CN117802541A - Method for improving stability of chemical nickel plating bath solution under barrel plating condition and additive - Google Patents
Method for improving stability of chemical nickel plating bath solution under barrel plating condition and additive Download PDFInfo
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- CN117802541A CN117802541A CN202311855659.0A CN202311855659A CN117802541A CN 117802541 A CN117802541 A CN 117802541A CN 202311855659 A CN202311855659 A CN 202311855659A CN 117802541 A CN117802541 A CN 117802541A
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- Prior art keywords
- stabilizer
- bath solution
- plating bath
- nickel plating
- plating
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 238000007747 plating Methods 0.000 title claims abstract description 106
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 55
- 239000000126 substance Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000000654 additive Substances 0.000 title claims abstract description 8
- 230000000996 additive effect Effects 0.000 title claims abstract description 8
- 239000003381 stabilizer Substances 0.000 claims abstract description 46
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 239000000758 substrate Substances 0.000 claims abstract description 7
- TVDSBUOJIPERQY-UHFFFAOYSA-N prop-2-yn-1-ol Chemical class OCC#C TVDSBUOJIPERQY-UHFFFAOYSA-N 0.000 claims description 40
- 230000001105 regulatory effect Effects 0.000 claims description 14
- 230000003750 conditioning effect Effects 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 2
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 238000004381 surface treatment Methods 0.000 abstract description 3
- 150000003839 salts Chemical class 0.000 abstract description 2
- 229910000831 Steel Inorganic materials 0.000 description 12
- 239000010959 steel Substances 0.000 description 12
- 206010027146 Melanoderma Diseases 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 230000004584 weight gain Effects 0.000 description 4
- 235000019786 weight gain Nutrition 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- 229910001096 P alloy Inorganic materials 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 description 1
- IIQJBVZYLIIMND-UHFFFAOYSA-J potassium;antimony(3+);2,3-dihydroxybutanedioate Chemical compound [K+].[Sb+3].[O-]C(=O)C(O)C(O)C([O-])=O.[O-]C(=O)C(O)C(O)C([O-])=O IIQJBVZYLIIMND-UHFFFAOYSA-J 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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- Chemically Coating (AREA)
Abstract
The invention belongs to the technical field of material surface treatment, and particularly relates to a method for improving stability of a chemical nickel plating bath solution under a barrel plating condition and an additive. The method comprises the following steps: preparing a debugging agent for plating solution debugging; determining the usable life cycle of the electroless nickel plating bath solution and the plating speed on the surface of the substrate; preparing a stabilizer according to the measured plating speed; and adding a stabilizer according to the proportion of the service cycle of the chemical nickel plating bath solution to the service life cycle according to the cycle. Compared with the conventional heavy metal salt stabilizer, the stabilizer used in the invention does not contain heavy metal, is environment-friendly, can adapt to barrel plating conditions with harsh requirements, has only very small influence on plating speed under the condition of keeping the stability of the chemical nickel plating bath solution in the whole service life period, thereby greatly improving production efficiency and ensuring the quality of products.
Description
Technical Field
The invention belongs to the technical field of material surface treatment, and particularly relates to a method for improving stability of a chemical nickel plating bath solution under a barrel plating condition and an additive.
Background
The chemical nickel plating method is a common surface treatment method, and the formed nickel-phosphorus alloy plating layer has excellent corrosion resistance, wear resistance and thickness uniformity and has wide application in the industrial field. However, since the process principle is based on self-catalyzed chemical reaction, the situation that the chemical reaction is out of control is easily caused by positive feedback catalysis in the plating process. Particularly in the case of barrel plating, the workpieces are rubbed against each other and bumped when rolling, which can produce particles of micrometer or nanometer size, and these floating particles can act as active sites for new nickel deposition. In the case of a relatively long one-time plating requirement, these particles may cause a significant nickel reduction reaction to occur in the nickel bath as a whole, and a large amount of black deposits may occur in the drum. The drum must be cleaned and the bath must be maintained or replaced considerably. Thus, the working strength of field workers is increased, the efficiency is reduced, and the cost is increased.
The traditional chemical nickel plating stabilizer generally takes heavy metal salt as a main material, has certain pollution to the environment and has obvious influence on the plating speed. Therefore, developing a stabilizer which has little influence on plating speed and is environment-friendly and suitable for chemical nickel plating and a corresponding adding strategy are particularly critical, and the technical scheme of the invention is also provided based on the stabilizer.
Disclosure of Invention
In order to solve the problems in the prior art, the scheme of the invention is to provide a method for improving the stability of an electroless nickel plating bath solution under a barrel plating condition, which comprises the following steps:
(1) Preparing a debugging agent for plating solution debugging;
(2) Determining the usable life cycle of the electroless nickel plating bath solution and the plating speed on the surface of the substrate;
(3) Preparing a stabilizer according to the plating speed measured in the step (2);
(4) Adding a stabilizer according to the proportion of the service cycle of the chemical nickel plating bath solution to the service life cycle according to the cycle;
wherein: the debugging agent consists of ethoxylated propynyl alcohol and propoxylated propynyl alcohol;
the stabilizer consists of ethoxylated propynyl alcohol and propoxylated propynyl alcohol or the stabilizer consists of propargyl alcohol, ethoxylated propynyl alcohol and propoxylated propynyl alcohol.
Preferably, in step (1), the conditioning agent consists of ethoxylated propynyl alcohol and propoxylated propynyl alcohol in a molar ratio of 1:1. The main function of the regulator for regulating the plating solution is to determine the components of the stabilizer through the influence of the regulator on the plating speed of the plating solution.
Preferably, in the step (2), the plating rate of the substrate surface includes V 1 And V 2 ；
The V is 1 In order to add the regulating agent, the plating speed of the chemical nickel plating bath solution under the production process condition is high, and the adding amount of the regulating agent is 200mg/L;
the V is 2 The plating speed of the chemical nickel plating bath solution under the production process condition is not added with the regulating agent. In the measurement, a newly prepared electroless nickel plating bath solution must be used.
In addition, the workpiece was electroless nickel plated on the same substrate (including other underlying metal layers such as electroplated nickel) and the electroless nickel deposition rate was measured. The test method is an industry-wide method such as X-fluorescence.
Preferably, in step (3), when V 1 Compare V 2 When the reduction is less than or equal to 5%, the stabilizer is the same as the regulating agent; when V is 1 Compare V 2 When the reduction is more than 5%, the preparation method of the stabilizer comprises the following steps: every time the plating speed is reduced by 1%, adding 25% of propargyl alcohol in the molar fraction of 5% to the components of the regulator (normally, the regulator cannot cause the reduction of more than 10% of the plating speed at the addition amount of 200 mg/L), thus obtaining the stabilizer.
Preferably, in the step (4), the addition amount of the stabilizer is determined by the proportion of the used period of the electroless nickel plating bath solution to the available life period, specifically: the first adding amount of the stabilizer in the chemical nickel plating bath solution is 200mg/L, and then 50mg/L is added in each period; when the service cycle reaches 1/3-2/3 of the life cycle, 30mg/L of each cycle is added; when the service cycle reaches 2/3 or more of the life cycle, 15mg/L of each cycle is added.
Based on the same technical conception, a further scheme of the invention is to provide an additive for improving the stability of the electroless nickel plating bath solution under the barrel plating condition, wherein the additive comprises a regulating agent and a stabilizing agent; wherein:
the debugging agent consists of ethoxylated propynyl alcohol and propoxylated propynyl alcohol;
the stabilizer consists of ethoxylated propynyl alcohol and propoxylated propynyl alcohol or the stabilizer consists of propargyl alcohol, ethoxylated propynyl alcohol and propoxylated propynyl alcohol.
The beneficial effects of the invention are as follows:
according to the method for improving the stability of the chemical nickel plating bath solution under the barrel plating condition, the additive which does not contain heavy metals or other harmful components to the environment is added into the chemical nickel plating bath solution, so that the stability of the bath solution in the chemical nickel plating barrel plating process is obviously improved, meanwhile, the plating speed is only slightly influenced, the production efficiency is greatly improved, the quality of products is ensured, and the comprehensive effect is excellent.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, based on the examples herein, which are within the scope of the invention as defined by the claims, will be within the scope of the invention as defined by the claims.
In the embodiment, the method for evaluating the long-term stability of the electroless nickel plating bath solution specifically comprises the following steps:
the workpiece is electroless nickel plated on the same substrate, including other underlying metal layers such as electroplated nickel. Including temperature, pH, loading, etc., under the same plating parameters. Observing whether macroscopic black spots, black spots or black blocks appear after the drum is continuously plated for a certain time. When a macroscopic black spot, spot or lump appears in the drum, it means that particles of nickel are produced in the bath during plating and that the concentration of such particles has reached a high value and deposited on the drum. That is, the time when the black spot, the black spot or the black block appears in the drum for the first time is a standard for judging the stability, and the longer the time is, the later the black spot, the black spot or the black block appears, that is, the more stable the bath solution is.
Example 1
In the embodiment of the invention, the chemical plating bath solution used comprises the following components and plating process conditions:
nickel ions: 5.3g/L;
sodium hypophosphite: 30g/L;
malic acid: 9.6g/L;
citric acid: 10.5g/L
Lactic acid: 22g/L;
ammonia water: 12ml/L;
temperature: 85+/-2 ℃;
pH：4.5±0.1
the production service life cycle of the electroless nickel plating bath solution is measured to be 8 cycles.
The method for improving the stability of the electroless nickel plating bath solution under the barrel plating condition comprises the following steps:
(1) Preparing a regulating agent which comprises the components of ethoxylated propynyl alcohol and propoxylated propynyl alcohol in a molar ratio of 1:1;
(2) Taking two parts of chemical nickel plating bath solutions, and adding a regulating reagent into one part of chemical nickel plating bath solution, wherein the adding amount is 200mg/L;
(3) And (3) weighing the two steel sheets with the identical size after degreasing and pickling, and then respectively placing the steel sheets into two electroless nickel plating bath solutions for plating for 1 hour, and taking out and weighing the steel sheets. Calculating to obtain the ratio of the weight gain of the steel sheet in the groove liquid added with the debugging agent to the weight gain of the steel sheet in the groove liquid which is not added with the debugging agent to be 0.93;
(4) Compared with the requirement that the plating speed is reduced by not more than 5%, the plating speed is reduced by 2% in practice. The composition of the stabilizer was thus determined, i.e. 10% propynyl alcohol was added to the conditioning agent;
(5) Two portions of the electroless nickel plating bath solution were used, one of which was added with 200mg/L of the stabilizer. Equal amounts of steel screws were barrel plated in a barrel plating tank using these two baths, with a new batch of plated parts replaced every 2 hours for a total of 8 hours of continuous plating.
(6) The results showed that the cell solution without the stabilizer had a clear turbidity and blackening, and dark deposits were produced in the cell. The tank liquor added with the stabilizer has no the phenomenon and no obvious sediment in the tank.
(7) Thereafter, 50mg/L of the stabilizer was added to the bath per cycle until 30mg/L of the stabilizer was added per cycle from the 3 rd cycle. Then 15mg/L of stabilizer was added per cycle until the 6 th cycle. During which no turbidity and large amounts of black deposits were observed in the bath.
Example 2
In the embodiment of the invention, the chemical plating bath solution used comprises the following components and plating process conditions:
nickel sulfate: 30g/L;
sodium hypophosphite: 15g/L;
ammonium chloride: 50g/L;
sodium citrate: 60g/L
Potassium antimony tartrate: 4mg/L calculated by stibium
Temperature: 85+/-2 ℃;
pH：4.0-4.5
the production service life cycle of the electroless nickel plating bath solution is measured to be 6 cycles.
The method for improving the stability of the electroless nickel plating bath solution under the barrel plating condition comprises the following steps:
(1) Preparing a regulating agent which comprises the components of ethoxylated propynyl alcohol and propoxylated propynyl alcohol in a molar ratio of 1:1;
(2) Taking two parts of chemical nickel plating bath solutions, and adding a regulating reagent into one part of chemical nickel plating bath solution, wherein the adding amount is 200mg/L;
(3) And (3) weighing the two steel sheets with the identical size after degreasing and pickling, and then respectively placing the steel sheets into two electroless nickel plating bath solutions for plating for 1 hour, and taking out and weighing the steel sheets. Calculating to obtain the ratio of the weight gain of the steel sheet in the groove liquid added with the debugging agent to the weight gain of the steel sheet in the groove liquid which is not added with the debugging agent to be 0.96;
(4) Compared with the requirement that the plating speed is reduced by not more than 5%, the plating speed is reduced by only 4% in practice. Determining therefrom that the composition of the stabilizer is the same as the composition of the conditioning agent;
(5) Two portions of the electroless nickel plating bath solution were used, one of which was added with 200mg/L of the stabilizer. Equal amounts of steel screws were barrel plated in a barrel plating tank using these two baths, with a new batch of plated parts replaced every 2 hours for a total of 8 hours of continuous plating.
(6) The results showed that the cell solution without the stabilizer had a clear turbidity and blackening, and dark deposits were produced in the cell. The tank liquor added with the stabilizer has no the phenomenon and no obvious sediment in the tank.
(7) Thereafter, 50mg/L of the stabilizer was added to the bath per cycle until 30mg/L of the stabilizer was added per cycle from the 3 rd cycle. Then 15mg/L of stabilizer was added per cycle until the 5 th cycle. During which no turbidity and large amounts of black deposits were observed in the bath.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any person skilled in the art will readily recognize that variations or substitutions are within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (6)
1. A method for improving stability of electroless nickel plating bath solution under barrel plating condition is characterized by comprising the following steps:
(1) Preparing a debugging agent for plating solution debugging;
(2) Determining the usable life cycle of the electroless nickel plating bath solution and the plating speed on the surface of the substrate;
(3) Preparing a stabilizer according to the plating speed measured in the step (2);
(4) Adding a stabilizer according to the proportion of the service cycle of the chemical nickel plating bath solution to the service life cycle according to the cycle;
wherein: the debugging agent consists of ethoxylated propynyl alcohol and propoxylated propynyl alcohol;
the stabilizer consists of ethoxylated propynyl alcohol and propoxylated propynyl alcohol or the stabilizer consists of propargyl alcohol, ethoxylated propynyl alcohol and propoxylated propynyl alcohol.
2. The method for improving the stability of an electroless nickel plating bath solution under barrel plating conditions according to claim 1, wherein in the step (1), the debugging agent consists of ethoxylated propynyl alcohol and propoxylated propynyl alcohol in a molar ratio of 1:1.
3. The method for improving the stability of an electroless nickel plating bath solution under barrel plating conditions according to claim 1, wherein in the step (2), the plating rate of the substrate surface comprises V 1 And V 2 ；
The V is 1 In order to add the regulating agent, the plating speed of the chemical nickel plating bath solution under the production process condition is high, and the adding amount of the regulating agent is 200mg/L;
the V is 2 The plating speed of the chemical nickel plating bath solution under the production process condition is not added with the regulating agent.
4. The method for improving the stability of an electroless nickel plating bath according to claim 3, wherein in the step (3), when V 1 Compare V 2 When the reduction is less than or equal to 5%, the stabilizer is the same as the regulating agent; when V is 1 Compare V 2 When the reduction is more than 5%, the preparation method of the stabilizer comprises the following steps: every time the plating speed is reduced by 1%, adding propynyl alcohol with the mole fraction of 5% into the components of the debugging agent, and adding propynyl alcohol with the mole fraction of 25% at most to obtain the stabilizer.
5. The method for improving the stability of an electroless nickel plating bath solution under barrel plating conditions according to claim 4, wherein in the step (4), the addition amount of the stabilizer is determined by the proportion of the used cycle of the electroless nickel plating bath solution to the usable life cycle thereof, specifically: the first adding amount of the stabilizer in the chemical nickel plating bath solution is 200mg/L, and then 50mg/L is added in each period; when the service cycle reaches 1/3-2/3 of the life cycle, 30mg/L of each cycle is added; when the service cycle reaches 2/3 or more of the life cycle, 15mg/L of each cycle is added.
6. An additive, comprising a conditioning agent and a stabilizing agent; wherein:
the debugging agent consists of ethoxylated propynyl alcohol and propoxylated propynyl alcohol;
the stabilizer consists of ethoxylated propynyl alcohol and propoxylated propynyl alcohol or the stabilizer consists of propargyl alcohol, ethoxylated propynyl alcohol and propoxylated propynyl alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311855659.0A CN117802541A (en) | 2023-12-29 | 2023-12-29 | Method for improving stability of chemical nickel plating bath solution under barrel plating condition and additive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311855659.0A CN117802541A (en) | 2023-12-29 | 2023-12-29 | Method for improving stability of chemical nickel plating bath solution under barrel plating condition and additive |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117802541A true CN117802541A (en) | 2024-04-02 |
Family
ID=90419712
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311855659.0A Pending CN117802541A (en) | 2023-12-29 | 2023-12-29 | Method for improving stability of chemical nickel plating bath solution under barrel plating condition and additive |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117802541A (en) |
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2023
- 2023-12-29 CN CN202311855659.0A patent/CN117802541A/en active Pending
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