CN111041531A - Capacitor nickel electroplating solution, electroplating method and application - Google Patents

Capacitor nickel electroplating solution, electroplating method and application Download PDF

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Publication number
CN111041531A
CN111041531A CN201911190868.1A CN201911190868A CN111041531A CN 111041531 A CN111041531 A CN 111041531A CN 201911190868 A CN201911190868 A CN 201911190868A CN 111041531 A CN111041531 A CN 111041531A
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China
Prior art keywords
nickel
electroplating
sodium
capacitor
solution
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CN201911190868.1A
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Chinese (zh)
Inventor
梁俊展
娄红涛
黄澳斌
梁炳联
万广宇
唐国辉
张旭玲
冯辉
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GUANGDONG LINGGUANG NEW MATERIAL CO LTD
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GUANGDONG LINGGUANG NEW MATERIAL CO LTD
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Priority to CN201911190868.1A priority Critical patent/CN111041531A/en
Publication of CN111041531A publication Critical patent/CN111041531A/en
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/12Electroplating: Baths therefor from solutions of nickel or cobalt
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34Pretreatment of metallic surfaces to be electroplated

Abstract

The invention relates to a capacitor nickel electroplating solution, an electroplating method and application, and belongs to the technical field of electronic component processing. The nickel electroplating solution comprises a pre-plating treatment solution and a main electroplating solution; the pre-plating treatment solution comprises: 1-10g/L of organic acid and 5-20g/L of complexing agent; the main electroplating solution comprises: 10-20g/L of nickel-containing metal salt, 300-500g/L of conductive salt, 40-50g/L of buffering agent and 0.01-0.1g/L of stress relieving agent. The 0201 type chip capacitor is subjected to nickel electroplating by adopting the electroplating solution and the electroplating method, the electroplating efficiency of the 0201 type chip capacitor can be effectively improved, the product has good welding resistance, the nickel electroplating solution has no corrosion to the product, the plating layer is uniform and compact, does not peel off or fall off, is corrosion-resistant, and has the advantages of simple process, energy conservation and environmental protection, the cost is greatly reduced, and the product performance is improved, so that better economic efficiency and social efficiency are generated.

Description

Capacitor nickel electroplating solution, electroplating method and application
Technical Field
The invention relates to the technical field of electronic component processing, in particular to a capacitor nickel electroplating solution, an electroplating method and application.
Background
In recent years, with the development of electronic devices toward short, small, light and thin devices, surface mount technology and surface mount components have been rapidly developed. This of course also accelerates the development of the chip capacitor industry, which, like other chip components (SMC and SMD), is a new generation of leadless or short-lead microelectronic components suitable for Surface Mount Technology (SMT). 0201 type chip capacitor devices are now widely used, but some problems in the industrialization process need to be solved urgently.
The 0201 type chip capacitor has small size and small metalized part at the end, so that the time for electroplating is long by using the conventional nickel electroplating technology, the product is seriously worn in the electroplating process and is easily corroded by electroplating solution to cause the electric performance failure of the product, and the nickel layer of the electroplated product is rough in crystallization to easily cause the poor welding resistance of the product. These are all the problems that 0201 type chip capacitors are urgently needed to be solved in the process of industrialization, and the industrialization process of 0201 type chip capacitors is directly influenced due to the restriction of nickel electroplating technology.
Disclosure of Invention
Therefore, the plating solution and the plating method are adopted to carry out nickel plating on the 0201 type chip capacitor, so that the plating efficiency of the 0201 type chip capacitor can be effectively improved, the product has good welding resistance, the nickel plating solution has no corrosion to the product, the plating layer is uniform and compact, does not peel off, does not fall off and is corrosion-resistant, the process is simple, energy is saved, the environment is protected, and the cost is greatly reduced.
A capacitor nickel electroplating solution comprises a pre-plating treatment solution and a main electroplating solution;
the pre-plating treatment solution comprises: 1-10g/L of organic acid and 5-20g/L of complexing agent;
the main electroplating solution comprises: 10-20g/L of nickel-containing metal salt, 300-500g/L of conductive salt, 40-50g/L of buffering agent, 0.01-0.1g/L of stress relieving agent and 2-20g/L of nickel ion stabilizing agent.
The capacitor nickel electroplating solution comprises a pre-plating treatment solution and a main electroplating solution, wherein the pre-plating treatment solution is activated by using an organic acid, so that the activity of a bottom substrate of a capacitor (particularly a 0201 chip capacitor) can be enhanced, and the capacitor nickel electroplating solution can be electroplated more easily; but also can prevent the surface of the steel from being corroded too fast by acid to cause the damage of the bottom layer and influence the product performance. The complexing agent is used for completely complexing copper ions in the activating solution, so that the surface of the component is cleaner. In the main electroplating liquid, the content of main nickel salt is lower than that of a common formula by more than 70 percent, and the main nickel salt is mainly used for improving the dispersing capacity and the covering capacity of the electroplating liquid, reducing the electroplating cost and reducing the burden of wastewater treatment; the content of the buffer is higher than that of the common formula, and the buffer is mainly used for keeping the pH value of the neutral nickel electroplating solution to be stable between 6.5 and 7.5 in the using process; the conventional nickel electroplating technology is conductive by using main nickel salt, and does not need to add conductive salt, but the conductivity of the invention is improved by adding the conductive salt because the main nickel salt content is low and the solution conductive effect is poor; meanwhile, the internal stress of the electroplated nickel layer is increased by using the conductive salt with the sodium salt as the formula, so that the internal stress of the nickel layer is reduced by adding the stress relieving agent; in addition, because the pH value is only controlled between 6.5 and 7.5, nickel ions are easy to combine with hydroxide radicals to form nickel hydroxide suspended substances in the pH value range, and the adverse phenomena of loose crystallization, coating peeling and the like of a nickel layer are caused. Therefore, the nickel ion stabilizer is added in the invention, so that the nickel ions can stably exist in 6.5-7.5 without forming nickel hydroxide suspended matters.
In one embodiment, the pH of the pre-plating treatment solution is 3.5 to 5.0, and the pH of the main electroplating solution is 6.5 to 7.5.
In one embodiment, the organic acid is selected from: at least one of citric acid, malic acid and tartaric acid; the complexing agent is selected from: at least one of sodium gluconate, sodium citrate and potassium sodium tartrate.
In one embodiment, the nickel-containing metal salt is selected from: at least one of nickel sulfamate, nickel sulfate, nickel chloride and nickel oxalate.
In one embodiment, the conductive salt is selected from: at least one of sodium sulfamate, sodium sulfate, sodium chloride and sodium acetate.
In one embodiment, the buffer is selected from: at least one of boric acid, sodium tetraborate, sodium oxalate and sodium citrate.
In one embodiment, the stress relief agent is selected from: at least one of sodium o-benzoylsulfonimide, bis-benzenesulfonylimide, sodium allylsulfonate and sodium propiolate; the nickel ion stabilizer is selected from: at least one of disodium ethylene diamine tetraacetate, tetrasodium ethylene diamine tetraacetate, sodium potassium tartrate and sodium alginate.
The invention also discloses a capacitor nickel electroplating method, which comprises the following steps:
pretreatment: activating the product by adopting the pre-plating treatment liquid;
nickel electroplating: the main electroplating solution is adopted to electroplate the product.
In one embodiment, in the pretreatment step, the pH value is controlled to be 3.5-5.0, the temperature is controlled to be 10-40 ℃, and the activation time is controlled to be 60-180 s; in the nickel electroplating step, the pH value is controlled to be 6.5-7.5, the electroplating temperature is controlled to be 40-60 ℃, and the electroplating current density is controlled to be 0.2-0.6A/dm 2; the electroplating time is 80-120 min.
The invention also discloses application of the capacitor nickel electroplating solution in 0201 surface mount capacitor nickel electrodeposition.
Compared with the prior art, the invention has the following beneficial effects:
according to the capacitor nickel electroplating solution, the plating pretreatment solution and the main electroplating solution are matched for use, so that the activity of the 0201 type chip capacitor can be improved in the plating pretreatment process, and the plating efficiency of the capacitor nickel electroplating solution is improved by more than 15%; the pH value of the main electroplating solution is 7.0 +/-0.5, the pH value belongs to neutrality, and the electroplating technology can reach zero corrosion for 0201 type chip components.
Meanwhile, the nickel content in the nickel electroplating solution is lower than that of the prior domestic equivalent technology by more than 70 percent, so that the content of nickel ions in the wastewater is reduced, the difficulty of sewage treatment is reduced, the burden of three-waste treatment is relieved, and the addition of the nickel ions can be reduced in daily maintenance, thereby reducing the production cost.
In addition, the conductive salt is used for replacing nickel ions for conducting, the conductivity of the nickel plating solution can be enhanced, the electroplating efficiency of a low-current density section of the nickel plating solution can be improved, the plating layer is bright and full in appearance, high in hardness, good in toughness and ductility, and the electroplated nickel plating layer is compact in crystallization.
Through the technical means, the invention can solve the problems existing in the process of electroplating the 0201 type chip capacitor, and mainly solves the problems of improving the efficiency of nickel electroplating and the electrical property failure of the product caused by the corrosion of the 0201 type chip capacitor product by the nickel electroplating solution. The nickel electroplating solution can be applied to the nickel electroplating of the 0201 type chip capacitor, can replace the existing nickel electroplating technology to be applied to other types of chip capacitors, has higher electroplating efficiency and better welding resistance, and can better solve the problem of corrosion of the nickel electroplating solution to products. After the device is used, the production efficiency of components can be greatly improved, the production cost is reduced, and the product performance is improved, so that better economic efficiency and social efficiency are generated.
Drawings
FIG. 1 is a schematic view showing that the copper bottom layer of the product after pretreatment and activation in the example is bright and has no obvious corrosion;
FIG. 2 is a schematic diagram illustrating the copper underlayer corrosion caused by the conventional activation process in an embodiment with an excessively long activation time;
FIG. 3 is an electron micrograph (1000 times magnification) of the product of example 1;
FIG. 4 is an electron micrograph (1000 times magnification) of a product of comparative example 1;
FIG. 5 is a schematic view of the welding effect of the product of example 1;
FIG. 6 is a schematic view of the welding effect of the product of example 1.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The starting materials used in the following examples are all commercially available unless otherwise specified.
Example 1
A0201 type capacitor is subjected to nickel electroplating treatment by adopting the following nickel electroplating solution and electroplating method:
1. and (4) pretreatment.
1.1 Pre-plating treatment solution.
The plating pretreatment liquids used are shown in the following table.
TABLE 1 pretreatment solution Components for plating
Composition (I) Name of Material Content (wt.)
Organic acids Citric acid 5g/L
Complexing agents Citric acid sodium salt 20g/L
1.2 pretreatment process of plating.
The pH value of the pre-plating treatment solution is controlled to be 4.0, and the pre-plating treatment solution is washed and activated for 60 seconds at room temperature.
2. And (4) nickel electroplating.
2.1 the main baths used are shown in the following table.
TABLE 2 Main electroplating bath composition
Composition (I) Materials name/Process Content (wt.)
Main salt (Nickel-containing metal salt) Nickel sulfate 15g/L
Buffering agent Sodium tetraborate 40g/L
Conductive salt Sodium sulfate 300g/L
Stress relieving agent Bis (phenylsulfonyl)Imine(s) 0.1g/L
Nickel ion stabilizer Ethylenediaminetetraacetic acid disodium salt 10g/L
2.2 nickel electroplating process.
The pH value of the main electroplating solution is 7.0, the electroplating temperature is 50 ℃, and the electroplating current density is 0.4A/dm2(ii) a The electroplating time is 100 min.
Example 2
A0201 type capacitor is subjected to nickel electroplating treatment by adopting the following nickel electroplating solution and electroplating method:
1. and (4) pretreatment.
1.1 Pre-plating treatment solution.
The plating pretreatment liquids used are shown in the following table.
TABLE 3 pretreatment solution Components before plating
Composition (I) Name of Material Content (wt.)
Organic acids Malic acid 10g/L
Complexing agents Sodium gluconate 20g/L
1.2 pretreatment process of plating.
Controlling the pH value of the pre-plating treatment solution to be 3.5, and washing and activating for 90 seconds at room temperature.
2. And (4) nickel electroplating.
2.1 the main baths used are shown in the following table.
TABLE 4 Main electroplating bath composition
Composition (I) Materials name/Process Content (wt.)
Main salt (Nickel-containing metal salt) Nickel sulfamate 20g/L
Buffering agent Boric acid 45g/L
Conductive salt Aminosulfonic acid sodium salt 400g/L
Stress relieving agent O-benzoylsulfonimide sodium salt 0.05g/L
Nickel ion stabilizer Tartaric acid potassium sodium salt 20g/L
2.2 nickel electroplating process.
The pH value of the main electroplating solution is 7.5, the electroplating temperature is 40 ℃, and the electroplating current density is 0.6A/dm2(ii) a The electroplating time is 80 min.
Example 3
A0201 type capacitor is subjected to nickel electroplating treatment by adopting the following nickel electroplating solution and electroplating method:
1. and (4) pretreatment.
1.1 Pre-plating treatment solution.
The plating pretreatment liquids used are shown in the following table.
TABLE 5 pretreatment solution Components before plating
Composition (I) Name of Material Content (wt.)
Organic acids Tartaric acid 10g/L
Complexing agents Tartaric acid potassium sodium salt 20g/L
1.2 pretreatment process of plating.
The pH value of the pre-plating treatment solution is controlled to be 4.5, and the pre-plating treatment solution is washed and activated for 120 seconds at room temperature.
2. And (4) nickel electroplating.
2.1 the main baths used are shown in the following table.
TABLE 6 Main electroplating bath composition
Composition (I) Materials name/Process Content (wt.)
Main salt (Nickel-containing metal salt) Nickel chloride 10g/L
Buffering agent Sodium oxalate 45g/L
Conductive salt Sodium chloride 400g/L
Stress relieving agent Sodium propiolate 0.05g/L
Nickel ion stabilizer Sodium alginate 20g/L
2.2 nickel electroplating process.
The pH value of the main electroplating solution is 6.5, the electroplating temperature is 60 ℃, and the electroplating current density is 0.2A/dm2(ii) a The plating time was 120 min.
Comparative example 1
A0201 type capacitor is subjected to nickel electroplating treatment by adopting the following nickel electroplating solution and electroplating method:
1. the plating solutions are shown in the following table.
TABLE 7 electroplating bath composition
Composition (I) Materials name/Process Content (wt.)
Main salt (Nickel-containing metal salt) Nickel sulfate 150g/L
Buffering agent Boric acid 35g/L
2. And (4) nickel electroplating process.
The pH value of the electroplating solution is 3.5, the electroplating temperature is 50 ℃, and the electroplating current density is 1A/dm2(ii) a The electroplating time is 150 min.
Examples of the experiments
The 0201 type chip capacitor products prepared in the above examples and comparative examples were subjected to a post-plating performance test in accordance with the standard for conventional ceramic capacitor inspection, and the test results are shown in the following table.
TABLE 8 after-plating Performance of the product
The results show that the 0201 type chip capacitor product treated by the nickel electroplating solution and the electroplating method in the embodiment of the invention has the advantages of no corrosion, compact crystallization of the nickel layer, no pinhole, thicker nickel layer, good welding resistance, low electrical property change rate, high tin coating rate after aging and excellent effect.
Wherein, the photo of the copper bottom layer of the product in example 1 is shown in figure 1, and it can be seen from the figure that the copper bottom layers at the two ends of the product are bright and have no obvious corrosion; the photograph of the copper underlayer of the product of comparative example 1 is shown in fig. 2, and it can be seen that the condition causes corrosion of the corners and magnetic exposure.
An electron microscope image obtained by observing the product of example 1 under a 1000-fold electron microscope is shown in FIG. 3, and it can be seen from the image that the nickel layer is dense in crystallization and has no pinholes; the electron microscope image of the product of comparative example 1 observed under 1000 times electron microscope is shown in fig. 4, and it can be seen from the image that the nickel layer crystal particles are loosely arranged and have pinholes.
In addition, the electroplated nickel of the invention has low concentration, compact electroplating crystal and is beneficial to product welding, and the welded end of the electroplated product is full and bright as shown in figure 5. The welding effect of the product of the embodiment 1 is poor, as shown in figure 6.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the appended claims.

Claims (10)

1. The capacitor nickel electroplating solution is characterized by comprising a pre-plating treatment solution and a main electroplating solution;
the pre-plating treatment solution comprises: 1-10g/L of organic acid and 5-20g/L of complexing agent;
the main electroplating solution comprises: 10-20g/L of nickel-containing metal salt, 300-500g/L of conductive salt, 40-50g/L of buffering agent, 0.01-0.1g/L of stress relieving agent and 2-20g/L of nickel ion stabilizing agent.
2. The capacitor nickel plating solution according to claim 1, wherein the pH of the pre-plating solution is 3.5 to 5.0, and the pH of the main plating solution is 6.5 to 7.5.
3. The capacitor nickel plating solution of claim 1, wherein the organic acid is selected from the group consisting of: at least one of citric acid, malic acid and tartaric acid; the complexing agent is selected from: at least one of sodium gluconate, sodium citrate and potassium sodium tartrate.
4. The capacitor nickel plating bath of claim 1, wherein the nickel-containing metal salt is selected from the group consisting of: at least one of nickel sulfamate, nickel sulfate, nickel chloride and nickel oxalate.
5. The capacitor nickel plating solution of claim 1, wherein the conductive salt is selected from the group consisting of: at least one of sodium sulfamate, sodium sulfate, sodium chloride and sodium acetate.
6. The capacitor nickel plating solution of claim 1, wherein the buffer is selected from the group consisting of: at least one of boric acid, sodium tetraborate, sodium oxalate and sodium citrate.
7. The capacitor nickel plating bath of claim 1, wherein the stress relief agent is selected from the group consisting of: at least one of sodium o-benzoylsulfonimide, bis-benzenesulfonylimide, sodium propenyl sulfonate and sodium propiolate; the nickel ion stabilizer is selected from: at least one of disodium ethylene diamine tetraacetate, tetrasodium ethylene diamine tetraacetate, sodium potassium tartrate and sodium alginate.
8. A nickel electroplating method for a capacitor is characterized by comprising the following steps:
pretreatment: activating a product by using the pretreatment liquid for plating described in any one of claims 1 to 7;
nickel electroplating: electroplating the product using the primary electroplating bath according to any one of claims 1 to 7.
9. The capacitor nickel plating solution as claimed in claim 1,
in the pretreatment step, the pH value is controlled to be 3.5-5.0, the temperature is controlled to be 10-40 ℃, and the activation time is 60-180 s;
in the nickel electroplating step, the pH value is controlled to be 6.5-7.5, the electroplating temperature is controlled to be 40-60 ℃, and the electroplating current density is controlled to be 0.2-0.6A/dm2(ii) a The electroplating time is 80-120 min.
10. Use of the capacitor nickel electroplating solution of any one of claims 1-7 in 0201 surface mount capacitor nickel electrodeposition.
CN201911190868.1A 2019-11-28 2019-11-28 Capacitor nickel electroplating solution, electroplating method and application Pending CN111041531A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111607816A (en) * 2020-06-03 2020-09-01 暨南大学 Method for pulse electrodeposition of Ni-SiC composite coating on surface of aluminum alloy
CN112342584A (en) * 2020-09-29 2021-02-09 扬州市景杨表面工程有限公司 Nonmagnetic copper-tin electroplating process for capacitor device of cardiac pacemaker

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103014795A (en) * 2012-11-22 2013-04-03 大连滨城活塞制造有限公司 Bush plating solution for cylinder sleeve
CN104593843A (en) * 2015-02-04 2015-05-06 广东羚光新材料股份有限公司 Normal temperature pretreatment method for electroplating chip multilayer ceramic capacitor
CN107587173A (en) * 2017-10-17 2018-01-16 广东羚光新材料股份有限公司 A kind of nickel plating solution and its application

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103014795A (en) * 2012-11-22 2013-04-03 大连滨城活塞制造有限公司 Bush plating solution for cylinder sleeve
CN104593843A (en) * 2015-02-04 2015-05-06 广东羚光新材料股份有限公司 Normal temperature pretreatment method for electroplating chip multilayer ceramic capacitor
CN107587173A (en) * 2017-10-17 2018-01-16 广东羚光新材料股份有限公司 A kind of nickel plating solution and its application

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111607816A (en) * 2020-06-03 2020-09-01 暨南大学 Method for pulse electrodeposition of Ni-SiC composite coating on surface of aluminum alloy
CN112342584A (en) * 2020-09-29 2021-02-09 扬州市景杨表面工程有限公司 Nonmagnetic copper-tin electroplating process for capacitor device of cardiac pacemaker

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Application publication date: 20200421