CN1632176A - Process of gold plating for industrial pure titanium - Google Patents

Process of gold plating for industrial pure titanium Download PDF

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Publication number
CN1632176A
CN1632176A CN 200410155460 CN200410155460A CN1632176A CN 1632176 A CN1632176 A CN 1632176A CN 200410155460 CN200410155460 CN 200410155460 CN 200410155460 A CN200410155460 A CN 200410155460A CN 1632176 A CN1632176 A CN 1632176A
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China
Prior art keywords
plating
pure titanium
industrial pure
gold
gold plating
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CN 200410155460
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Chinese (zh)
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CN100351433C (en
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梁成浩
杨长江
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Dalian University of Technology
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Dalian University of Technology
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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
    • 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
    • C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
    • C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
    • 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
    • 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
    • C25D5/50—After-treatment of electroplated surfaces by heat-treatment

Abstract

A process of gold plating for an industrial pure titanium belongs to a surface processing technic field of the industrial pure titanium. The process comprises polish, degreasing, alkali cleaning, descaling, acid pickling, activation, chemically plating nickel, plating gold, isopropanol dehydration, heat treatment; and washing between the processes by using distilled water. The process is characterised in that descaling, acid pickling, activation performed on the industrial pure titanium are completed in a special solution, and then the industrial pure titanium is directly entered into a chemical nickel plating solution to perform chemically plating, subsequently the industrial pure titanium is instantly put into a gold plating groove. The industrial pure titanium is dried for 4 hours by a 200 DEG C heat wind after plating 4-5 hours and isopropanol dehydration. The obtained plating layer has a good binding force after a bending and breaking test. The nickel layer has a thickness of 5-20 mu m, the plating layer is burnished, a P content is 7-9% (wt).

Description

A kind of process of gold plating for industrial pure titanium
Technical field
The invention belongs to the technical field of surface of industrially pure titanium.The craft of gilding that relates to a kind of industrially pure titanium workpiece.
Background technology
Titanium is the metal of height chemical property activity, and very easily passivation under the condition of aerobic is so have superior corrosion resistance.At air, seawater and many media is anti-corrosion, not with chlorine, chloride soln, the nitric acid effect of humidity, during room temperature not with dilute sulphuric acid, dilute hydrochloric acid effect.Titanium not only solidity to corrosion is good, and the specific tenacity height, and the tensile strength of pure titanium is 350-700Mpa.Therefore be widely used in various fields such as chemical industry, space flight, military project.But titanium parts scratches easily, kill, and electroconductibility is bad, also is subjected to certain limitation so use.Therefore to handle the titanium surface, wait as nickel plating, chromium plating and improve its antiseptic property.Gold plate becomes ideal coating to have very good anti-corrosion surface and excellent shielding property under certain environment.
The steel part difficulty that titanium base metal lining is more common, reason is that titanium and oxygen have stronger avidity, though useable solvents degreasing, remove original oxide skin through acid etching, but inevitable later on through washing, the workpiece ingress of air, moment forms layer oxide film again in oxygen-containing medium, this oxide film has very high chemical stability, is difficult to the good coating of plating one deck bonding force on this layer film.At present, both at home and abroad about titanium base chemical nickel plating and more gold-plated reports are arranged.But the method technical process that they provide is comparatively complicated, and the work period is longer, and operation easier is higher, the titanium hydrogen embrittlement in indivedual not consideration processes of method and the influence of binding force of cladding material.The direct chemical nickel layer obtains nickel-phosphorus coating on titanium, and direct gold-plated technology is not seen patent, bibliographical information on nickel phosphorus layer again.
Summary of the invention
The purpose of this invention is to provide a kind ofly can access the good proof gold coating of bonding force, simultaneously technology also can obtain the process of gold plating for industrial pure titanium of good middle phosphorus nickel layer.
Technical solution of the present invention is: titanium material workpiece is through polishing, and oil removing is after the alkali cleaning, descale acid etching, activation with solution provided by the invention and processing parameter, the titanium surface enters in the chemical nickel-plating solution after forming layer of even beige surface film, and control pH is 4.5-5.5, temperature is under 85-95 ℃, under the agitation condition, plating 0.5-1.5 hour, can obtain the coating of 5-20 μ m, coating can use as nickel-phosphorus coating separately through after 400 ℃ of vacuum heat treatment.Also can put plating bath immediately into, adopt sulphite to make complexing agent, at 45-60 ℃, pH=8-10, current density 0.1-0.3mA/cm 2, negative electrode moves stirring, carries out gold-plated.Electroplate after 4-5 hour, behind isopropanol dehydration, 200 ℃ of following warm air dryings 4 hours.The thickness of the chemical Ni-plating layer that obtains is 5-20 μ m, gold plate thickness 5-10 μ m, and coating is through bending and breaking test, and bonding force is good.Ni-P coating light P content is 7-9% (wt), and gold plate any surface finish, smooth, fine and close under 10,000 times of scanning electron microscope, is not seen the space.
The solution composition of above-mentioned operation and related process parameter are as follows:
Descale solution composition and processing parameter is:
HF(40％wt) 300-400ml/L
HNO 3(60％wt) 30-50ml/L，
Time 0.5-1min
The temperature room temperature
Acid etching solution composition and processing parameter are:
HNO 3(60％wt) 150-180ml/L
HF(40％wt) 15-25ml/L
Time 10-30s
The temperature room temperature
Activated solution is formed and processing parameter is:
NaBF 4 30-50g/L
NaNO 3 30-50g/L
Titanium sulfate 2-5g/L
Temperature 60-80 ℃
Time 4-15min
Chemical nickel-plating solution consists of:
Single nickel salt 20-25g/L
Inferior sodium phosphate 20-25g/L
Lactic acid, 25-35g/L
Tartrate 1-3g/L
Oxysuccinic acid 0.5-1.5g/L
Gold-plating solution consists of:
Gold sodium sulfide (in Au) 5-25g/L
Tripotassium Citrate 80-120g/L
Ammonium sulphite 180-250g/L
EDTA 2-4g/L
Polyoxyethylene glycol 1-2g/L
The beneficial effect that the present invention reached is: because the rational pretreatment technology of process using, the gold-plated operating time is greatly reduced, gold plate adopts nickel to make prime coat, can be used as the blocking layer between gold, the titanium, prevent phase mutual diffusion between gold, the titanium, improve gold plate substrate hardness simultaneously, also can use nickel-phosphorus coating as required separately simultaneously.Chemical nickel-plating liquid and gold plating liquid that the present invention proposes have good stability, and use continuously by reasonably adding solution compolision, can prolong the plating bath life cycle.This gold plating for industrial pure titanium technological operation is simple, and less investment all has broad application prospects in many departments such as aviation, chemical industry, ocean, the energy
Embodiment
Getting label is TA 2The commercial titanium sheet, volume is 35.0 * 20.0 * 0.8mm, this titanium sheet adopts following technical process gold-plated without use: the polishing? oil removing Quince neodymium?-descale? acid etching? activation? the flat Nang isopropanol dehydration of chemical nickel plating Shu Duo? thermal treatment.
Concrete steps are:
The 1st step. polishing: polish to light the water flushing with 500#SiC sand paper wet method.
The 2nd step. oil removing: under the room temperature, ultrasonic wave acetone oil removing 15min, water flushing.
The 3rd step. alkali cleaning: washing lotion composition and technological specification are as follows
NaOH 30-50g/L
NaCO 3 20-40g/L
Na3PO 4 20-40g/L
Temperature 80-90 ℃
Time 5-10min
After the alkali cleaning, the water flushing.
The 4th step. descale:
HF(40％wt) 300-400ml/L
HNO 3(60％wt) 30-50ml/L，
Time 0.5-1min
The temperature room temperature
The 5th step. acid etching:
HNO 3(60％wt) 150-180ml/L
HF(40％wt) 15-25ml/L
Time 10-30s
The temperature room temperature
The 6th step. activation:
NaBF 4 30-50g/L
NaNO 3 30-50g/L
Titanium sulfate 2-5g/L
Temperature 60-80 ℃
Time 4-15min
Be activated to the film that titanium spare surface generates one deck grey black.
The 7th step. chemical nickel plating:
Single nickel salt 20-25g/L
Inferior sodium phosphate 20-25g/L
Lactic acid, 25-35g/L
Tartrate 1-3g/L
Oxysuccinic acid 0.5-1.5g/L
pH 4.5-5.0
Temperature 80-90,
Sedimentation velocity, 10 μ m/h
1. the load of chemical plating fluid should be controlled at 1dm 2/ L.
2. the preparation of chemical nickel-plating liquid in proper order: at first will dissolve in distilled water as the lactic acid and the oxysuccinic acid of complexing agent, the water yield is no more than 10% of total amount.Transfer pH to be about 4 with sodium hydroxide or ammoniacal liquor, add dissolved nickel sulfate solution, stir.Add the ortho phosphorous acid sodium solution while stirring, transfer pH=4.8, be diluted to volume, filter with pH meter, behind the assay, heating in water bath to 90 ℃ use.
3. adding of the nickel salt of chemical plating fluid, reductive agent: whenever separate out 1g nickel, should add the 5.6g inferior sodium phosphate, add the stablizer of original formulation 1.9%.
4. if only need nickel layer, can use after 150 ℃ of warm air dryings,, plating piece be got final product 400 ℃ of vacuum heat treatment if need fabulous bonding force.
The 8th step. electrogilding
Gold sodium sulfide (in Au) 5-25g/L
Tripotassium Citrate 80-120g/L
Ammonium sulphite 180-250g/L
EDTA 2-4g/L
Polyoxyethylene glycol 1-2g/L
pH 8-10
Temperature 50-55 ℃,
Anode, Pt/Ti
Cathode current density 0.1-0.3mA/cm 2
Time 4hr
The alr mode negative electrode moves
1. after the electroless plating, behind distilled water flushing, electroplate immediately.If the residence time is longer in air for some reason, should be warm 1: carry out gold-plated among the 1HCl behind the activation 20-30s.
2. the preparation of electroplate liquid: get 25% ammonium sulphite 85ml, be heated to 50-60 ℃.(add under constantly stirring, obtain faint yellow transparent liquid earlier, be stirred and heated to 70-80 ℃, solution becomes water white transparency with gold sodium sulfide solution.Adding Tripotassium Citrate 10g, add EDTA and polyglycol solution, behind the accent pH, the examination plating.
3. the gold of plating bath can directly be replenished by gold sodium sulfide
The 9th step. the isopropanol dehydration drying
The 10th step. thermal treatment: 200 ℃ of following air cycle dryings, 4 hours
The gold plate uniform and delicate that obtains, any surface finish, wiping does not have powder and comes off.Through electron probe microanalysis, the thickness of chemical Ni-plating layer is about 10 μ m, and gold plate thickness is about 5 μ m,, through Ni-P coating is carried out point analysis, its P content is about 7.82% (wt), belongs to typical middle phosphorus coating (4-11%wt).Gold plate is bright and clean, smooth, fine and close.With 10,000 times of scanning electron microscope analysis, do not see the space.With pliers the titanium sheet after plating will then to 90 ° of the other side bendings as far as possible rapidly, be ruptured up to plating piece earlier to crooked 90 ° on one side, binding force of cladding material is good.

Claims (7)

1. process of gold plating for industrial pure titanium, flow process comprises polishing, oil removing, alkali cleaning descales, acid etching, activation, chemical nickel plating, electrogilding, isopropanol dehydration, thermal treatment, the per pass inter process all is no less than 20 seconds with distilled water flushing; It is characterized in that, industrially pure titanium is carried out oxide film dissolving, acid etching, activation is finished in certain solution respectively, and the surface enters in the chemical nickel-plating solution after forming layer of even beige surface film, control pH is 4.5-5.5, and temperature is under 85-95 ℃, after plating 0.5-1.5 hour, afterwards, promptly put plating bath into, adopt sulphite to make complexing agent, under 45-60 ℃, negative electrode moves to stir and carries out gold-platedly, electroplates to go out groove after 4-5 hour and wash, behind isopropanol dehydration, 200 ℃ of following warm air dryings 4 hours.
2. a kind of process of gold plating for industrial pure titanium according to claim 1 is characterized in that, descale solution composition and processing parameter are:
HF(40％wt) 300-400ml/L，
HNO3(60％wt) 30-50ml/L，
Time 0.5-1min,
The temperature room temperature.
3. a kind of process of gold plating for industrial pure titanium according to claim 1 is characterized in that, acid etching solution composition and processing parameter are:
HNO3(60％wt) 150-180ml/L，
HF(40％wt) 15-25ml/L，
Time 10-30s,
The temperature room temperature.
4. a kind of process of gold plating for industrial pure titanium according to claim 1 is characterized in that, activated solution is formed and processing parameter is:
NaBF4 30-50g/L，
NaNO3 30-50g/L，
Titanium sulfate 2-5g/L,
Temperature 60-80 ℃,
Time 4-15min.
5. a kind of process of gold plating for industrial pure titanium according to claim 1 is characterized in that chemical nickel-plating solution consists of:
Single nickel salt 20-25g/L,
Inferior sodium phosphate 20-25g/L,
Lactic acid, 25-35g/L,
Tartrate 1-3g/L,
Oxysuccinic acid 0.5-1.5g/L.
6. a kind of process of gold plating for industrial pure titanium according to claim 1 is characterized in that gold-plating solution consists of:
Gold sodium sulfide (in Au) 5-25g/L,
Tripotassium Citrate 80-120g/L,
Ammonium sulphite 180-250g/L,
EDTA 2-4g/L，
Polyoxyethylene glycol 1-2g/L.
7. a kind of process of gold plating for industrial pure titanium according to claim 1 is characterized in that, behind the chemical nickel plating, through 400 ℃ of vacuum heat treatment.
CNB2004101554608A 2004-11-19 2004-11-19 Process of gold plating for industrial pure titanium Expired - Fee Related CN100351433C (en)

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Application Number Priority Date Filing Date Title
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Application Number Priority Date Filing Date Title
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CN1632176A true CN1632176A (en) 2005-06-29
CN100351433C CN100351433C (en) 2007-11-28

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101235524B (en) * 2006-11-07 2010-12-08 恩伊凯慕凯特股份有限公司 Non-cyanide electrolysis gold plating bath for gold bump and gold wiring
CN1944716B (en) * 2005-09-30 2011-12-14 美泰乐科技(日本)股份有限公司 Non-cyanogen type electrolytic gold plating bath for bump forming
CN101204861B (en) * 2007-12-03 2013-03-13 中国科学院上海硅酸盐研究所 Titanium alloy parts protection and its preparation method and uses of hydrogen prevention crisp
CN103741180A (en) * 2014-01-10 2014-04-23 哈尔滨工业大学 Cyanide-free bright electrogilding additive and application thereof
CN104032343A (en) * 2014-05-14 2014-09-10 蚌埠富源电子科技有限责任公司 Novel electroplating pre-treatment technology for titanium and titanium alloy
CN109530438A (en) * 2018-11-07 2019-03-29 湖北第二师范学院 A kind of light radiation the space pure titanium strip in razor-thin of Zn-Ag composite deposite and its production method
CN109537011A (en) * 2018-12-06 2019-03-29 上海众新五金有限公司 A kind of auto parts and components electroplate technology
CN111500996A (en) * 2020-05-15 2020-08-07 中国科学院兰州化学物理研究所 Method for preparing gold conductive lubricating film of vacuum electric contact component by magnetron sputtering method
CN113463148A (en) * 2021-06-29 2021-10-01 惠州市安泰普表面处理科技有限公司 Method for electroplating gold on surface of titanium or titanium alloy substrate
CN113897648A (en) * 2021-11-22 2022-01-07 东莞中探探针有限公司 Connector terminal electroplating process
KR102605141B1 (en) * 2022-11-29 2023-11-22 김기형 Plating processing method for surface treatment of metal

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62124290A (en) * 1985-11-22 1987-06-05 Citizen Watch Co Ltd Plate method to titanium surface
JP3020673B2 (en) * 1991-08-21 2000-03-15 同和鉱業株式会社 Pre-plating method for titanium alloy material

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1944716B (en) * 2005-09-30 2011-12-14 美泰乐科技(日本)股份有限公司 Non-cyanogen type electrolytic gold plating bath for bump forming
CN101235524B (en) * 2006-11-07 2010-12-08 恩伊凯慕凯特股份有限公司 Non-cyanide electrolysis gold plating bath for gold bump and gold wiring
CN101204861B (en) * 2007-12-03 2013-03-13 中国科学院上海硅酸盐研究所 Titanium alloy parts protection and its preparation method and uses of hydrogen prevention crisp
CN103741180A (en) * 2014-01-10 2014-04-23 哈尔滨工业大学 Cyanide-free bright electrogilding additive and application thereof
CN103741180B (en) * 2014-01-10 2015-11-25 哈尔滨工业大学 Non-cyanide bright electrogilding additive and application thereof
CN104032343A (en) * 2014-05-14 2014-09-10 蚌埠富源电子科技有限责任公司 Novel electroplating pre-treatment technology for titanium and titanium alloy
CN109530438A (en) * 2018-11-07 2019-03-29 湖北第二师范学院 A kind of light radiation the space pure titanium strip in razor-thin of Zn-Ag composite deposite and its production method
CN109537011A (en) * 2018-12-06 2019-03-29 上海众新五金有限公司 A kind of auto parts and components electroplate technology
CN111500996A (en) * 2020-05-15 2020-08-07 中国科学院兰州化学物理研究所 Method for preparing gold conductive lubricating film of vacuum electric contact component by magnetron sputtering method
CN111500996B (en) * 2020-05-15 2021-12-31 中国科学院兰州化学物理研究所 Method for preparing gold conductive lubricating film of vacuum electric contact component by magnetron sputtering method
CN113463148A (en) * 2021-06-29 2021-10-01 惠州市安泰普表面处理科技有限公司 Method for electroplating gold on surface of titanium or titanium alloy substrate
CN113897648A (en) * 2021-11-22 2022-01-07 东莞中探探针有限公司 Connector terminal electroplating process
KR102605141B1 (en) * 2022-11-29 2023-11-22 김기형 Plating processing method for surface treatment of metal

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