CN110306220B - Electroplating process for connector - Google Patents

Electroplating process for connector Download PDF

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Publication number
CN110306220B
CN110306220B CN201910665091.3A CN201910665091A CN110306220B CN 110306220 B CN110306220 B CN 110306220B CN 201910665091 A CN201910665091 A CN 201910665091A CN 110306220 B CN110306220 B CN 110306220B
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nickel
plating
degreasing
washing
phosphorus
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CN110306220A (en
Inventor
朱秀芳
钱诚
孙锋
石莹莹
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Huizhou Jinxin Surface Treatment Co.,Ltd.
Jiangxi Liangben Information Technology Co ltd
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Huaiyin Institute of Technology
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/10—Electroplating with more than one layer of the same or of different metals
    • C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
    • C25D5/14—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium two or more layers being of nickel or chromium, e.g. duplex or triplex layers
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34—Pretreatment of metallic surfaces to be electroplated
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F1/00—Electrolytic cleaning, degreasing, pickling or descaling
    • C25F1/02—Pickling; Descaling
    • C25F1/04—Pickling; Descaling in solution

Abstract

The invention relates to the technical field of electroplating of electronic connectors, and discloses a connector electroplating process, which comprises the following steps: degreasing: firstly, ultrasonic degreasing, then cathode electrolytic degreasing, and finally anode electrolytic degreasing; degreasing and washing with water; and (3) activation: carrying out anodic electrolysis activation on the solid inorganic acid salt aqueous solution, and washing with water after activation; nickel plating: firstly plating nickel-phosphorus-tellurium multi-element alloy nickel, plating semi-gloss nickel after washing, and plating nickel-phosphorus-tellurium multi-element alloy nickel after washing. Compared with the prior art, the process optimizes the pretreatment, water washing and nickel plating processes, particularly the design optimization of the multi-element alloy nickel layer, so that the plating layer has a flat and pinhole-free surface under the observation of a 1000-time microscope, a salt spray test can be carried out without using an organic hole sealing film after electroplating, and a product has no potential quality hazards of impedance and soldering tin when in use; after the plating layer is electroplated on the connector by the electroplating process, sodium chloride can be effectively prevented from entering the plating layer during a salt spray test, and the corrosion of the primary battery is effectively avoided.

Description

Electroplating process for connector
Technical Field
The invention relates to the technical field of electroplating of electronic connectors, in particular to a connector electroplating process.
Background
The electroplating of the connector needs nickel plating to play a role in priming and corrosion resistance, and then gold, tin and the like are plated on the nickel layer. In the last two years, the salt fog judgment standard of the plating layer of the electronic connector is continuously tightened, the requirement on the salt fog is more severe, the contact area is judged only by early visual observation and the grade is judged according to the corrosion area, and then the whole product at the later stage is not corroded by any visual observation, but the current judgment standard is that all products are judged to pass through without any defect after the salt fog test under a 40-time microscope. The conventional electroplating process solution is to use a sealant after electroplating, and the sealant is an organic substance, which has functional hidden troubles for impedance and soldering tin, and has a risk of seriously affecting impedance or causing short circuit after carbonization on high-current connectors (such as USB interfaces and BATTERY).
Disclosure of Invention
The purpose of the invention is as follows: aiming at the problems in the prior art, the invention provides a connector electroplating process, the electroplated connector can meet the requirements of the current plating salt spray test, an organic hole sealing film is not used, and the product has no hidden quality trouble in use.
The technical scheme is as follows: the invention provides a connector electroplating process, which comprises the following steps: degreasing: firstly, ultrasonic degreasing, then cathode electrolytic degreasing, and finally anode electrolytic degreasing; degreasing and washing with water; and (3) activation: carrying out anodic electrolysis activation on the solid inorganic acid salt aqueous solution, and washing with water after activation; nickel plating: firstly plating nickel-phosphorus-tellurium multi-element alloy nickel, plating semi-gloss nickel after washing, and plating nickel-phosphorus-tellurium multi-element alloy nickel after washing.
Preferably, in the activation step, the solid inorganic acid salt aqueous solution is a mixed aqueous solution of ammonium bifluoride and sodium fluoride.
Preferably, the preparation method of the mixed aqueous solution of ammonium bifluoride and sodium fluoride is as follows: after 30% of ammonium bifluoride and 70% of sodium fluoride are uniformly mixed, weighing 80-100 g/L of the mixture to prepare an aqueous solution.
The voltage during the electrolytic activation is 3-5V.
Preferably, in the nickel plating step, when the nickel-phosphorus-tellurium multi-element alloy is plated for the first time, the mass percent of phosphorus is 0.1-0.2%, and the mass percent of tellurium is 0.1-0.2%.
Preferably, in the nickel plating step, when the nickel-phosphorus-tellurium multi-element alloy is plated for the second time, the mass percent of phosphorus is 0.1-0.2%, and the mass percent of tellurium is 0.1-0.2%.
Preferably, in the degreasing step, the temperature of the bath solution in the ultrasonic degreasing is 60 ℃; and the current density of the cathode electrolytic degreasing and the current density of the anode electrolytic degreasing are both 12-18 ASD.
Preferably, the step of washing with water after degreasing is as follows: and after two normal-temperature water washes, performing one hot water wash at 45-55 ℃.
Preferably, the water washing step after activation is: and after two normal-temperature water washes, performing one hot water wash at 45-55 ℃.
Preferably, the water washing steps after the first nickel-phosphorus-tellurium multi-element alloy nickel plating and after the semi-gloss nickel plating are as follows: and after two normal-temperature water washes, performing one hot water wash at 45-55 ℃. The residual electroplating liquid on the surface of the plating layer can be fully cleaned by hot water washing, and no impurity is left between the plating layer and the plating layer.
Has the advantages that: in the connector electroplating process, the degreasing adopts a mixed degreasing mode of cathode degreasing and anode degreasing, hydrogen is separated out from the surface of a product during cathode degreasing, oxygen is separated out from the surface of the product during anode degreasing, and oxygen molecules are larger than hydrogen molecules, so that the anode degreasing can quickly and effectively impact and tear an oil film, and a better degreasing effect is achieved; the activation is anodic electrolytic activation of solid inorganic acid aqueous solution, the traditional process using sulfuric acid activation can only remove the oxide on the surface of the substrate, but the process can not only remove the oxide on the surface of the substrate, but also remove the burrs of the substrate and polish and level the scratches and other defects of the substrate by using fluoride anodic electrolysis, so that the coating is level, and sodium chloride is more difficult to permeate into the coating when a salt spray test is carried out, thereby playing a role in corrosion resistance; the nickel plating is to plate nickel-phosphorus-tellurium multi-element alloy nickel firstly, then plate common semi-gloss nickel, and finally plate a layer of nickel-phosphorus-tellurium multi-element alloy nickel, the molecular lattice of the nickel-phosphorus-tellurium multi-element alloy plating layer is flat and compact, the pores among the nickel in the process of using multi-layer nickel plating are minimum, and sodium chloride is more difficult to permeate into the plating layer, thereby playing a role in corrosion resistance.
The process is a continuous metal electroplating process for the electronic connector, the pretreatment, water washing and nickel plating processes are optimized, particularly the design of a multi-element alloy nickel layer is optimized, so that the plating layer has small pores, the flatness and no pinholes are observed on the surface of the plating layer under a 1000-time microscope, a salt spray test can be carried out without using an organic hole sealing film after electroplating, the product has no potential quality hazards of impedance and soldering tin when used at the terminal, and the electroplating cost can be saved; the requirement of the plating layer of the connector of the electronic product on the salt spray test is met, and after the plating layer is electroplated on the connector through the electroplating process, sodium chloride can be effectively prevented from entering the plating layer during the salt spray test, and the corrosion of a primary battery is effectively avoided.
Drawings
FIG. 1 is a flow chart of a plating process for a connector according to the present invention;
FIG. 2 is an SEM photograph of a plated layer formed by the plating process according to embodiment 1;
FIG. 3 is an SEM image of a plated layer formed by a prior art electroplating process.
FIG. 4 is a 40-hour microscopic photograph of the plating layer formed by the electroplating process of embodiment 1 without the organic film salt spray test;
FIG. 5 is a 40-hour microscopic photograph of a prior art plating process without an organic film salt spray test.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
Embodiment 1:
the embodiment provides a connector electroplating process, the flow of the process is as shown in fig. 1, firstly, a connector to be plated is placed in an electroplating bath, and then, degreasing treatment is carried out on the connector, wherein the degreasing treatment process comprises the following steps:
keeping the temperature of bath solution at 60 ℃, firstly carrying out ultrasonic degreasing on the connector to be plated for 5-10 seconds, then keeping the current density at 12-18 ASD (at the moment, the temperature of bath solution is still 60 ℃) to carry out cathodic electrolytic degreasing (connecting the connector to be plated with a cathode) for 10-20 seconds, and finally keeping the current density at 12-18 ASD (at the moment, the temperature of bath solution is still 60 ℃) to carry out anodic electrolytic degreasing (connecting the connector to be plated with an anode) for 5-10 seconds; after degreasing, washing the degreased waste water by two times of normal-temperature water, and then washing the degreased waste water by one time of hot water at the temperature of 45-55 ℃.
After degreasing and washing, carrying out acid washing activation on the connector to be plated, wherein the acid washing activation process comprises the following steps:
the connector to be plated (connected with the anode) is placed in a mixed aqueous solution of ammonium bifluoride and sodium fluoride (the preparation method of the mixed aqueous solution of ammonium bifluoride and sodium fluoride is that after 30 percent of ammonium bifluoride and 70 percent of sodium fluoride are uniformly mixed, 90 g/L of the mixture is weighed to prepare an aqueous solution), and acid washing activation is carried out, and the electrifying voltage is 3V. After activation, the mixture is washed by two times of normal-temperature water and then washed by hot water at the temperature of 45-55 ℃ for one time.
And (3) after activation and water washing, carrying out nickel plating on the strip-plated connector: the nickel plating process is as follows:
firstly plating nickel-phosphorus-tellurium multi-element alloy nickel, wherein the mass percent of phosphorus is 0.1%, and the mass percent of tellurium is 0.2%, then washing the nickel-phosphorus-tellurium multi-element alloy by two times of normal-temperature water, and then washing the nickel-phosphorus-tellurium multi-element alloy nickel by hot water at the temperature of 45-55 ℃;
after washing, plating semi-gloss nickel, washing with two pieces of normal-temperature water, and washing with hot water at the temperature of 45-55 ℃ for one time;
and (3) plating nickel-phosphorus-tellurium multi-element alloy nickel again after washing, wherein the mass percent of phosphorus is 0.1 percent, and the mass percent of tellurium is 0.2 percent.
Thus, the electroplating process is completed.
Fig. 2 is a picture of the plating layer prepared by the electroplating process according to the embodiment, which is observed under a scanning electron microscope of 1000 times, and it can be seen that the plating layer is flat and has no pores, sodium chloride does not enter the plating layer during the salt spray test, and the plating layer is not corroded after the salt spray test (see fig. 4).
However, in the prior art (ultrasonic degreasing and cathodic electrolytic degreasing or anodic electrolytic degreasing are used during degreasing, sulfuric acid or hydrochloric acid is used for activation during activation, and only one layer of common semi-gloss nickel is plated during nickel plating), the prepared plating layer is rough and uneven in surface and has more pores, sodium chloride easily enters the plating layer during a salt spray test, and the plating layer is severely corroded after the salt spray test (as shown in fig. 5).
Embodiment 2:
the embodiment provides a connector electroplating process, and the degreasing process is completely the same as that of the embodiment 1; in the acid washing activation process, after 30 percent of ammonium bifluoride and 70 percent of sodium fluoride are uniformly mixed, 80 g/L of the mixture is weighed to prepare an aqueous solution, the electrifying voltage is 4V, and the rest is completely the same as that of the embodiment 1; in the nickel plating process, when the first nickel-phosphorus-tellurium multi-element alloy is plated with nickel, the mass percent of phosphorus in the first nickel-phosphorus-tellurium multi-element alloy is 0.2%, the mass percent of tellurium in the second nickel-phosphorus-tellurium multi-element alloy is 0.2%, the mass percent of phosphorus in the second nickel-phosphorus-tellurium multi-element alloy is 0.2%, and the rest is completely the same as that in the embodiment 1, and details are not repeated here.
Embodiment 3:
the embodiment provides a connector electroplating process, and the degreasing process is completely the same as that of the embodiment 1; in the acid washing activation process, after 30 percent of ammonium bifluoride and 70 percent of sodium fluoride are uniformly mixed, 100 g/L of the mixture is weighed to prepare an aqueous solution, the electrifying voltage is 4V, and the rest is completely the same as that of the embodiment 1; in the nickel plating process, when the nickel-phosphorus-tellurium multi-element alloy is plated for the first time, the mass percent of phosphorus in the nickel-phosphorus-tellurium multi-element alloy is 0.1%, the mass percent of tellurium in the nickel-phosphorus-tellurium multi-element alloy is 0.1%, the mass percent of phosphorus in the nickel-phosphorus-tellurium multi-element alloy is 0.1%, and the rest is completely the same as that in the embodiment 1, and details are not repeated here.
Embodiment 4:
the embodiment provides a connector electroplating process, and the degreasing process is completely the same as that of the embodiment 1; in the acid washing activation process, after 30 percent of ammonium bifluoride and 70 percent of sodium fluoride are uniformly mixed, 90 g/L of the mixture is weighed to prepare an aqueous solution, the electrifying voltage is 5V, and the rest is completely the same as that of the embodiment 1; in the nickel plating process, when the nickel-phosphorus-tellurium multi-element alloy is plated for the first time, the mass percent of phosphorus in the nickel-phosphorus-tellurium multi-element alloy is 0.2%, the mass percent of tellurium in the nickel-phosphorus-tellurium multi-element alloy is 0.1%, and when the nickel-phosphorus-tellurium multi-element alloy is plated for the second time, the mass percent of phosphorus in the nickel-phosphorus-tellurium multi-element alloy is 0.2%, the mass percent of tellurium in the nickel-phosphorus-tellurium multi-element alloy is 0.1%.
The above embodiments are merely illustrative of the technical concepts and features of the present invention, and the purpose of the embodiments is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.

Claims (8)

1. A connector electroplating process is characterized in that: the method comprises the following steps:
degreasing: firstly, ultrasonic degreasing, then cathode electrolytic degreasing, and finally anode electrolytic degreasing; degreasing and washing with water;
and (3) activation: carrying out anodic electrolysis activation on the solid inorganic acid salt aqueous solution, and washing with water after activation;
wherein the solid inorganic acid salt aqueous solution is a mixed aqueous solution of ammonium bifluoride and sodium fluoride;
the preparation method of the mixed aqueous solution of ammonium bifluoride and sodium fluoride comprises the following steps: after 30% of ammonium bifluoride and 70% of sodium fluoride are uniformly mixed, weighing 80-100 g/L of the mixture to prepare an aqueous solution;
nickel plating: firstly plating nickel-phosphorus-tellurium multi-element alloy nickel, plating semi-gloss nickel after washing, and plating nickel-phosphorus-tellurium multi-element alloy nickel after washing.
2. The electroplating process for the connector as claimed in claim 1, wherein the voltage during the electrolytic activation is 3-5V.
3. The electroplating process for the connector as claimed in claim 1, wherein in the step of plating nickel, the first time of plating nickel-phosphorus-tellurium multi-element alloy nickel, the mass percent of phosphorus is 0.1-0.2%, and the mass percent of tellurium is 0.1-0.2%.
4. The electroplating process for the connector as claimed in claim 1, wherein in the step of plating nickel, the mass percent of phosphorus is 0.1-0.2% and the mass percent of tellurium is 0.1-0.2% in the second nickel-phosphorus-tellurium multi-element alloy plating process.
5. The electroplating process for the connector assembly according to any one of claims 1 to 4, wherein in the degreasing step, the temperature of the bath solution during the ultrasonic degreasing is 60 ℃; and the current density of the cathode electrolytic degreasing and the current density of the anode electrolytic degreasing are both 12-18 ASD.
6. The plating process for the connector as claimed in any one of claims 1 to 4, wherein the step of washing with water after degreasing is: and after two normal-temperature water washes, performing one hot water wash at 45-55 ℃.
7. The connector electroplating process according to any one of claims 1 to 4, wherein the water washing step after activation is: and after two normal-temperature water washes, performing one hot water wash at 45-55 ℃.
8. The electroplating process for the connector assembly according to any one of claims 1 to 4, wherein the steps of water washing after the first nickel-phosphorus-tellurium multi-element alloy nickel plating and after the semi-gloss nickel plating are as follows: and after two normal-temperature water washes, performing one hot water wash at 45-55 ℃.
CN201910665091.3A 2019-07-23 2019-07-23 Electroplating process for connector Active CN110306220B (en)

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Publication number Priority date Publication date Assignee Title
CN111215106A (en) * 2020-01-17 2020-06-02 陕西瑞科新材料股份有限公司 Preparation method of high-activity silicon carbide palladium catalyst
CN114318449A (en) * 2020-10-12 2022-04-12 江苏澳光电子有限公司 Innovative process for plating thin gold on silver

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3112502A1 (en) * 2015-06-30 2017-01-04 Vazzoler, Evio Method for plating metallic wire or tape and product obtained with said method
CN108315791A (en) * 2018-04-23 2018-07-24 江苏澳光电子有限公司 A kind of electronic connector electroplating technology
CN109208049A (en) * 2018-11-08 2019-01-15 天津亿鑫通金属表面处理有限公司 A kind of uniform stainless steel continuous plating process of tint

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3112502A1 (en) * 2015-06-30 2017-01-04 Vazzoler, Evio Method for plating metallic wire or tape and product obtained with said method
CN108315791A (en) * 2018-04-23 2018-07-24 江苏澳光电子有限公司 A kind of electronic connector electroplating technology
CN109208049A (en) * 2018-11-08 2019-01-15 天津亿鑫通金属表面处理有限公司 A kind of uniform stainless steel continuous plating process of tint

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