CN107955943A - Phosphorus alkaline electroless plating nickel-phosphor bath and its chemical plating process in medium temperature - Google Patents
Phosphorus alkaline electroless plating nickel-phosphor bath and its chemical plating process in medium temperature Download PDFInfo
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- CN107955943A CN107955943A CN201711195741.XA CN201711195741A CN107955943A CN 107955943 A CN107955943 A CN 107955943A CN 201711195741 A CN201711195741 A CN 201711195741A CN 107955943 A CN107955943 A CN 107955943A
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- Prior art keywords
- plating
- phosphorus
- nickel
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- medium temperature
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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
Abstract
The present invention relates to phosphorus alkaline electroless plating nickel-phosphor bath and its chemical plating process in a kind of medium temperature, which includes aqueous solvent and following component：25 35g/L of nickel sulfate, 30 40g/L of sodium hypophosphite, 15 25g/L of sodium citrate, 10 20ml/L of ammonium hydroxide, 0 10ml/L of triethanolamine, 2 4g/L of accelerator, 4 5g/L of buffer；The pH value of plating solution is 8.4 9.3.Phosphorus alkaline electroless plating nickel-phosphor bath uses compound complex agent in above-mentioned medium temperature, improves the stability of alkali plating solution, while adds accelerator propionic acid, further increases the plating speed and phosphorus content of chemical plating nickel-phosphorus alloy.Gained coating is bright fine and close, there is good a corrosion resistance and wearability, and coating phosphorus content scope is 6% 8%；Ensure that reduces the temperature of chemical plating nickel-phosphorus alloy under faster plating speed, greatly reduces the cost of production, improves productivity effect.
Description
Technical field
The present invention relates to electroless plating technology field, more particularly to phosphorus alkaline electroless plating nickel-phosphor bath in a kind of medium temperature and its
Electroplating technology.
Background technology
Chemical plating nickel-phosphorus alloy with outstanding properties such as excellent corrosion resistance, wearability and high rigidity due to extensively should
Used in industrial circle, the nickel-phosphorus alloy (phosphorus content 6%-9%) of middle phosphorus content industrially most widely used.
For the operating temperature of current chemical plating nickel-phosphorus alloy technique generally more than 85 DEG C, bath stability is poor, to coating bath and
Equipment it is more demanding, and be easy to cause the deformation of plating piece.Chemical plating nickel-phosphorus alloy technique can be divided into acidity for electrolyte
With alkalescence two kinds.Acid chemical plating nickel-phosphorus alloy plate under mesophilic condition speed it is very low, therefore on medium temperature chemical nickel phosphorus plating close
Gold process uses alkali plating solution more.
The plating speed of alkaline electroless plating nickel-phosphorus alloy technique is very fast, is conducive to carry out chemical nickel plating nickel-phosphorus alloy under medium temperature,
But it is poor that alkaline electroless plating nickel-phosphorus alloy technique still suffers from bath stability, the shortcomings such as coating phosphorus content is low.Therefore, existing alkali
Property chemical nickel plating phosphor bath still has much room for improvement.
The content of the invention
Based on this, the object of the present invention is to provide phosphorus alkaline electroless plating nickel-phosphor bath in a kind of medium temperature.
Specific technical solution is as follows：
Phosphorus alkaline electroless plating nickel-phosphor bath in a kind of medium temperature, including aqueous solvent and following component：
The pH value of phosphorus alkaline electroless plating nickel-phosphor bath is 8.4-9.3 in medium temperature.
In wherein some embodiments, the accelerator is selected from propionic acid.
In wherein some embodiments, the buffer is selected from sodium carbonate.
It is a further object of the present invention to provide a kind of chemical nickel phosphorus plating technique.
Specific technical solution is as follows：
A kind of chemical nickel phosphorus plating technique, includes the following steps：
Pre-treatment：Workpiece to be plated is subjected to pre-treatment；
Chemical plating：Workpiece to be plated after pre-treatment is immersed into phosphorus alkalization in claim 1-3 any one of them medium temperatures
Nickel plating phosphor bath is learned, controlled at 60-65 DEG C, plating time 50-70min, one layer is formed in the workpiece surface to be plated
Nickel-phosphorus alloy coating, you can.
In wherein some embodiments, further included in the electroless plating step and draw plating step, the plating step of drawing is by salt
Acid-treated stainless steel wire contacts the workpiece to be plated, duration 8-12s.
In wherein some embodiments, the pre-treatment step includes washing, acid after alkaline degreasing, acid neutralization, neutralization
Washed after property microetch and microetch.
In wherein some embodiments, the plating surface of the workpiece to be plated is copper face.
In wherein some embodiments, phosphorus content is 6-8wt% in the nickel-phosphorus alloy coating.
Phosphorus alkaline electroless plating nickel-phosphor bath uses compound complex agent (sodium citrate, ammonium hydroxide, triethanolamine three in above-mentioned medium temperature
The cooperation of kind complexing agent), the stability of alkali plating solution is improved, while accelerator propionic acid is added, further increase chemical plating
The plating speed and phosphorus content of nickel-phosphorus alloy.
Above-mentioned chemical nickel phosphorus plating technique uses phosphorus alkaline electroless plating nickel-phosphor bath in above-mentioned medium temperature and coordinates electrochemistry accidental
Method realizes the chemical nickel phosphorus plating technique on copper surface, and technique plating speed is very fast, and gained coating is bright fine and close, there is good corrosion resistance
And wearability, coating phosphorus content scope are 6%-8%；And ensure that reduces chemical plating nickel-phosphorus alloy under faster plating speed
Temperature, greatly reduce the cost of production, improve productivity effect.
Embodiment
For the ease of understanding the present invention, the present invention will be described more fully below.But the present invention can be with perhaps
More different form is realized, however it is not limited to embodiment described herein.On the contrary, the purpose for providing these embodiments is to make
Understanding more thorough and comprehensive to the disclosure.
Unless otherwise defined, all of technologies and scientific terms used here by the article is with belonging to technical field of the invention
The normally understood implication of technical staff is identical.Term used in the description of the invention herein is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein "and/or" includes one or more phases
The arbitrary and all combination of the Listed Items of pass.
Embodiment 1
The present embodiment a kind of composition and content of chemical nickel plating phosphor bath：Nickel sulfate 30g/L, sodium hypophosphite 35g/L, lemon
Lemon acid sodium 20g/L, ammonium hydroxide 15mL, triethanolamine 5mL/L, sodium carbonate 4g/L, with the H of 1mol/L2SO4It is 9.3 to adjust pH.
It is as follows using carry out chemical nickel phosphorus plating operating procedure of the above-mentioned plating solution on copper-based bottom：
It will be put into 60 DEG C of thermostat water bath by above-mentioned plating solution and be heated to constant temperature.
The Copper base material (workpiece to be plated) of 2 × 3cm is completely immersed in plating solution, the stainless steel wire crossed with HCl treatment contacts copper
Substrate, draws plating 10s, takes out after plating 60min and rinsed with water in the plating solution, dried up with cold wind.
The surface of above-mentioned Copper base material has obtained the Ni-P alloy layers of shiny appearance.Weight method is used to measure plating speed as 8.32
μm/h。
By the content of P in phosphorus molybdenum vanadium Huang spectrophotometry coating, the percentage composition of P element is 6.30%, is belonged to
The coating of middle phosphorus content.
Use PdCl2Experimental method measures the stability of plating solution, plating solution blackening after 1h.Time, longer stability was better, one hour
Belong to the index of high stability plating solution.
Plating piece is 1:30s not blackening is soaked in 1 nitric acid, it is good corrosion-resistant to show that coating provided by the present invention has
Property.
Embodiment 2
The present embodiment a kind of composition and content of chemical nickel plating phosphor bath：Nickel sulfate 30g/L, sodium hypophosphite 35g/L, lemon
Lemon acid sodium 15g/L, ammonium hydroxide 10mL, sodium carbonate 4g/L, without triethanolamine.It has been investigated that the amount of ammonium hydroxide can influence chemical nickel plating
Deposition velocity and coating in phosphorus content, therefore, in implementation process with 5% NaOH adjust pH be 9.3.
The concrete operations technique of chemical nickel phosphorus plating is carried out with embodiment 1 in Copper base material using above-mentioned plating solution.
The chemical nickeling phosphorus alloy film shiny appearance obtained by above-mentioned technique, chemical nickel phosphorus plating is measured using weight method
The plating speed of alloy is 5.95 μm/h.
By the content of P in phosphorus molybdenum vanadium Huang spectrophotometry coating, the percentage composition of P element is 8.01%, is belonged to
The coating of middle phosphorus content.
Plating piece is 1:30s not blackening is soaked in 1 nitric acid, it is good corrosion-resistant to show that coating provided by the present invention has
Property.
Embodiment 3
The present embodiment a kind of composition and content of chemical nickel plating phosphor bath：Nickel sulfate 30g/L, sodium hypophosphite 30g/L, lemon
Lemon acid sodium 15g/L, ammonium hydroxide 20mL, triethanolamine 5mL/L, sodium carbonate 5g/L, with the H of 1mol/L2SO4It is 9.3 to adjust pH.
The concrete operations technique of chemical nickel phosphorus plating is carried out with embodiment 1 to Copper base material using above-mentioned plating solution.
The chemical nickeling phosphorus alloy film shiny appearance obtained by above-mentioned technique, chemical nickel phosphorus plating is measured using weight method
The plating speed of alloy is 7.22 μm/h.
By the content of P in phosphorus molybdenum vanadium Huang spectrophotometry coating, the percentage composition of P element is 6.39%, is belonged to
The coating of middle phosphorus content.
Plating piece is 1:30s not blackening is soaked in 1 nitric acid, it is good corrosion-resistant to show that coating provided by the present invention has
Property.
Embodiment 4
The present embodiment a kind of composition and content of chemical nickel plating phosphor bath：Nickel sulfate 30g/L, sodium hypophosphite 35g/L, lemon
Lemon acid sodium 20g/L, ammonium hydroxide 15mL, triethanolamine 5mL/L, propionic acid 1.5g/L, sodium carbonate 4g/L, with the H of 1mol/L2SO4Adjust pH
For 9.3.
The concrete operations technique of chemical nickel phosphorus plating is carried out with embodiment 1 to Copper base material using above-mentioned plating solution.
The chemical nickeling phosphorus alloy film shiny appearance obtained by above-mentioned technique, chemical nickel phosphorus plating is measured using weight method
The plating speed of alloy is 8.45 μm/h.
By the content of P in phosphorus molybdenum vanadium Huang spectrophotometry coating, the percentage composition of P element is 6.34%, is belonged to
The coating of middle phosphorus content.
Plating piece is 1:30s not blackening is soaked in 1 nitric acid, it is good corrosion-resistant to show that coating provided by the present invention has
Property.
Embodiment 5
The present embodiment a kind of composition and content of chemical nickel plating phosphor bath：Nickel sulfate 30g/L, sodium hypophosphite 35g/L, lemon
Lemon acid sodium 20g/L, ammonium hydroxide 15mL, triethanolamine 5mL/L, propionic acid 3g/L, sodium carbonate 4g/L, with the H of 1mol/L2SO4Adjusting pH is
9.3。
The concrete operations technique of chemical nickel phosphorus plating is carried out with embodiment 1 to Copper base material using above-mentioned plating solution.
The chemical nickeling phosphorus alloy film shiny appearance obtained by above-mentioned technique, chemical nickel phosphorus plating is measured using weight method
The plating speed of alloy is 8.72 μm/h.
By the content of P in phosphorus molybdenum vanadium Huang spectrophotometry coating, the percentage composition of P element is 6.45%, is belonged to
The coating of middle phosphorus content.
Plating piece is 1:30s not blackening is soaked in 1 nitric acid, it is good corrosion-resistant to show that coating provided by the present invention has
Property.
The bath stability of phosphorus alkaline electroless plating nickel-phosphor bath in a kind of medium temperature of the present invention is understood from above-mentioned 5 embodiments
Good, obtained Deposit appearance is bright, has not only reduced the temperature of chemical plating nickel-phosphorus alloy technique, but also realizes faster plating speed, together
When also ensure that P content in chemical nickeling phosphorus alloy film, corrosion resistance of coating is excellent, has reached current high-temperature acidic chemical nickel plating
The standard of phosphor alloy coating.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality
Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, the scope that this specification is recorded all is considered to be.
Embodiment described above only expresses the several embodiments of the present invention, its description is more specific and detailed, but simultaneously
Cannot therefore it be construed as limiting the scope of the patent.It should be pointed out that come for those of ordinary skill in the art
Say, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (8)
1. phosphorus alkaline electroless plating nickel-phosphor bath in a kind of medium temperature, it is characterised in that including aqueous solvent and following component：
The pH value of phosphorus alkaline electroless plating nickel-phosphor bath is 8.4-9.3 in medium temperature.
2. phosphorus alkaline electroless plating nickel-phosphor bath in medium temperature according to claim 1, it is characterised in that the accelerator is selected from
Propionic acid.
3. phosphorus alkaline electroless plating nickel-phosphor bath in medium temperature according to claim 1, it is characterised in that the buffer is selected from
Sodium carbonate.
4. a kind of chemical nickel phosphorus plating technique, it is characterised in that include the following steps：
Pre-treatment：Workpiece to be plated is subjected to pre-treatment；
Chemical plating：Workpiece to be plated after pre-treatment is immersed into phosphorus alkaline electroless plating in claim 1-3 any one of them medium temperatures
Nickel-phosphor bath, controlled at 60-65 DEG C, plating time 50-70min, one layer of nickel phosphorus is formed in the workpiece surface to be plated
Alloy layer, you can.
5. chemical nickel phosphorus plating technique according to claim 4, it is characterised in that further included in the electroless plating step and draw plating
Step, the plating step of drawing is that the stainless steel wire for crossing HCl treatment contacts the workpiece to be plated, duration 8-12s.
6. chemical nickel phosphorus plating technique according to claim 4, it is characterised in that the pre-treatment step is removed including alkalescence
Oil, acid neutralization, wash after neutralizing, washed after acid etching and microetch.
7. according to claim 4-6 any one of them chemical nickel phosphorus plating techniques, it is characterised in that the plating of the workpiece to be plated
Surface is copper face.
8. according to claim 4-6 any one of them chemical nickel phosphorus plating techniques, it is characterised in that in the nickel-phosphorus alloy coating
Phosphorus content is 6-8wt%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711195741.XA CN107955943A (en) | 2017-11-24 | 2017-11-24 | Phosphorus alkaline electroless plating nickel-phosphor bath and its chemical plating process in medium temperature |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711195741.XA CN107955943A (en) | 2017-11-24 | 2017-11-24 | Phosphorus alkaline electroless plating nickel-phosphor bath and its chemical plating process in medium temperature |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113774369A (en) * | 2021-08-20 | 2021-12-10 | 张家口原轼新型材料有限公司 | Plating solution and plating process for plating nickel-cobalt-phosphorus alloy on surface of emery and obtained emery and golden steel wire |
Citations (2)
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|---|---|---|---|---|
| WO2005038084A2 (en) * | 2003-10-17 | 2005-04-28 | Applied Materials, Inc. | Selective self-initiating electroless capping of copper with cobalt-containing alloys |
| CN101705481A (en) * | 2009-10-29 | 2010-05-12 | 高远新 | Chemical nickel-phosphorus alloy plating process of heat radiator |
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2017
- 2017-11-24 CN CN201711195741.XA patent/CN107955943A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005038084A2 (en) * | 2003-10-17 | 2005-04-28 | Applied Materials, Inc. | Selective self-initiating electroless capping of copper with cobalt-containing alloys |
| CN101705481A (en) * | 2009-10-29 | 2010-05-12 | 高远新 | Chemical nickel-phosphorus alloy plating process of heat radiator |
Non-Patent Citations (2)
| Title |
|---|
| 模具实用技术丛书编委会: "《模具精饰加工及表面强化技术》", 31 October 1999, 机械工业出版社 * |
| 钱苗根等: "《材料表面技术及其应用手册》", 30 November 1998, 机械工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113774369A (en) * | 2021-08-20 | 2021-12-10 | 张家口原轼新型材料有限公司 | Plating solution and plating process for plating nickel-cobalt-phosphorus alloy on surface of emery and obtained emery and golden steel wire |
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Application publication date: 20180424 |