CN116575087A - Method for electroplating nickel-gold on kovar alloy - Google Patents
Method for electroplating nickel-gold on kovar alloy Download PDFInfo
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- CN116575087A CN116575087A CN202310432906.XA CN202310432906A CN116575087A CN 116575087 A CN116575087 A CN 116575087A CN 202310432906 A CN202310432906 A CN 202310432906A CN 116575087 A CN116575087 A CN 116575087A
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- 238000009713 electroplating Methods 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 45
- 229910000833 kovar Inorganic materials 0.000 title claims abstract description 33
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 32
- 239000000956 alloy Substances 0.000 title claims abstract description 32
- MSNOMDLPLDYDME-UHFFFAOYSA-N gold nickel Chemical compound [Ni].[Au] MSNOMDLPLDYDME-UHFFFAOYSA-N 0.000 title claims abstract description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 158
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 78
- 238000007747 plating Methods 0.000 claims abstract description 48
- 239000010931 gold Substances 0.000 claims abstract description 37
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910052737 gold Inorganic materials 0.000 claims abstract description 36
- 230000003213 activating effect Effects 0.000 claims abstract description 26
- 238000005238 degreasing Methods 0.000 claims abstract description 22
- 239000003960 organic solvent Substances 0.000 claims abstract description 14
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 11
- 239000000126 substance Substances 0.000 claims abstract description 9
- 238000005554 pickling Methods 0.000 claims abstract description 7
- 230000003116 impacting effect Effects 0.000 claims abstract description 3
- 230000004913 activation Effects 0.000 claims description 69
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 67
- 238000005406 washing Methods 0.000 claims description 60
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 18
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 13
- 238000004140 cleaning Methods 0.000 claims description 13
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 11
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- 230000005484 gravity Effects 0.000 claims description 10
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 8
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 8
- 239000004327 boric acid Substances 0.000 claims description 8
- IZLAVFWQHMDDGK-UHFFFAOYSA-N gold(1+);cyanide Chemical compound [Au+].N#[C-] IZLAVFWQHMDDGK-UHFFFAOYSA-N 0.000 claims description 8
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 8
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 8
- 229910052700 potassium Inorganic materials 0.000 claims description 8
- 239000011591 potassium Substances 0.000 claims description 8
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 6
- 238000009472 formulation Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000003208 petroleum Substances 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 238000003466 welding Methods 0.000 abstract description 12
- 238000005187 foaming Methods 0.000 abstract description 9
- 238000010923 batch production Methods 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000009863 impact test Methods 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 238000005476 soldering Methods 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000005282 brightening Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- NRTDAKURTMLAFN-UHFFFAOYSA-N potassium;gold(3+);tetracyanide Chemical compound [K+].[Au+3].N#[C-].N#[C-].N#[C-].N#[C-] NRTDAKURTMLAFN-UHFFFAOYSA-N 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- C25D7/00—Electroplating characterised by the article coated
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The invention discloses a method for electroplating nickel-gold on kovar alloy, which comprises the following steps: hanging, degreasing by an organic solvent, chemical degreasing, cathodic electrolysis degreasing, pickling, activating, nickel impacting, activating, nickel electroplating, activating, gold electroplating and the like; the invention has simple process, low cost and suitability for batch production, solves the problems of high-temperature foaming and laser seal welding foaming of the kovar alloy after nickel electroplating and gold electroplating, can meet the requirement of the later-stage laser seal welding of products, and has good plating binding force.
Description
Technical Field
The invention relates to a method for electroplating nickel-gold on a kovar alloy.
Background
The Kovar alloy of the invention refers to Kovar alloy (Ni 29%, co17%, and the balance Fe), which is a material widely used for airtight packaging, because the thermal expansion coefficient of the Kovar alloy is matched with that of other packaging components (such as glass-metal sealing), and the electroplated Kovar alloy has good corrosion resistance and good machining performance. Kovar is more dense and heavier than aluminum, has little problems with respect to weld metallurgy than aluminum alloys, and has the advantage of low coefficient of thermal expansion.
Many hermetic packages employ electroplating to improve corrosion resistance, solderability, or better absorb laser energy. Nickel and gold are the most common electroplating materials; the gold-plated kovar alloy package has good welding performance, and only needs to use electroplated nickel as a bottom plating layer.
There are many reports on nickel plating, gold plating and silver plating of kovar alloy at present, such as "research on silver plating process of kovar alloy" of Tan Zhishen et al, and such as chinese patent application CN 104466589A;
these methods, which have been reported to date, have the following problems: (1) High-temperature foaming after nickel electroplating and gold electroplating of the kovar alloy, and laser seal welding foaming; (2) The electroplating process is unstable, and the quality of electroplated products in different batches is different; (3) The process is not universal, the steps are complex, and the method is not suitable for batch production.
Disclosure of Invention
The invention aims to provide a method for electroplating nickel-gold on kovar alloy to solve the problems.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: a method for electroplating nickel-gold on kovar alloy, comprising the following steps: hanging, degreasing by an organic solvent, chemical degreasing, cathodic electrolysis degreasing, pickling, activating, nickel impacting, activating, nickel electroplating, activating and gold electroplating, and the specific steps are as follows:
(1) Hanging: hanging a workpiece to be treated;
(2) Deoiling by using an organic solvent: soaking a workpiece in an organic solvent to remove greasy dirt on the surface, and then drying to remove the organic solvent on the surface;
(3) Chemical degreasing: immersing the dried workpiece treated in the step (2) in the heated solution; simultaneously turning on ultrasonic waves, and then carrying out overflow double-water washing, wherein the temperature is 60-80 ℃ and the time is 5-10min;
(4) Cathode electrolysis degreasing: will step by stepImmersing the dried workpiece treated in the step (3) in a heated cathode electrolytic oil removing groove for oil removal treatment, and then carrying out overflow double water washing; the temperature is 55-65deg.C, the residence time in the solution is 55-65s, and the cathode current density is 2.5-3.5A/dm 2 ；
(5) Acid washing: placing the workpiece treated in the step (4) in an acid solution, and then carrying out overflow double-water washing; the temperature is normal temperature, and the residence time in the solution is 30-60min; then ultrasonic cleaning is carried out;
(6) Activating: placing the workpiece treated in the step (5) into an activation tank, completely immersing the workpiece into an activation solution, and then performing overflow double-water washing; the activation temperature is room temperature, and the activation time is 35-55S;
(7) Impact nickel: placing the workpiece treated in the step (6) into a nickel impact groove for nickel impact, and then carrying out overflow double-water washing; the formulation of the impact nickel solution is as follows: 200-250g/L nickel chloride, 250-300ml/L hydrochloric acid, current density 9-11A/dm 2 The time is 30-60S;
(8) Activating: placing the workpiece treated in the step (7) into an activation tank, completely immersing the workpiece into an activation solution, and then performing overflow double-water washing; the activation temperature is room temperature, and the activation time is 35-55S;
(9) Electroplating dark nickel: placing the workpiece treated in the step (8) into an electroplating dark nickel groove for electroplating dark nickel, and then carrying out overflow double-water washing; cathode current density: 0.5-1.5A/dm 2 Temperature: 50-60 ℃ and pH 4-5;
(10) Electroplating bright nickel: placing the workpiece treated in the step (9) into an electroplating dark and bright groove for electroplating bright nickel, and then carrying out overflow double-water washing; cathode current density: 1-3A/dm 2 Temperature: 50-60 ℃ and pH 4-5;
(11) Activating: placing the workpiece treated in the step (10) into an activation tank, completely immersing the workpiece into an activation solution, and then performing overflow double-water washing; the activation temperature is room temperature, and the activation time is 35-55S;
(12) Preplating: placing the workpiece treated in the step (11) into a preplating groove for preplating, and then carrying out overflow double-water washing; the pH of the preplating solution is 5.6-6.8, the specific gravity is 1.12-1.20g/cm, the temperature is 50-60 ℃, and the cathode current density is as follows: 0.1-0.3A/dm;
(13) Gold plating: and (3) putting the workpiece treated in the step (12) into a gold plating tank for gold plating, and then carrying out overflow double-water washing. The pH of the gold plating solution is 5.6-6.8, the specific gravity is 1.12-1.20g/cm, the temperature is 50-60 ℃, and the cathode current density is 0.2-0.4A/dm;
(14) Ultrasonic hot pure water cleaning: putting the workpiece treated in the step (13) into ultrasonic waves for cleaning;
(15) And (3) drying: and (5) putting the workpiece treated in the step (14) into an oven for drying.
As a preferable technical scheme: in the step (2), the organic solvent is petroleum ether.
As a preferable technical scheme: in the step (3), the solution is 50g/L deoiling powder solution.
As a preferable technical scheme: in step (5), the acid solution was 37wt% hcl.
As a preferable technical scheme: in the step (6), the step (8) and the step (11), the formula of the activating solution is 10-20wt% of dilute sulfuric acid solution.
As a preferable technical scheme: in the step (9) and the step (10), the formulas of the electroplating dark nickel solution and the electroplating bright nickel solution are as follows: nickel sulfate: 260-380 g/L, nickel chloride: 35-55 g/L, boric acid: 35-55 g/L.
As a preferable technical scheme: in the step (12), the formula of the pre-gold plating solution is as follows: potassium aurous cyanide: 0.8-3.0 g/L.
As a preferable technical scheme: in the step (13), the formula of the gold plating solution is as follows: 4.4-12 g/L of potassium aurous cyanide.
In order to solve the problems of nickel plating and high-temperature foaming after gold plating of the kovar alloy, unstable laser seal welding foaming and electroplating processes and different quality of electroplated products in different batches, the inventor finds that the main reasons are probably that the bonding force between a substrate of the kovar alloy and a coating is poor per se through a large number of experiments, and the inventor can achieve good effects by electroplating in an electroplating way of increasing acid pickling time and impact nickel, and does not find foaming phenomena after experiments are carried out at a high temperature of 300 ℃ for 10min and laser seal welding is carried out;
the invention has simple and easy realization process flow, does not need special pickling solution, and directly uses hydrochloric acid because similar kovar alloy nickel plating and gold plating processes are not available at present and are always difficult to produce.
The plating layer obtained by the electroplating method can meet the baking requirement of ten minutes at 300 ℃; the temperature impact test at the temperature of-55 ℃ to 125 ℃ can be satisfied, the temperature is kept for 0.25h at the limit temperature, the cycle times are 5 times, and the conversion time is 5 minutes; the method can meet the moisture resistance test of the method 106 in the GJB360B-2009 and the welding heat resistance test of the method 210 in the GJB 360B-2009;
the effect can be achieved and the whole flow is not separated, and the oxide skin on the surface of the kovar alloy is not easy to remove, so that the pickling time is prolonged to remove the oxide skin, and the oxide skin on the surface is better removed; in addition, the kovar alloy surface is not easy to directly form good binding force with the coating, so that the impact nickel is used as a bottom layer, and the binding force between the substrate and the coating is better.
Compared with the prior art, the invention has the advantages that: the invention has simple process, low cost and suitability for batch production, solves the problems of high-temperature foaming and laser seal welding foaming of the kovar alloy after nickel electroplating and gold electroplating, can meet the requirement of the later-stage laser seal welding of products, and has good plating binding force.
Description of the embodiments
The invention will be further illustrated with reference to examples.
In the following examples:
the solution used in chemical degreasing is a degreasing powder solution of 50g/L, wherein the degreasing powder is universal electrolytic powder U-251 (DR), solid powder and water for dissolving.
The solution used in the bright nickel electroplating is 0.75 mL/L bright nickel 88 brightening agent solution, purchased from Anmeite, the brand name is bright nickel 88 brightening agent, and the solvent is water; the bright nickel additive is purchased from Anmeite, the brand of which is nickel Y-19 wetting agent, and the solvent is water.
50g/L of gold-plating additive soft pure gold added during gold plating is purchased from Anmeite, the brand is K24 HF, and the solvent is water.
Example 1
Ni plating for kovar alloy cavity of filter of certain model 5 Au 1 Comprising the steps of:
1. hanging: fixing the workpiece on the hanger according to the requirement of hanging the operation instruction, wherein the fixing mode is strictly according to the operation instruction;
2. deoiling by using an organic solvent: soaking the workpiece in petroleum ether to remove greasy dirt on the surface;
3. and (3) drying: drying the workpiece treated in the step 2 by compressed air to dry redundant solvent gasoline;
4. chemical degreasing: immersing the dried workpiece treated by the step 3 in the heated solution; simultaneously turning on ultrasonic waves, and then carrying out overflow double-water washing, wherein the temperature is 60 ℃ and the time is 5min;
5. cathode electrolysis degreasing: immersing the dried workpiece treated in the step 4 in a cathode electrolysis oil removing groove which is heated to carry out oil removal treatment, and then carrying out overflow double water washing; the temperature was 55℃and the residence time in the solution was 55s, the cathodic current density was 3A/dm 2 ；
6. Acid washing: placing the workpiece treated by the method 5 into a hydrochloric acid solution containing 37wt% of HCl, and then carrying out overflow double-water washing; the temperature is normal temperature, and the residence time in the solution is 30min;
7. ultrasonic cleaning: placing the workpiece treated by the step 6 into an ultrasonic cleaner for ultrasonic cleaning, wherein the blind hole workpiece needs to be turned over during cleaning, so that all blind holes are guaranteed to be provided with an opportunity to face upwards;
8. activating: and (3) placing the workpiece treated by the step (7) in an activation tank, completely immersing the workpiece in an activation solution, and then performing overflow double-water washing. The activation formula is in a dilute sulfuric acid solution with 15+/-5%, the activation temperature is room temperature, and the activation time is 35s;
9. impact nickel: putting the workpiece treated by the step 8 into a nickel impact groove for nickel impact, and then carrying out overflow double-water washing; the formulation of the impact nickel solution is as follows: 200g/L nickel chloride, 250ml/L hydrochloric acid, current density 10A/dm 2 The time is 30s;
10. activating: placing the workpiece treated by the step 9 into an activation tank, completely immersing the workpiece into an activation solution, and then performing overflow double-water washing; the activation formula is in a dilute sulfuric acid solution with 15wt%, the activation temperature is room temperature, and the activation time is 35s;
11. electroplating dark nickel: placing the workpiece treated by the method 10 into an electroplating dark nickel tank for electroplating dark nickel, and then carrying out overflow double-water washing; the formula of the electroplating dark nickel solution comprises: nickel sulfate: 320 g/L, nickel chloride: 45 g/L, boric acid: 45 g/L, cathode current density: 1A/dm 2 Temperature: 50 ℃, pH4.0, time 600s;
12. electroplating bright nickel: placing the workpiece treated by the step 11 into an electroplating dark and bright groove for electroplating bright nickel, and then carrying out overflow double-water washing; the formula of the electroplating bright nickel solution comprises: nickel sulfate: 3260 g/L, nickel chloride: 35 g/L, boric acid: 35 g/L, cathode current density: 2A/dm 2 Temperature: 50 ℃, pH 4.0; time 600s;
13. activating: placing the workpiece treated by the step 12 into an activation tank, completely immersing the workpiece into an activation solution, and then performing overflow double-water washing; the activation formula is in a dilute sulfuric acid solution with 15wt%, the activation temperature is room temperature, and the activation time is 35s;
4. preplating: putting the workpiece treated by the step 13 into a preplating groove for preplating, and then carrying out overflow double-water washing; the formula of the preplating solution is as follows: potassium aurous cyanide: 0.8 g/L, pH5.6, specific gravity 1.12g/cm 3 Cathode current density at 50 ℃): 0.2 A/dm 30s;
15. gold plating: putting the workpiece treated by the step 14 into a gold plating tank for gold plating, and then carrying out overflow double-water washing; the formula of the gold plating solution is as follows: gold potassium cyanide 5.4 g/L, pH5.6, specific gravity 1.12g/cm, temperature 50 ℃, cathodic current density 0.3A/dm, time 450s;
16. ultrasonic hot pure water cleaning: placing the 15-treated workpiece into ultrasonic waves, and cleaning the part by using hot pure water at 70 ℃ for 35 times;
17. and (3) drying: and (3) putting the workpiece subjected to the treatment of 16 into an oven for drying, wherein the temperature is 85 ℃.
The coating of the embodiment can meet the requirement of baking at 300 ℃ for 15 minutes; the temperature impact test at the temperature of-55 ℃ to 125 ℃ can be satisfied, the temperature is kept for 0.3h at the limit temperature, the cycle times are 5 times, and the conversion time is 5 minutes; the method can meet the moisture resistance test of the method 106 in the GJB360B-2009, and can meet the soldering heat resistance test of the method 210 in the GJB360B-2009, and the laser sealing welding is not foamed and does not generate cracks.
Example 2
A method for plating Ni5Au0.5 on a kovar alloy small cavity of a filter of a certain model comprises the following steps:
1. hanging: fixing the workpiece on the hanger according to the requirement of hanging the operation instruction, wherein the fixing mode is strictly according to the operation instruction;
2. deoiling by using an organic solvent: soaking the workpiece in petroleum ether to remove greasy dirt on the surface;
3. and (3) drying: drying the workpiece treated in the step 2 by compressed air to dry redundant solvent gasoline;
4. chemical degreasing: immersing the dried workpiece treated by the step 3 in the heated solution; simultaneously turning on ultrasonic waves, and then carrying out overflow double-water washing, wherein the temperature is 80 ℃ and the time is 10min;
5. cathode electrolysis degreasing: immersing the dried workpiece treated in the step 4 in a cathode electrolysis oil removing groove which is heated to carry out oil removal treatment, and then carrying out overflow double water washing; the temperature was 65℃and the residence time in the solution was 65s, the cathodic current density was 3A/dm 2 ；
6. Acid washing: placing the workpiece subjected to the treatment 5 into a hydrochloric acid solution containing 37wt% of HCl, and then performing overflow double-water washing, wherein the temperature is normal temperature, and the residence time in the solution is 60min;
7. ultrasonic cleaning: placing the workpiece treated by the step 6 into an ultrasonic cleaner for ultrasonic cleaning, wherein the blind hole workpiece needs to be turned over during cleaning, so that all blind holes are guaranteed to be provided with an opportunity to face upwards;
8. activating: placing the workpiece treated by the step 7 into an activation tank, completely immersing the workpiece into an activation solution, and then performing overflow double-water washing; the activation formula is in a dilute sulfuric acid solution with 15wt%, the activation temperature is room temperature, and the activation time is 55s;
9. impact nickel: putting the workpiece treated by the step 8 into a nickel impact groove for nickel impact, and then carrying out overflow double-water washing; the formulation of the impact nickel solution is as follows: 250g/L Nickel chloride, 300ml/L hydrochloric acid, current density10A/dm 2 The time is 30s;
10. activating: placing the workpiece treated by the step 9 into an activation tank, completely immersing the workpiece into an activation solution, and then performing overflow double-water washing; the activation formula is in a dilute sulfuric acid solution with 15wt%, the activation temperature is room temperature, and the activation time is 55s;
11. electroplating dark nickel: placing the workpiece treated by the method 10 into an electroplating dark nickel tank for electroplating dark nickel, and then carrying out overflow double-water washing; the formula of the electroplating dark nickel solution comprises: nickel sulfate: 380 g/L, nickel chloride: 55g/L, boric acid: 55g/L, cathode current density: 1A/dm 2 Temperature: 60 ℃, pH5.0, time 600s;
12. electroplating bright nickel: placing the workpiece treated by the step 11 into an electroplating dark and bright groove for electroplating bright nickel, and then carrying out overflow double-water washing; the formula of the electroplating bright nickel solution comprises: nickel sulfate: 380 g/L, nickel chloride: 55g/L, boric acid: 55g/L, cathode current density: 2A/dm 2 Temperature: 60 ℃; PH4.5, time 600s;
13. activating: placing the workpiece treated by the step 12 into an activation tank, completely immersing the workpiece into an activation solution, and then performing overflow double-water washing; the activation formula is in a dilute sulfuric acid solution with 15wt%, the activation temperature is room temperature, and the activation time is 55s;
14. preplating: putting the workpiece treated by the step 13 into a preplating groove for preplating, and then carrying out overflow double-water washing; the formula of the preplating solution is as follows: potassium aurous cyanide: 3. 3 g/L, pH6.8, specific gravity 1.12g/cm 3 Cathode current density at 60 ℃): 0.2 A/dm, time 30s;
15. gold plating: and (3) putting the workpiece treated by the step (14) into a gold plating tank for gold plating, and then carrying out overflow double-water washing. The formula of the gold plating solution is as follows: 12. 12 g/L potassium aurous cyanide, pH6.8, specific gravity 1.12g/cm, temperature 60 ℃, cathodic current density 0.3A/dm, time 230s;
16. ultrasonic hot pure water cleaning: placing the 15-treated workpiece into ultrasonic waves, and cleaning the workpiece with hot pure water at 70 ℃ for 35 seconds;
17. and (3) drying: and (3) putting the workpiece subjected to the treatment of 16 into an oven for drying, wherein the temperature is 85 ℃.
The coating of the embodiment can meet the requirement of baking at 300 ℃ for 10 minutes; the temperature impact test at the temperature of-55 ℃ to 125 ℃ can be satisfied, the temperature is kept for 0.3h at the limit temperature, the cycle times are 5 times, and the conversion time is 5 minutes; the method can meet the moisture resistance test of the method 106 in the GJB360B-2009, and can meet the soldering heat resistance test of the method 210 in the GJB360B-2009, and the laser sealing welding is not foamed and does not generate cracks.
Example 3
A method for plating Ni2Au1.5 on a kovar alloy cover plate of a certain model comprises the following steps:
1. hanging: fixing the workpiece on the hanger according to the requirement of hanging the operation instruction, wherein the fixing mode is strictly according to the operation instruction;
2. deoiling by using an organic solvent: soaking the workpiece in petroleum ether to remove greasy dirt on the surface;
3. and (3) drying: drying the workpiece treated in the step 2 by compressed air to dry redundant solvent gasoline;
4. chemical degreasing: immersing the dried workpiece treated by the step 3 in the heated solution; simultaneously turning on ultrasonic waves, and then carrying out overflow double-water washing, wherein the temperature is 70 ℃ and the time is 7min;
5. cathode electrolysis degreasing: immersing the dried workpiece treated in the step 4 in a cathode electrolysis oil removing groove which is heated to carry out oil removal treatment, and then carrying out overflow double water washing; the temperature was 60℃and the residence time in the solution was 60s, the cathodic current density was 3A/dm 2 ；
6. Acid washing: placing the workpiece treated by the method 5 into a hydrochloric acid solution containing 37wt% of HCl, and then carrying out overflow double-water washing; the temperature is normal temperature, and the residence time in the solution is 50min;
7. ultrasonic cleaning: placing the workpiece treated by the step 6 into an ultrasonic cleaner for ultrasonic cleaning, wherein the blind hole workpiece needs to be turned over during cleaning, so that all blind holes are guaranteed to be provided with an opportunity to face upwards;
8. activating: placing the workpiece treated by the step 7 into an activation tank, completely immersing the workpiece into an activation solution, and then performing overflow double-water washing; the activation formula is in a dilute sulfuric acid solution with 15wt%, the activation temperature is room temperature, and the activation time is 45s;
9. impact nickel: putting the workpiece treated by the step 8 into a nickel impact groove for nickel impact, and then performing overflow double-water washingThe method comprises the steps of carrying out a first treatment on the surface of the The formulation of the impact nickel solution is as follows: 220g/L nickel chloride, 280ml/L hydrochloric acid, current density 10A/dm 2 The time is 30s;
10. activating: placing the workpiece treated by the step 9 into an activation tank, completely immersing the workpiece into an activation solution, and then performing overflow double-water washing; the activation formula is in a dilute sulfuric acid solution with 15wt%, the activation temperature is room temperature, and the activation time is 45s;
11. electroplating dark nickel: placing the workpiece treated by the method 10 into an electroplating dark nickel tank for electroplating dark nickel, and then carrying out overflow double-water washing; the formula of the electroplating dark nickel solution comprises: nickel sulfate: 320 g/L, nickel chloride: 45 g/L, boric acid: 45 g/L, cathode current density: 1A/dm 2 Temperature: 55 ℃, pH4.5, time 300s;
12. electroplating bright nickel: placing the workpiece treated by the step 11 into an electroplating dark and bright groove for electroplating bright nickel, and then carrying out overflow double-water washing; the formula of the electroplating bright nickel solution comprises: nickel sulfate: 320 g/L, nickel chloride: 45 g/L, boric acid: 45 g/L, cathode current density: 2A/dm 2 Temperature: 55 ℃, pH 4.5; time 300s;
13. activating: placing the workpiece treated by the step 12 into an activation tank, completely immersing the workpiece into an activation solution, and then performing overflow double-water washing; the activation formula is in a dilute sulfuric acid solution with 15wt%, the activation temperature is room temperature, and the activation time is 45s;
14. preplating: putting the workpiece treated by the step 13 into a preplating groove for preplating, and then carrying out overflow double-water washing; the formula of the preplating solution is as follows: potassium aurous cyanide: 1.9 g/L, pH 6.2, specific gravity 1.16. 1.16g/cm 3 Cathode current density at 55 deg.c: 0.2 A/dm, time 30s;
15. gold plating: putting the workpiece treated by the step 14 into a gold plating tank for gold plating, and then carrying out overflow double-water washing; the formula of the gold plating solution is as follows: gold potassium cyanide 8.2 g/L, pH 6.2, specific gravity 1.16g/cm, temperature 55 ℃, cathodic current density 0.3A/dm, time 900s;
16. ultrasonic hot pure water cleaning: placing the 15-treated workpiece into ultrasonic waves, and cleaning the workpiece with hot pure water at 70 ℃ for 35 seconds;
17. and (3) drying: and (3) putting the workpiece subjected to the treatment of 16 into an oven for drying, wherein the temperature is 85 ℃.
The coating of the embodiment can meet the requirement of baking for 20 minutes at 300 ℃; the temperature impact test at the temperature of-55 ℃ to 125 ℃ can be satisfied, the temperature is kept for 0.3h at the limit temperature, the cycle times are 5 times, and the conversion time is 5 minutes; the method can meet the moisture resistance test of the method 106 in the GJB360B-2009, and can meet the soldering heat resistance test of the method 210 in the GJB360B-2009, and the laser sealing welding is not foamed and does not generate cracks.
Comparative 1
This comparative example was compared to example 3, and only the step "9, impact nickel" was omitted, and the remainder was identical to example 3,
as a result, the plated article obtained was foamed without being subjected to high temperature, and thus, the subsequent experiments were not conducted. The nickel strike step proves to be very important.
Comparative example 2
In this comparative example, the residence time of only the step "6 and the acid washing" was 5 minutes as compared with example 3, and the rest was the same as example 3,
the resulting plated article was pickled for 5 minutes according to the ordinary metal article, and baked at 300℃for 10 minutes to foam, which proves that the pickling time was very important.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (8)
1. A method for electroplating nickel-gold on kovar alloy, which is characterized by comprising the following steps: hanging, degreasing by an organic solvent, chemical degreasing, cathodic electrolysis degreasing, pickling, activating, nickel impacting, activating, nickel electroplating, activating and gold electroplating, and the specific steps are as follows:
(1) Hanging: hanging a workpiece to be treated;
(2) Deoiling by using an organic solvent: soaking a workpiece in an organic solvent to remove greasy dirt on the surface, and then drying to remove the organic solvent on the surface;
(3) Chemical degreasing: immersing the dried workpiece treated in the step (2) in the heated solution; simultaneously turning on ultrasonic waves, and then carrying out overflow double-water washing, wherein the temperature is 60-80 ℃ and the time is 5-10min;
(4) Cathode electrolysis degreasing: immersing the dried workpiece treated in the step (3) in a heated cathode electrolytic oil removing groove for oil removal treatment, and then carrying out overflow double water washing; the temperature is 55-65deg.C, the residence time in the solution is 55-65s, and the cathode current density is 2.5-3.5A/dm 2 ；
(5) Acid washing: placing the workpiece treated in the step (4) in an acid solution, and then carrying out overflow double-water washing; the temperature is normal temperature, and the residence time in the solution is 30-60min; then ultrasonic cleaning is carried out;
(6) Activating: placing the workpiece treated in the step (5) into an activation tank, completely immersing the workpiece into an activation solution, and then performing overflow double-water washing; the activation temperature is room temperature, and the activation time is 35-55S;
(7) Impact nickel: placing the workpiece treated in the step (6) into a nickel impact groove for nickel impact, and then carrying out overflow double-water washing; the formulation of the impact nickel solution is as follows: 200-250g/L nickel chloride, 250-300ml/L hydrochloric acid, current density 9-11A/dm 2 The time is 30-60S;
(8) Activating: placing the workpiece treated in the step (7) into an activation tank, completely immersing the workpiece into an activation solution, and then performing overflow double-water washing; the activation temperature is room temperature, and the activation time is 35-55S;
(9) Electroplating dark nickel: placing the workpiece treated in the step (8) into an electroplating dark nickel groove for electroplating dark nickel, and then carrying out overflow double-water washing; cathode current density: 0.5-1.5A/dm 2 Temperature: 50-60 ℃ and pH 4-5;
(10) Electroplating bright nickel: placing the workpiece treated in the step (9) into an electroplating dark and bright groove for electroplating bright nickel, and then carrying out overflow double-water washing; cathode current density: 1-3A/dm 2 Temperature: 50-60 ℃ and pH 4-5;
(11) Activating: placing the workpiece treated in the step (10) into an activation tank, completely immersing the workpiece into an activation solution, and then performing overflow double-water washing; the activation temperature is room temperature, and the activation time is 35-55S;
(12) Preplating: placing the workpiece treated in the step (11) into a preplating groove for preplating, and then carrying out overflow double-water washing; the pH of the preplating solution is 5.6-6.8, the specific gravity is 1.12-1.20g/cm, the temperature is 50-60 ℃, and the cathode current density is as follows: 0.1-0.3A/dm;
(13) Gold plating: and (3) putting the workpiece treated in the step (12) into a gold plating tank for gold plating, and then carrying out overflow double-water washing. The pH of the gold plating solution is 5.6-6.8, the specific gravity is 1.12-1.20g/cm, the temperature is 50-60 ℃, and the cathode current density is 0.2-0.4A/dm;
(14) Ultrasonic hot pure water cleaning: putting the workpiece treated in the step (13) into ultrasonic waves for cleaning;
(15) And (3) drying: and (5) putting the workpiece treated in the step (14) into an oven for drying.
2. The method for plating nickel-gold on kovar alloy according to claim 1, wherein: in the step (2), the organic solvent is petroleum ether.
3. The method for plating nickel-gold on kovar alloy according to claim 1, wherein: in the step (3), the solution is 50g/L deoiling powder solution.
4. The method for plating nickel-gold on kovar alloy according to claim 1, wherein: in step (5), the acid solution was 37wt% hcl.
5. The method for plating nickel-gold on kovar alloy according to claim 1, wherein: in the step (6), the step (8) and the step (11), the formula of the activating solution is 10-20wt% of dilute sulfuric acid solution.
6. The method for plating nickel-gold on kovar alloy according to claim 1, wherein: in the step (9) and the step (10), the formulas of the electroplating dark nickel solution and the electroplating bright nickel solution are as follows: nickel sulfate: 260-380 g/L, nickel chloride: 35-55 g/L, boric acid: 35-55 g/L.
7. The method for plating nickel-gold on kovar alloy according to claim 1, wherein: in the step (12), the formula of the pre-gold plating solution is as follows: potassium aurous cyanide: 0.8-3.0 g/L.
8. The method for plating nickel-gold on kovar alloy according to claim 1, wherein: in the step (13), the formula of the gold plating solution is as follows: 4.4-12 g/L of potassium aurous cyanide.
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