CN113337817A - Electroplating process of copper diamond - Google Patents
Electroplating process of copper diamond Download PDFInfo
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- CN113337817A CN113337817A CN202110619209.6A CN202110619209A CN113337817A CN 113337817 A CN113337817 A CN 113337817A CN 202110619209 A CN202110619209 A CN 202110619209A CN 113337817 A CN113337817 A CN 113337817A
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 54
- 239000010432 diamond Substances 0.000 title claims abstract description 54
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 51
- 239000010949 copper Substances 0.000 title claims abstract description 51
- 238000009713 electroplating Methods 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 28
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 126
- 239000000126 substance Substances 0.000 claims abstract description 79
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 76
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 63
- 238000007747 plating Methods 0.000 claims abstract description 51
- 239000010931 gold Substances 0.000 claims abstract description 49
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229910052737 gold Inorganic materials 0.000 claims abstract description 43
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 38
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000005238 degreasing Methods 0.000 claims abstract description 25
- 239000002253 acid Substances 0.000 claims abstract description 23
- 230000002378 acidificating effect Effects 0.000 claims abstract description 17
- 230000004913 activation Effects 0.000 claims abstract description 14
- 238000005530 etching Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 69
- 239000002904 solvent Substances 0.000 claims description 30
- 238000002791 soaking Methods 0.000 claims description 26
- 230000003213 activating effect Effects 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000003381 stabilizer Substances 0.000 claims description 14
- 238000004140 cleaning Methods 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 7
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 5
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 5
- 239000001119 stannous chloride Substances 0.000 claims description 5
- 235000011150 stannous chloride Nutrition 0.000 claims description 5
- 238000007664 blowing Methods 0.000 claims description 3
- 239000012190 activator Substances 0.000 claims 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 claims 1
- 230000008021 deposition Effects 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 238000005728 strengthening Methods 0.000 abstract description 2
- 238000004381 surface treatment Methods 0.000 description 12
- 239000003921 oil Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- 108091008716 AR-B Proteins 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- XTFKWYDMKGAZKK-UHFFFAOYSA-N potassium;gold(1+);dicyanide Chemical compound [K+].[Au+].N#[C-].N#[C-] XTFKWYDMKGAZKK-UHFFFAOYSA-N 0.000 description 3
- 241000208125 Nicotiana Species 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004100 electronic packaging Methods 0.000 description 2
- IZLAVFWQHMDDGK-UHFFFAOYSA-N gold(1+);cyanide Chemical compound [Au+].N#[C-] IZLAVFWQHMDDGK-UHFFFAOYSA-N 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000005022 packaging material Substances 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 230000037452 priming Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 235000010724 Wisteria floribunda Nutrition 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 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
- -1 aluminum silicon carbon Chemical compound 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- WUUZKBJEUBFVMV-UHFFFAOYSA-N copper molybdenum Chemical compound [Cu].[Mo] WUUZKBJEUBFVMV-UHFFFAOYSA-N 0.000 description 1
- SBYXRAKIOMOBFF-UHFFFAOYSA-N copper tungsten Chemical compound [Cu].[W] SBYXRAKIOMOBFF-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
- C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1646—Characteristics of the product obtained
- C23C18/165—Multilayered product
- C23C18/1653—Two or more layers with at least one layer obtained by electroless plating and one layer obtained by electroplating
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1837—Multistep pretreatment
- C23C18/1844—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
-
- 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
- C25D3/48—Electroplating: Baths therefor from solutions of gold
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Electrochemistry (AREA)
- Inorganic Chemistry (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The invention discloses an electroplating process of copper diamond, which comprises the following steps: ultrasonic chemical degreasing, micro-etching, hydrochloric acid activation, colloidal palladium activation, dispergation, alkaline chemical nickel plating, acidic chemical nickel plating and soft gold electroplating. The invention removes oil stain and oxide skin on the surface of copper diamond by ultrasonic degreasing and micro-etching, further coarsens the surface of diamond by acid activation to facilitate the deposition of colloidal palladium and the strengthening of the binding force of a plating layer, improves the catalytic activity of the colloidal palladium on the surface of copper diamond by peptizing treatment, facilitates the direct chemical reaction in alkaline chemical nickel solution, accelerates the deposition speed of chemical plating, plates an alkaline chemical nickel layer on the whole surface, plays a role in bottoming, plates to the required thickness of the nickel layer in acidic chemical nickel solution, and plates soft gold finally. The invention can form an electroplated layer with uniform plating, excellent binding force and good appearance quality on the surface of the copper diamond, and has the advantages of simple process, uniform plating and the like.
Description
Technical Field
The invention belongs to the technical field of electroplating processes, and particularly relates to an electroplating process for copper diamond.
Background
The commonly used electronic packaging material is a single metal material such as copper, aluminum and silver, and a composite material such as copper tungsten, copper molybdenum, aluminum silicon and aluminum silicon carbon, and as a novel composite material, copper diamond has the remarkable advantages of incomparable high heat-conducting property and low thermal expansion coefficient, and has a very wide application prospect in the fields of semiconductor lasers and electronic packaging. The copper diamond is prepared by doping a large amount of micro diamond particles with copper as a matrix, and in order to meet the bonding requirement of high quality and high reliability during packaging, the surface of the copper diamond needs to be subjected to metallization treatment or electroplating treatment. The difficult point of the copper diamond electroplating process lies in how to manufacture a coating film layer with excellent bonding force with the copper diamond substrate due to poor wettability of the diamond substrate and a metal material, so that the wettability requirement of a bonding process can be met, the requirement of no peeling and bubbling at high temperature can be met, and the reliability requirement after bonding and in use can be met.
Because the physical and chemical properties of the two components of the copper diamond are greatly different, the copper is easy to react with acid and alkali, and the physical and chemical inertness of the diamond is extremely high, the two materials cannot be effectively and safely modified simultaneously by common electroplating pretreatment. The quality problem of plating binding force can be caused by insufficient pretreatment, and the surface roughness of copper diamond can be caused by excessive pretreatment, so that the requirements of the uniformity and the packaging flatness of a plating film layer are influenced. At present, the invention discloses a surface gold plating method of a diamond copper composite material, the patent number is CN201410407949.3, the invention adopts a vacuum and high-temperature annealing method to enhance the binding force of an electroplated nickel layer and a copper diamond matrix, but the method is not easy to realize in the actual electroplating industry, so that an electroplating process which is suitable for industrial production, easy to operate, capable of ensuring the binding force quality of a plating layer and stable in production needs to be developed, and the problem that the popularization and application of the copper diamond as a novel packaging material are urgently needed to be solved.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the prior art and provide the electroplating process of the copper diamond, which has the advantages of simple process, suitability for industrial production and production line control, uniform plating layer, excellent binding force and good bonding performance and meets the use requirement of gold-tin bonding.
The electroplating process of the electroplated copper diamond provided by the invention comprises the following steps:
s1: ultrasonic chemical oil removal: putting the copper diamond into a chemical degreasing solution with an ultrasonic field for degreasing, wherein the degreasing solution is at the temperature of 50-70 ℃, the soaking time is 10-15 minutes, and taking out the copper diamond and cleaning the copper diamond by using pure water for electroplating;
s2: micro-etching: putting the plated part finished in the step S1 into a microetching solution, wherein the temperature of the microetching solution is 20-30 ℃, the soaking time is 50-70 seconds, and taking out the plated part to be cleaned by pure water;
s3: activating with hydrochloric acid: soaking and activating the plated part finished in the step S2 in a 20% hydrochloric acid solution for 50-70 seconds, and taking out the plated part and cleaning the plated part with pure water;
s4: activation of colloidal palladium: activating the plated part finished in the step S3 in a colloidal palladium solution, wherein the temperature of the colloidal palladium solution is 30-35 ℃, the soaking time is 3-5 minutes, a colloidal palladium layer is formed on the outer surface of the plated part, and the plated part is taken out and cleaned with pure water;
s5: and (3) gel releasing: putting the plated piece finished in the step S4 into 10g/L sodium hydroxide solution for degumming, soaking for 5-10 seconds, removing stannous chloride wrapping palladium gold, taking out the plated piece, and cleaning with pure water;
s6: alkaline chemical nickel plating: putting the plated part obtained in the step S5 into an alkaline chemical nickel solution for plating, wherein the pH value of the alkaline chemical nickel solution is 9.6-11.5, the temperature is 35-40 ℃, the alkaline chemical nickel layer with the thickness of 0.5-1 micron is formed after the plating time is 3-5 minutes, and the plated part is taken out and cleaned with pure water;
s7: acid chemical nickel plating: putting the plated piece finished in the step S6 into an acidic chemical nickel solution, wherein the pH value of the acidic chemical nickel solution is 4.5-5.5, the temperature is 60-80 ℃, the plating time is 20-30 minutes, then an acidic chemical nickel layer with the thickness of 2.5-4.0 microns is formed, and the plated piece is taken out and cleaned with pure water;
s8: electroplating soft gold: and (5) putting the plated part obtained in the step (S7) into a soft gold solution for plating, wherein the temperature of the soft gold solution is 55-65 ℃, the pH value is 4.5-5.0, the current density is 0.1-0.5A/dm 2, a soft gold layer with the thickness of 0.3-1 micrometer is formed after electroplating for 8-18 minutes, and the plated part is taken out after electroplating, cleaned by pure water, dried by blowing and dried after surface moisture is dried.
The chemical oil removing solution of the invention is as follows: 40-60 g/L of C02 deoiling powder, and pure water as a solvent.
The microetching solution of the invention comprises: microetching powder-MEOX 100-130 g/L, AR sulfuric acid 10-40 ml/L, and pure water as solvent.
The colloidal palladium solution of the invention is: 8-10 ml/L, HN-200B of HN-200A colloidal palladium activator, 50-60 ml/L, AR ml/310 ml/L of hydrochloric acid and a solvent of pure water.
The alkaline chemical nickel solution of the invention is: AL-8100A175ml/L, AL-8100C60ml/L, 8100 stabilizer 60ml/L, and solvent is pure water.
The acidic chemical nickel solution of the invention is: HN-310A60ml/L, HN-310B150ml/L and the solvent is pure water.
The soft gold plating solution is a weak acid soft gold electroplating solution, and the weak acid soft gold electroplating solution comprises the following components in parts by weight: 100g/L of Au-MakeUp salt, 3.7-4.4 g/L, Au g/4.4 g/L, Au-potassium aurum cyanide-MLA acid 30g/L, Au-Grainrefiner8.4ml/L and pure water as solvent
The invention has the beneficial effects that:
(1) the invention removes oil stain and oxide skin on the surface of copper diamond by ultrasonic degreasing and micro-etching, further coarsens the surface of diamond by acid activation to facilitate the deposition of colloidal palladium and the strengthening of the binding force of a plating layer, improves the catalytic activity of colloidal palladium on the surface of copper diamond by peptizing treatment, facilitates the direct chemical reaction in alkaline chemical nickel solution, accelerates the deposition speed of chemical plating, plates an alkaline chemical nickel layer on the whole surface, plays a role in priming, plates to the required nickel layer thickness in acidic chemical nickel solution, and plates soft gold finally.
(2) The invention does not need to carry out vacuum heat treatment on the interface of the plating layer, forms the required thickness of the nickel layer and the required thickness of the gold layer on the surface of the copper diamond, has good bonding force and apparent quality, has the surface roughness Ra of the plated copper diamond less than 0.4 micron, has good wetting property, does not bubble at the high temperature of 350 ℃, does not peel, and meets the requirement of eutectic bonding with gold and tin.
(3) The invention is suitable for industrialized mass production, and has the advantages of simple process, easy operation and production line control, uniform plating layer, excellent binding force and bonding performance, and can meet the use requirement of gold-tin bonding.
Drawings
FIG. 1 is a process flow diagram of one embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
As shown in fig. 1, the electroplating process of copper diamond of the present embodiment includes the following steps:
s1: ultrasonic chemical oil removal: putting the copper diamond into a chemical degreasing solution with an ultrasonic field for degreasing, wherein the chemical degreasing solution is as follows: 50g/L of CO2 degreasing powder and pure water as a solvent, wherein the CO2 degreasing powder is provided by Kai Si surface treatment materials Co., Ltd, the temperature of a degreasing solution is 60 ℃, the soaking time is 12 minutes, the copper diamond is taken out and cleaned by the pure water, and oil stains and oxide skins on the surface of the copper diamond are removed by ultrasonic degreasing in the step;
s2: micro-etching: putting the plated part finished in the step S1 into a microetching solution, wherein the microetching solution is as follows: 30ml/L sulfuric acid of micro-etching agent-MEOX 120ml/L, AR, solvent are pure water, the micro-etching agent-MEOX is provided by Kai surface treatment material Co., Ltd, the temperature of micro-etching solution is 25 ℃, the soaking time is 60 seconds, the plated part is taken out and cleaned by pure water, and the oil stain and the oxide skin on the surface of the copper diamond are further removed by micro-etching in the step;
s3: activating with hydrochloric acid: the plated part finished in the step S2 is put into a hydrochloric acid solution with the concentration of 20% for soaking and activation, the soaking time is 60 seconds, the plated part is taken out and cleaned by pure water, and the surface of the diamond is further roughened through acid activation in the step so as to be beneficial to the deposition of colloidal palladium and the enhancement of the bonding force of a plating layer;
s4: activation of colloidal palladium: and (4) putting the plated part finished in the step (S3) into a colloidal palladium solution for activation, wherein the colloidal palladium solution is as follows: 9ml/L, HN-200B of HN-200A activating agent, 55ml/L, AR B of stabilizing agent, 290ml/L of hydrochloric acid and pure water as solvent, wherein the HN-200A activating agent and the HN-200B stabilizing agent are provided by Kai surface treatment materials, Inc. of Huizhou city, the temperature of a colloidal palladium solution is 33 ℃, the soaking time is 4 minutes, a colloidal palladium layer is formed on the outer surface of a plated part, and the plated part is taken out and cleaned by the pure water;
s5: and (3) gel releasing: putting the plated piece finished in the step S4 into 10g/L sodium hydroxide solution for dispergation, wherein the soaking time is 8 seconds, removing stannous chloride on a colloidal palladium layer wrapped by the plated piece, taking out the plated piece, and cleaning the plated piece with pure water;
s6: alkaline chemical nickel plating: and (4) putting the plated part finished in the step S5 into an alkaline chemical nickel solution for plating, wherein the alkaline chemical nickel solution is as follows: Al-8100A175ml/L, AL-8100C60ml/L, 8100 stabilizer 60ml/L, solvent is pure water, AL-8100A, AL-8100C, 8100 stabilizer are offered by Juzhen's Hongshiku technology development Limited company, pH value of alkaline chemical nickel solution is 10.5, the temperature is 37 ℃, the alkaline chemical nickel layer with thickness of 0.8 micron is formed after plating time is 4 minutes, the pure water is cleaned after being taken out, the step plates the alkaline chemical nickel layer on the whole plated part surface, the plating layer plays a role of priming;
s7: acid chemical nickel plating: putting the plated part finished in the step S6 into an acidic chemical nickel solution, wherein the acidic chemical nickel solution is as follows: HN-310A60ml/L, HN-310B150ml/L and pure water as solvent, HN-310A, HN-310B provided by Kaiki surface treatment materials, Inc., Huizhou, the pH value of the acid chemical nickel solution is 5, the temperature is 70 ℃, after 25 minutes of plating time, an acid chemical nickel layer with the thickness of 3 microns is formed, and the pure water is cleaned after being taken out;
s8: electroplating soft gold: putting the plated part finished in the step S7 into a soft gold groove solution for plating, wherein the soft gold groove solution is as follows: the method comprises the steps of providing 100g/L of Au-MakeUp salt, 4g/L, Au-30 g/L, Au-Grainrefiner8.4ml/L of potassium aurous cyanide, 8.4ml/L of Grainrefiner and pure water as a solvent, providing the Au-MakeUp salt, the Au-MLA acid and the Au-Grainrefiner by Japan rural area companies, providing the potassium aurous cyanide by Fujie noble metal Co., Ltd of tobacco terrace, providing a soft gold solution with the gold concentration of 3g/L, the temperature of 60 ℃, the pH value of 4.8 and the current density of 0.3A/dm2, forming a soft gold layer with the thickness of 0.8 micron after electroplating for 15 minutes, taking out a plated part after electroplating, cleaning the plated part by using the pure water, drying after drying the surface water by blowing, and forming a plated layer with uniform plating, excellent binding force and good appearance quality on the surface of the copper diamond.
Example 2
The electroplating process of the copper diamond of the embodiment comprises the following steps:
s1: ultrasonic chemical oil removal: putting the copper diamond into a chemical degreasing solution with an ultrasonic field for degreasing, wherein the chemical degreasing solution is as follows: 40g/L of CO2 degreasing powder and pure water as a solvent, wherein the CO2 degreasing powder is provided by Kai surface treatment materials Co., Ltd, the temperature of a degreasing solution is 50 ℃, the soaking time is 10 minutes, and the copper diamond is taken out and cleaned by the pure water;
s2: micro-etching: putting the plated part finished in the step S1 into a microetching solution, wherein the microetching solution is as follows: the microetching solution-MEOX 100ml/L, AR sulfuric acid 10ml/L and the solvent are pure water, the microetching solution-MEOX is provided by Kai surface treatment material Co., Ltd, the temperature of the microetching solution is 20 ℃, the soaking time is 50 seconds, and the plated part is taken out and cleaned by the pure water;
s3: activating with hydrochloric acid: soaking and activating the plated part finished in the step S2 in a hydrochloric acid solution for 50 seconds, and taking out the plated part and cleaning the plated part with pure water;
s4: activation of colloidal palladium: and (4) putting the plated part finished in the step (S3) into a colloidal palladium solution for activation, wherein the colloidal palladium solution is as follows: 8ml/L, HN-200B of HN-200A activating agent, 270ml/L of L, AR B of stabilizing agent, 50ml/L, AR of hydrochloric acid and pure water as solvent, wherein the HN-200A activating agent and the HN-200B stabilizing agent are provided by Kai surface treatment materials, Inc., of Huizhou city, the temperature of a colloidal palladium solution is 30 ℃, the soaking time is 3 minutes, a colloidal palladium layer is formed on the outer surface of a plated piece, and the plated piece is taken out and cleaned by the pure water;
s5: and (3) gel releasing: putting the plated piece finished in the step S4 into 10g/L sodium hydroxide solution for degumming, soaking for 5 seconds, removing stannous chloride of a colloidal palladium layer wrapped by the plated piece, taking out the plated piece, and cleaning with pure water;
s6: alkaline chemical nickel plating: and (4) putting the plated part finished in the step S5 into an alkaline chemical nickel solution for plating, wherein the alkaline chemical nickel solution is as follows: Al-8100A175ml/L, AL-8100C60ml/L, 8100 stabilizer 60ml/L, solvent is pure water, Al-8100A, AL-8100C, 8100 stabilizer are provided by Juzhen, Macrocisco technology development Limited company, pH value of alkaline chemical nickel solution is 9.6, temperature is 35 ℃, alkaline chemical nickel layer with thickness of 0.5 micron is formed after plating time is 3 minutes, and pure water is cleaned after being taken out;
s7: acid chemical nickel plating: putting the plated part finished in the step S6 into an acidic chemical nickel solution, wherein the acidic chemical nickel solution is as follows: HN-310A60ml/L, HN-310B150ml/L and pure water as solvent, HN-310A, HN-310B provided by Kaiki surface treatment materials, Inc., Huizhou, the pH value of the acid chemical nickel solution is 4.5, the temperature is 60 ℃, an acid chemical nickel layer with the thickness of 2.5 micrometers is formed after 20 minutes of plating time, and the pure water is cleaned after being taken out;
s8: electroplating soft gold: putting the plated part finished in the step S7 into a soft gold groove solution for plating, wherein the soft gold groove solution is as follows: the gold plating solution is prepared from 100g/L of Au-MakeUp salt, 3.7g/L, Au g-30 g/L, Au g-8.4 ml/L of potassium aurocyanide, pure water as a solvent, 2.7g/L of gold concentration of the soft gold solution, 55 ℃ of pH value of 4.5 and 0.1A/dm2 by Japan rural area, and the soft gold layer with thickness of 0.3 micron is formed after electroplating for 8 minutes, and the plated part is taken out after electroplating, cleaned by pure water, dried and dried after surface moisture drying.
Example 3
The electroplating process of the copper diamond of the embodiment comprises the following steps:
s1: ultrasonic chemical oil removal: putting the copper diamond into a chemical degreasing solution with an ultrasonic field for degreasing, wherein the chemical degreasing solution is as follows: 60g/L of CO2 deoiling powder and pure water as a solvent, wherein the CO2 deoiling powder is provided by Sikha surface treatment material Co., Ltd, the temperature of the deoiling solution is 70 ℃, the soaking time is 15 minutes, and the copper diamond is taken out and cleaned by the pure water;
s2: micro-etching: putting the plated part finished in the step S1 into a microetching solution, wherein the microetching solution is as follows: the microetching solution-MEOX 130ml/L, AR sulfuric acid 40ml/L and the solvent are pure water, the microetching solution-MEOX is provided by Kai surface treatment material Co., Ltd, the temperature of the microetching solution is 30 ℃, the soaking time is 70 seconds, and the plated part is taken out and cleaned by the pure water;
s3: activating with hydrochloric acid: soaking and activating the plated part finished in the step S2 in a hydrochloric acid solution for 70 seconds, and taking out the plated part and cleaning the plated part with pure water;
s4: activation of colloidal palladium: and (4) putting the plated part finished in the step (S3) into a colloidal palladium solution for activation, wherein the colloidal palladium solution is as follows: 10ml/L, HN-200B of HN-200A activating agent, 60ml/L, AR B of stabilizing agent, 310ml/L of hydrochloric acid and pure water as solvent, wherein the HN-200A activating agent and the HN-200B stabilizing agent are provided by Kai surface treatment materials, Inc. of Huizhou city, the temperature of a colloidal palladium solution is 35 ℃, the soaking time is 5 minutes, a colloidal palladium layer is formed on the outer surface of a plated piece, and the plated piece is taken out and cleaned by the pure water;
s5: and (3) gel releasing: putting the plated piece finished in the step S4 into 10g/L sodium hydroxide solution for degumming, wherein the soaking time is 10 seconds, removing stannous chloride of a colloidal palladium layer wrapped by the plated piece, taking out the plated piece, and cleaning the plated piece by using pure water;
s6: alkaline chemical nickel plating: and (4) putting the plated part finished in the step S5 into an alkaline chemical nickel solution for plating, wherein the alkaline chemical nickel solution is as follows: Al-8100A175ml/L, AL-8100C60ml/L, 8100 stabilizer 60ml/L, solvent is pure water, Al-8100A, AL-8100C, 8100 stabilizer are provided by Juzhen, Macrocisco technology development Limited company, pH value of alkaline chemical nickel solution is 11.5, temperature is 40 ℃, alkaline chemical nickel layer with thickness of 1 micron is formed after plating time is 5 minutes, pure water is cleaned after taking out;
s7: acid chemical nickel plating: putting the plated part finished in the step S6 into an acidic chemical nickel solution, wherein the acidic chemical nickel solution is as follows: HN-310A60ml/L, HN-310B150ml/L and pure water as solvent, HN-310A, HN-310B provided by Kaiki surface treatment materials, Inc., Huizhou, the pH value of the acid chemical nickel solution is 5.5, the temperature is 80 ℃, an acid chemical nickel layer with the thickness of 4 micrometers is formed after 30 minutes of plating time, and the pure water is cleaned after being taken out;
s8: electroplating soft gold: putting the plated part finished in the step S7 into a soft gold groove solution for plating, wherein the soft gold groove solution is as follows: the gold plating solution is prepared from 100g/L of Au-MakeUp salt, 4.4g/L, Au g-30 g/L, Au g-4 ml/L of potassium aurocyanide, 8.4ml/L of Grainrefiner and pure water as a solvent, wherein the Au-MakeUp salt, the Au-MLA acid and the Au-Grainrefiner are provided by Japan rural area, the potassium aurocyanide salt is provided by Nicotiana Fuji metal GmbH, the gold concentration of the soft gold bath solution is 2.5g/L, the temperature of the soft gold solution is 65 ℃, the pH value is 5.0, the current density is 0.5A/dm2, a soft gold layer with the thickness of 1 micron is formed after being electroplated for 18 minutes, the plated part is taken out after being electroplated and cleaned, and dried after drying the surface moisture.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention.
Claims (7)
1. The electroplating process of the copper diamond is characterized by comprising the following steps:
s1: ultrasonic chemical oil removal: putting the copper diamond into a chemical degreasing solution with an ultrasonic field for degreasing, wherein the degreasing solution is at the temperature of 50-70 ℃, the soaking time is 10-15 minutes, and taking out the copper diamond and cleaning the copper diamond by using pure water for electroplating;
s2: micro-etching: putting the plated part finished in the step S1 into a microetching solution, wherein the temperature of the microetching solution is 20-30 ℃, the soaking time is 50-70 seconds, and taking out the plated part to be cleaned by pure water;
s3: activating with hydrochloric acid: soaking and activating the plated part finished in the step S2 in a 20% hydrochloric acid solution for 50-70 seconds, and taking out the plated part and cleaning the plated part with pure water;
s4: activation of colloidal palladium: activating the plated part finished in the step S3 in a colloidal palladium solution, wherein the temperature of the colloidal palladium solution is 30-35 ℃, the soaking time is 3-5 minutes, a colloidal palladium layer is formed on the outer surface of the plated part, and the plated part is taken out and cleaned with pure water;
s5: and (3) gel releasing: putting the plated piece finished in the step S4 into 10g/L sodium hydroxide solution for degumming, soaking for 5-10 seconds, removing stannous chloride wrapping palladium gold, taking out the plated piece, and cleaning with pure water;
s6: alkaline chemical nickel plating: putting the plated part obtained in the step S5 into an alkaline chemical nickel solution for plating, wherein the pH value of the alkaline chemical nickel solution is 9.6-11.5, the temperature is 35-40 ℃, the alkaline chemical nickel layer with the thickness of 0.5-1 micron is formed after the plating time is 3-5 minutes, and the plated part is taken out and cleaned with pure water;
s7: acid chemical nickel plating: putting the plated piece finished in the step S6 into an acidic chemical nickel solution, wherein the pH value of the acidic chemical nickel solution is 4.5-5.5, the temperature is 60-80 ℃, the plating time is 20-30 minutes, then an acidic chemical nickel layer with the thickness of 2.5-4.0 microns is formed, and the plated piece is taken out and cleaned with pure water;
s8: electroplating soft gold: and (5) putting the plated part obtained in the step (S7) into a soft gold solution for plating, wherein the temperature of the soft gold solution is 55-65 ℃, the pH value is 4.5-5.0, the current density is 0.1-0.5A/dm 2, a soft gold layer with the thickness of 0.3-1 micrometer is formed after electroplating for 8-18 minutes, and the plated part is taken out after electroplating, cleaned by pure water, dried by blowing and dried after surface moisture is dried.
2. The electroplating process of copper diamond according to claim 1, characterized in that: the chemical oil removing solution comprises: 40-60 g/L of C02 deoiling powder, and pure water as a solvent.
3. The electroplating process of copper diamond according to claim 1, characterized in that: the microetching solution comprises: microetching powder-MEOX 100-130 g/L, AR sulfuric acid 10-40 ml/L, and pure water as solvent.
4. The electroplating process of copper diamond according to claim 1, characterized in that: the colloidal palladium solution is as follows: 8-10 ml/L, HN-200B of HN-200A colloidal palladium activator, 50-60 ml/L, AR ml/310 ml/L of hydrochloric acid and a solvent of pure water.
5. The electroplating process of copper diamond according to claim 1, characterized in that: the alkaline chemical nickel solution is as follows: Al-8100A175ml/L, AL-8100C60ml/L, 8100 stabilizer 60ml/L, and solvent is pure water.
6. The electroplating process of copper diamond according to claim 1, characterized in that: the acidic chemical nickel solution is as follows: HN-310A60ml/L, HN-310B150ml/L, solvent is pure water.
7. The electroplating process of copper diamond according to claim 1, characterized in that: the soft gold solution is a weak acid soft gold electroplating solution, and the weak acid soft gold electroplating solution comprises: 100g/L of Au-Make Up salt, 3.7-4.4 g/L, Au g/4.4 g/L, Au-30 g/L, Au-8.4 ml/L of gold potassium cyanide-containing MLA acid, and pure water as a solvent.
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