CN101748427A - Titanium plate of a kind of plated with thick gold membrane and preparation method thereof - Google Patents

Titanium plate of a kind of plated with thick gold membrane and preparation method thereof Download PDF

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Publication number
CN101748427A
CN101748427A CN200810227769A CN200810227769A CN101748427A CN 101748427 A CN101748427 A CN 101748427A CN 200810227769 A CN200810227769 A CN 200810227769A CN 200810227769 A CN200810227769 A CN 200810227769A CN 101748427 A CN101748427 A CN 101748427A
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China
Prior art keywords
plated
titanium plate
gold
thickness
substrate
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CN200810227769A
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Chinese (zh)
Inventor
罗远辉
王力军
陈松
张力
尹延西
江洪林
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Beijing General Research Institute for Non Ferrous Metals
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Beijing General Research Institute for Non Ferrous Metals
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Priority to CN200810227769A priority Critical patent/CN101748427A/en
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Abstract

The invention discloses titanium plate of a kind of plated with thick gold membrane that belongs to metallic substance coating technology field and preparation method thereof.Its preparation process comprises: choosing thickness is the titanium plate of 1~3mm, to carrying out chemical nickel plating, electrogilding and heat treatment process after its surface treatment, obtaining plated thickness is 5~10 μ m, and binding force of cladding material is 20~25MPa, and the Gold plated Layer surface is amplified 2000 times with scanning electron microscope and observed free of pinholes.Behind the titanium surface-coated gold, Gold plated Layer is fine and close and have a certain thickness, titanium combines with Gold plated Layer firmly, gold-plated titanium plate like this can either keep good electrochemical catalysis reactive behavior and electroconductibility, have very strong erosion resistance and electrochemical stability again, can be used as the negative electrode of electrode, can satisfy long-time large-current electric and separate/electroplate requirements of one's work, be specially adapted to the electrochemical treatment process in the nuclear industry as electrolyzer.

Description

Titanium plate of a kind of plated with thick gold membrane and preparation method thereof
Technical field
The invention belongs to metallic substance coating technology field, the titanium plate of particularly a kind of plated with thick gold membrane (thickness is 5~10 μ m) the invention still further relates to the preparation method of above-mentioned gold-plated titanium plate simultaneously.
Background technology
In the production of weapon material, parts, usually to use electrochemical surface processing treatment technology, as electrolysis and plating etc., make parts surface form special functional coating, to satisfy its use properties and Working environment requirement.What use morely both at home and abroad at present is noble coatings (gold and silver, platinum and rhodium etc.).In the process of using electrochemical treatment prepared top coat, generally to use noble electrode, as graphite, stainless steel, lead alloy, nickelalloy, titanium alloy and titanium alloy/coated electrode etc., because electrolysis/plating generally is to use in acidity or basic solution environment, the environment for use harshness, not only require electrode itself to have good electrochemical catalysis reactive behavior and conductivity, and require electrode to have superior corrosion resistance and electrochemical stability, reduce the energy consumption of electrochemical reaction process as far as possible.
Gold has very high electropotential in the aqueous solution, have very strong chemical stability and erosion resistance, does not dissolve in many kind acid, alkali and Oxidant.
Au→Au ++e
Au→Au 3++3e
Be standard potential.
Titanium to cause blunt current potential more negative, the surface very easily forms the thin and fine and close oxide film of one deck, has very strong passivation tendency and passive state stability in many media.Titanium has superior corrosion resistance in many media (as acid, neutrality, week reduction and Oxidant etc.), particularly have good anti-local corrosion (spot corrosion, crevice corrosion, intergranular corrosion, abrasion, fatigue corrosion and stress corrosion etc.) performance.
The electrode of titanium surface-coated gold can either keep good electrochemical catalysis reactive behavior and electroconductibility, has very strong erosion resistance and electrochemical stability again.Even kind electrode uses in the solution of chloride, still has good solidity to corrosion.If titanium is combined with Gold plated Layer firmly, Gold plated Layer is fine and close and have a certain thickness, the electrode that makes like this has good electrochemical activity, stability and good electroconductibility in electrochemistry Working environment (electrolysis/plating), can satisfy long-time large-current electric and separate/electroplate requirements of one's work.
Summary of the invention
The purpose of this invention is to provide a kind of titanium plate of plated with thick gold membrane, it is characterized in that, is matrix with the titanium plate, and the titanium plate thickness is 1~3mm, and plated thickness is 5~10 μ m.
Another object of the present invention provides a kind of preparation method of above-mentioned gold-plated titanium plate, it is characterized in that, concrete steps are as follows:
(1) choosing thickness is that the titanium plate of 1~3mm is a substrate;
(2) titanium plate surface treatment: sandblasting 8~20 minutes, the remover cutter trade increases roughness, obtains the surface of comparatively fresh, helps improving the bonding force of coating; Ultrasonic cleaning 8~20 minutes is that 40% NaOH heat alkali liquid cleans with concentration, removes substrate surface because of the greasy dirt of depositing or machining is adsorbed; Adopt hot 20%HF-20%HCl or 20%HF-20%HNO 3Mixing acid etch substrate 8~20 minutes, the oxide film of removal substrate surface;
(3) chemical nickel plating:
Adopt the weakly alkaline chemical nickel-plating liquid, plated nickel bottom on substrate, the composition of the nickel-plating liquid of employing is: the NiSO of 25~40g/L 47H 2O, the NaH of 10~25g/L 2PO 2H 2O, the NH of 40~60g/L 4Cl, the Na of 70~90g/L 3C 6H 5O 72H 2O; Its pH value is 8~9.5; Technological temperature is 75~90 ℃, and the process time is 8~20 minutes; Put into clear water after the nickel plating and clean up, nickel layer thickness is 1~2 μ m;
Adopt the purpose of chemical nickel plating bottom, the one, prevent that the titanium alloy substrate unsalted surface from forming oxide passivation film before plating; The 2nd, guarantee to electroplate out bonding force and the qualified gold plate of density;
(4) electrogilding:
Adopt double-pulse plating technology gold-plated, adopting the composition of electroplate liquid is the KAuCN of 8~15g/L, and the pH value is 3.8~5.2, and temperature is 30~35 ℃; The titanium plate is made negative electrode, and the negative electrode rotating speed is 5~15m/min, and platinum titanium net is made anode; Pulse parameter is: average current density is 0.7~1.2A/dm 2, peak current density is 4.5~5.5A/dm 2, dutycycle is 1: 3~1: 5, frequency is 750~850Hz; Electroplating time is 36~60 hours, puts into clear water after gold-plated to clean up thickness of coating 5~10 μ m;
Adopt periodic reverse two pulse electric current when gold is electroplated, the inhomogeneous anodic current of the caused height of the reverse impulse of short period of time distributes significantly, makes the protruding place of coating be dissolved strongly and flatten.The remarkable advantage of double-pulse plating gold is: (1) coating crystallization is careful, bright, and porosity is low; (2) thickness of coating is even, and leveling property is good; (3) elimination of hydrogen embrittlement reduces the coating internal stress; (4) improve binding force of cladding material; (5) coating deposition rate is accelerated.Adopt the double-pulse plating gold that performance index such as the heatproof of coating, wear-resisting, welding, toughness, anticorrosion, electric conductivity, smooth finish are significantly improved, and can save gold (saving 20~50%) significantly, save additive (saving 50~80%) as brightening agent;
(5) thermal treatment:
Thermal treatment is carried out in the vacuum heat treatment furnace of argon shield is arranged, and thermal treatment temp is 400 ℃, and the time is 2 hours, and thermal treatment can make the bonding force between titanium plate and the Gold plated Layer reliably be guaranteed.
After thermal treatment finishes,, measure binding force of cladding material, with scanning electron microscopic observation Gold plated Layer condition of surface with stretching method with the thickness of thickness tester measurement Gold plated Layer.
Beneficial effect of the present invention is: the bonding force between titanium plate and the Gold plated Layer is 20~25MPa, uses the scanning electron microscopic observation condition of surface, amplifies and observes free of pinholes more than 2000 times; Behind the titanium surface-coated gold, Gold plated Layer is fine and close and have a certain thickness, titanium combines with Gold plated Layer firmly, gold-plated titanium plate like this can either keep good electrochemical catalysis reactive behavior and electroconductibility, have very strong erosion resistance and electrochemical stability again, can be used as the negative electrode of electrode, can satisfy long-time large-current electric and separate/electroplate requirements of one's work, be applicable to the electrochemical treatment process in the nuclear industry as electrolyzer.
Embodiment
The invention provides titanium plate of a kind of plated with thick gold membrane and preparation method thereof, the present invention will be further described below in conjunction with embodiment.
Embodiment 1
1, by long 100mm, the thick titanium plate of wide 100mm cutting 1mm is a substrate;
2, titanium plate surface treatment: sandblasting 10 minutes; Ultrasonic cleaning 10 minutes; With concentration is that 40% NaOH heat alkali liquid cleaned 10 minutes, removes substrate surface because of the greasy dirt of depositing or machining is adsorbed; With the 20%HF-20%HCl mixing acid etch substrate of heat 10 minutes, remove the oxide film of substrate surface;
3, to surface-treated titanium plate gauge model nickel plating 10 minutes, the composition of the nickel-plating liquid that nickel plating technology adopts is: the N iSO of 33g/L 47H 2O, the NaH of 17g/L 2PO 2H 2O, the NH of 50g/L 4Cl, the Na of 84g/L 3C 6H 5O 72H 2O, the pH value is 9.5, and technological temperature is 85 ℃, puts into clear water after the nickel plating and cleans up, and nickel layer thickness is 1.5 μ m;
4, adopted double-pulse plating technology gold-plated 48 hours, electroplate liquid is that concentration is the KAuCN solution of 12g/L, and the pH value is 4.9,32 ± 3 ℃ of temperature, and the titanium plate is made negative electrode, and the negative electrode rotating speed is 7m/min, and platinum titanium net is made anode; Pulse parameter is: average current density 1A/dm 2, peak current density 5A/dm 2, dutycycle 1: 5, frequency: 800Hz; Putting into clear water after gold-plated cleans up;
5, thermal treatment: carry out in the vacuum heat treatment furnace of argon shield is arranged, thermal treatment temp is 400 ℃, and the time is 2 hours.
After thermal treatment finished, the thickness of measuring Gold plated Layer with thickness tester was 8 μ m, and measuring binding force of cladding material with stretching method is 21.6MPa, with scanning electron microscopic observation Gold plated Layer condition of surface, amplified 2500 times of observations, did not find pin hole.
Embodiment 2
1, by long 150mm, the thick titanium plate of wide 150mm cutting 2mm is a substrate;
2, titanium plate surface treatment: sandblasting 12 minutes; Ultrasonic cleaning 12 minutes; With concentration is that 40% NaOH heat alkali liquid cleaned 12 minutes, removes substrate surface because of the greasy dirt of depositing or machining is adsorbed; With the 20%HF-20%HCl mixing acid etch substrate of heat 12 minutes, remove the oxide film of substrate surface;
3, to surface-treated titanium plate gauge model nickel plating 12 minutes, the composition of the nickel-plating liquid that nickel plating technology adopts is: the NiSO of 30g/L 47H 2O, the NaH of 20g/L 2PO 2H 2O, the NH4Cl of 55g/L, the Na of 80g/L 3C 6H 5O 72H 2O, the pH value is 9.8, and technological temperature is 85 ℃, puts into clear water after the nickel plating and cleans up, and nickel layer thickness is 1.7 μ m;
4, adopted double-pulse plating technology gold-plated 48 hours, electroplate liquid is that concentration is the KAuCN solution of 10g/L, and the pH value is 5.1,32 ± 3 ℃ of temperature, and the titanium plate is made negative electrode, and the negative electrode rotating speed is 7m/min, and platinum titanium net is made anode; Pulse parameter is: average current density 1.2A/dm 2, peak current density 4.5A/dm 2, dutycycle 1: 4, frequency: 800Hz; Putting into clear water after gold-plated cleans up;
5, thermal treatment: carry out in the vacuum heat treatment furnace of argon shield is arranged, thermal treatment temp is 400 ℃, and the time is 2 hours.
After thermal treatment finished, the thickness of measuring Gold plated Layer with thickness tester was 8.6 μ m, and measuring binding force of cladding material with stretching method is 23MPa, with scanning electron microscopic observation Gold plated Layer condition of surface, amplified 3000 times of observations, did not find pin hole.
Embodiment 3
1, by long 200mm, the thick titanium plate of wide 200mm cutting 2.5mm is a substrate;
2, titanium plate surface treatment: sandblasting 15 minutes; Ultrasonic cleaning 15 minutes; With concentration is that 40% NaOH heat alkali liquid cleaned 10 minutes, removes substrate surface because of the greasy dirt of depositing or machining is adsorbed; 20%HF-20%HNO with heat 3Mixing acid etch substrate 15 minutes, the oxide film of removal substrate surface;
3, to surface-treated titanium plate gauge model nickel plating 20 minutes, the composition of the nickel-plating liquid that nickel plating technology adopts is: the NiSO of 37g/L 47H 2O, the NaH of 24g/L 2PO 2H 2O, the NH of 55g/L 4Cl, the Na of 90g/L 3C 6H 5O 72H 2O, the pH value is 10.2, and technological temperature is 85 ℃, puts into clear water after the nickel plating and cleans up, and nickel layer thickness is 1.9 μ m;
4, adopted double-pulse plating technology gold-plated 48 hours, electroplate liquid is that concentration is the KAuCN solution of 15g/L, and the pH value is 4.6,32 ± 3 ℃ of temperature, and the titanium plate is made negative electrode, and the negative electrode rotating speed is 7m/min, and platinum titanium net is made anode; Pulse parameter is: average current density 0.8A/dm 2, peak current density 5.5A/dm 2, dutycycle 1: 5, frequency: 850Hz; Putting into clear water after gold-plated cleans up;
5, thermal treatment: carry out in the vacuum heat treatment furnace of argon shield is arranged, thermal treatment temp is 400 ℃, and the time is 2 hours.
After thermal treatment finished, the thickness of measuring Gold plated Layer with thickness tester was 9.5 μ m, and measuring binding force of cladding material with stretching method is 24.7MPa, with scanning electron microscopic observation Gold plated Layer condition of surface, amplified 3000 times of observations, did not find pin hole.
Above embodiment is the typical embodiment of the present invention, and those skilled in the art can corresponding within the scope of the claims change.

Claims (4)

1. the titanium plate of a plated with thick gold membrane is characterized in that, the titanium plate is a matrix, and the thickness of titanium plate is 1~3mm, and plated thickness is 5~10 μ m.
2. the preparation method of a plated with thick gold membrane titanium plate is characterized in that, concrete processing step is as follows:
(1) choosing thickness is that the titanium plate of 1~3mm is a substrate;
(2) titanium plate surface treatment: sandblasting 8~20 minutes; Ultrasonic cleaning 8~20 minutes uses the NaOH heat alkali liquid of concentration 40% to clean 8~20 minutes, removes the greasy dirt of substrate surface; Adopting the concentration of heat is 20%HF-20%HCl or 20%HF-20%HNO 3Mixed acid solution etch substrate 8~20 minutes, remove the oxide film of substrate surface;
(3) chemical nickel plating: plated thickness is the nickel bottom of 1~2 μ m on substrate, after the nickel plating substrate is put into clear water and cleans up;
(4) electrogilding: adopt double-pulse plating technology gold-plated, plated thickness is 5~10 μ m, substrate is put into clear water after gold-plated to clean up;
(5) thermal treatment: under 360~480 ℃, vacuum heat treatment is 1.5~2.5 hours under the argon shield, obtains described plated with thick gold membrane titanium plate.
3. the preparation method of a kind of plated with thick gold membrane titanium plate according to claim 2 is characterized in that: the composition of the nickel-plating liquid that the nickel chemical plating technology of described step (3) adopts is: the NiSO of 25~40g/L 47H 2O, the NaH of 10~25g/L 2PO 2H 2O, the NH of 40~60g/L 4Cl, the Na of 70~90g/L 3C 6H 5O 72H 2O; Its pH value is 8~9.5; Technological temperature is 75~90 ℃, and the process time is 8~20 minutes.
4. the preparation method of plated with thick gold membrane titanium plate according to claim 2 is characterized in that: the double-pulse plating technology of described step (4): adopting the composition of electroplate liquid is the KAuCN of 8~15g/L, and the pH value is 3.8~5.2, and temperature is 30~35 ℃; The titanium plate is made negative electrode, and the negative electrode rotating speed is 5~15m/min, and platinum titanium net is made anode; Pulse parameter is: average current density is 0.7~1.2A/dm 2, peak current density is 4.5~5.5A/dm 2, dutycycle is 1: 3~1: 5, frequency is 750~850Hz; Electroplating time is 36~60 hours.
CN200810227769A 2008-12-02 2008-12-02 Titanium plate of a kind of plated with thick gold membrane and preparation method thereof Pending CN101748427A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102154669A (en) * 2011-03-28 2011-08-17 冠锋电子科技(梅州)有限公司 Method for plating thick soft gold by utilizing plating thin golden cylinder
CN102410927A (en) * 2011-08-23 2012-04-11 复旦大学 Determination method of nuclear power apparatus heat exchanger failure reason
US9062384B2 (en) 2012-02-23 2015-06-23 Treadstone Technologies, Inc. Corrosion resistant and electrically conductive surface of metal
CN108264134A (en) * 2018-01-25 2018-07-10 石家庄市源生园环保有限公司 A kind of high-COD waste water electrolysis electrode with high salt and electrolytic oxidation process method

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102154669A (en) * 2011-03-28 2011-08-17 冠锋电子科技(梅州)有限公司 Method for plating thick soft gold by utilizing plating thin golden cylinder
CN102154669B (en) * 2011-03-28 2013-03-13 冠锋电子科技(梅州)有限公司 Method for plating thick soft gold by utilizing plating thin golden cylinder
CN102410927A (en) * 2011-08-23 2012-04-11 复旦大学 Determination method of nuclear power apparatus heat exchanger failure reason
US9062384B2 (en) 2012-02-23 2015-06-23 Treadstone Technologies, Inc. Corrosion resistant and electrically conductive surface of metal
US9493883B2 (en) 2012-02-23 2016-11-15 Treadstone Technologies, Inc. Corrosion resistant and electrically conductive surface of metal
CN108264134A (en) * 2018-01-25 2018-07-10 石家庄市源生园环保有限公司 A kind of high-COD waste water electrolysis electrode with high salt and electrolytic oxidation process method
CN108264134B (en) * 2018-01-25 2020-09-11 石家庄市源生园环保有限公司 High-salt high-COD wastewater electrolytic electrode and electrolytic oxidation treatment method

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