodium dodecylbenzene sulfonate.Plating bath composition and operational condition that present embodiment adopted are as follows:
Components and concentration (mol)
NiSO
4·7H
2O 0.10
CrCl
3·6H
2O 0.15
NaH
2PO
2·H
2O 0.60
Tartrate 0.20
Padil 0.10
Potassium monofluoride 0.35
2-mercapto benzothiazole 2ppm
Sodium dodecylbenzene sulfonate 5ppm
Sodium-acetate 0.1
pH 5.1
80 ℃ of temperature
Coating deposition rate is 3.5 * 10
-3G cm
-2h
-1About.
The nickel chromium triangle phosphor alloy coating that the obtains metalluster that is silvery white in color, coating hardness is about 500Hv.
The nickel chromium triangle phosphor alloy coating that obtains is measured by analysis and is contained chromium 7.8～8.7wt%, phosphorus 13～14wt%.
The concentrated nitric acid accelerated corrosion test test gained nickel chromium triangle phosphor alloy coating of employing standard, etching time is 920 seconds.
Obviously, those skilled in the art, can make improvements, change and replace explanation of the present invention and listed examples according to above-mentioned the present invention, but do not exceed essence of the present invention and the application's claims institute restricted portion.
Claims (12)
1, a kind of acidic bath of chemically plating amorphous nickel, chromium and phosphur alloy contains nickel salt, chromium chloride, sodium hypophosphite, main complexing agent, auxiliary complex-former, it is characterized in that consisting of of this plating bath:
Components and concentration (mol)
NiSO
4·7H
2O 0.05～0.20
CrCl
3·6H
2O 0.01～0.15
NaH
2PO
2·H
2O 0.20～0.80
Main complexing agent 0.05～0.20
Auxiliary complex-former 0.05～0.20,
PH value 4.1～5.1 wherein, main complexing agent is citric acid or tartrate and their sodium or sylvite; Auxiliary complex-former is that carbonatoms is monocarboxylic acid or the di-carboxylic acid of 1-4, is wherein replaced by alkyl, hydroxyl, hydroxyalkyl, amino, carboxyl, alkoxy base 1 or 2.
2, a kind of acidic bath of chemically plating amorphous nickel, chromium and phosphur alloy contains nickel salt, chromium chloride, sodium hypophosphite, main complexing agent, auxiliary complex-former, fluorochemical, stablizer, tensio-active agent and buffer reagent, its this be characterised in that consisting of of this plating bath:
Components and concentration (mol)
NiSO
4·7H
2O 0.05～0.20
CrCl
3·6H
2O 0.01～0.15
NaH
2PO
2·H
2O 0.20～0.80
Main complexing agent 0.05～0.20
Auxiliary complex-former 0.05～0.20
Fluorochemical 0.12～0.48
Stablizer 1～2ppm
Tensio-active agent 1～10ppm
Sodium-acetate 0.1～0.2
PH value 4.1～5.1
3. according to claim (1) or (2) described plating bath, it is characterized in that also containing the sylvite or the sodium salt of 0.12～0.48 (mol) fluorochemical.
4,, it is characterized in that also containing the stablizer that is selected from Sodium orthomolybdate, 2-mercapto benzothiazole, fumaric acid of 1～2ppm according to claim (1) or (2) described plating bath.
5,, it is characterized in that also containing the tensio-active agent that is selected from sodium lauryl sulphate, sodium laurylsulfonate, OP class of 1～10ppm according to claim (1) or (2) described plating bath.
6,, it is characterized in that also containing the sodium-acetate of 0.1～0.2 (mol) according to claim (1) or (2) described plating bath.
7,, it is characterized in that wherein auxiliary complex-former is oxyacetic acid, Padil, lactic acid, propanedioic acid, Succinic Acid according to claim (1) or (2) described plating bath.
8, according to the described plating bath of claim (2), its this be characterised in that consisting of of this plating bath:
Components and concentration (mol)
NiSO
4·7H
2O 0.05
CrCl
3·6H
2O 0.03
NaH
2PO
2·H
2O 0.30
Citric acid 0.10
Oxyacetic acid 0.20
NaF 0.12
Na
2MoO
3 1ppm
Sodium lauryl sulphate 10ppm
Sodium-acetate 0.2
pH 4.6
9, according to the described plating bath of claim (2), its this be characterised in that consisting of of this plating bath:
Components and concentration (mol)
NiSO
4·7H
2O 0.15
CrCl
3·6H
2O 0.10
NaH
2PO
2·H
2O 0.50
Citric acid 0.15
Lactic acid 0.20
NaF 0.45
Fumaric acid 1ppm
OP-10 1ppm
Sodium-acetate 0.2
pH 4.8
10, according to the described plating bath of claim (2), its this be characterised in that consisting of of this plating bath:
Components and concentration (mol)
NiSO
4·7H
2O 0.10
CrCl
3·6H
2O 0.15
NaH
2PO
2·H
2O 0.60
Tartrate 0.20
Padil 0.10
Potassium monofluoride 0.35
2-mercapto benzothiazole 2ppm
Sodium dodecylbenzene sulfonate 5ppm
Sodium-acetate 0.1
pH 5.1
11, a kind of method of electroless plating plating nickel chromium triangle phosphor alloy coating is characterized in that using any plating bath of aforesaid right requirement 1～11, is plating under 80～95 ℃ the temperature in temperature, and the pH value of plating bath maintains in 4.1～5.1 scopes.
12, the acidic bath method of any chemically plating amorphous nickel, chromium and phosphur of a kind of preparation and adjustment aforesaid right requirement 1～11 is characterized in that first chromium chloride with weighing in advance dissolves with complexing agent, and other composition that adds plating bath then is mixed with complete plating bath; Adjust PH in 4.1～5.1 scopes with 10% (weight) NaOH in the plating process, nickel salt and sodium hypophosphite consumption are added by 1: 2.4 mol ratio.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97115250 CN1050865C (en) | 1997-08-26 | 1997-08-26 | Solution and coating method for chemically plating amorphous nickel, chromium and phosphur alloys |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97115250 CN1050865C (en) | 1997-08-26 | 1997-08-26 | Solution and coating method for chemically plating amorphous nickel, chromium and phosphur alloys |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1178259A true CN1178259A (en) | 1998-04-08 |
| CN1050865C CN1050865C (en) | 2000-03-29 |
Family
ID=5173240
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 97115250 Expired - Fee Related CN1050865C (en) | 1997-08-26 | 1997-08-26 | Solution and coating method for chemically plating amorphous nickel, chromium and phosphur alloys |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1050865C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1079449C (en) * | 1999-07-12 | 2002-02-20 | 西北有色金属研究院 | Self-catalytic nickel alloy plating layer and plating process thereof |
| CN103866307A (en) * | 2014-03-13 | 2014-06-18 | 沈阳市环东电镀厂 | Environment-friendly single-dose and double-color galvanized trivalent chromium passivation agent and preparation and application methods thereof |
| CN107475698A (en) * | 2017-06-23 | 2017-12-15 | 安庆师范大学 | A kind of extra thin copper foil peel ply Ni Cr B P preparation method |
| CN108998779A (en) * | 2018-10-13 | 2018-12-14 | 四川鑫元瑞科技有限公司 | A kind of chemical plating fluid and environment-friendly type alloy surface self-catalysis processing method |
| CN109183011A (en) * | 2018-11-21 | 2019-01-11 | 丽水学院 | For imporous chemical nickel-plating additive concentrate |
| CN111005011A (en) * | 2014-10-27 | 2020-04-14 | 表面技术公司 | Plating bath solution |
| CN112458506A (en) * | 2020-12-08 | 2021-03-09 | 赵伟 | Co-Fe binary alloy electroplating solution |
| CN114438481A (en) * | 2022-01-24 | 2022-05-06 | 四川轻化工大学 | Amorphous nickel-phosphorus alloy coating and preparation method thereof |
-
1997
- 1997-08-26 CN CN 97115250 patent/CN1050865C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1079449C (en) * | 1999-07-12 | 2002-02-20 | 西北有色金属研究院 | Self-catalytic nickel alloy plating layer and plating process thereof |
| CN103866307A (en) * | 2014-03-13 | 2014-06-18 | 沈阳市环东电镀厂 | Environment-friendly single-dose and double-color galvanized trivalent chromium passivation agent and preparation and application methods thereof |
| CN111005011A (en) * | 2014-10-27 | 2020-04-14 | 表面技术公司 | Plating bath solution |
| CN111005011B (en) * | 2014-10-27 | 2022-04-01 | 表面技术公司 | Plating bath solution |
| CN107475698A (en) * | 2017-06-23 | 2017-12-15 | 安庆师范大学 | A kind of extra thin copper foil peel ply Ni Cr B P preparation method |
| CN108998779A (en) * | 2018-10-13 | 2018-12-14 | 四川鑫元瑞科技有限公司 | A kind of chemical plating fluid and environment-friendly type alloy surface self-catalysis processing method |
| CN108998779B (en) * | 2018-10-13 | 2020-03-10 | 绵阳高新区天力机械有限责任公司 | Chemical plating solution and environment-friendly alloy surface autocatalytic treatment method |
| CN109183011A (en) * | 2018-11-21 | 2019-01-11 | 丽水学院 | For imporous chemical nickel-plating additive concentrate |
| CN112458506A (en) * | 2020-12-08 | 2021-03-09 | 赵伟 | Co-Fe binary alloy electroplating solution |
| CN112458506B (en) * | 2020-12-08 | 2023-10-31 | 佳盛电子科技(惠州)有限公司 | Electroplating solution for metal substrate |
| CN114438481A (en) * | 2022-01-24 | 2022-05-06 | 四川轻化工大学 | Amorphous nickel-phosphorus alloy coating and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1050865C (en) | 2000-03-29 |
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