CN101016639A - Process of titanium basal body electric plating platinum coating - Google Patents
Process of titanium basal body electric plating platinum coating Download PDFInfo
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- CN101016639A CN101016639A CN 200610155616 CN200610155616A CN101016639A CN 101016639 A CN101016639 A CN 101016639A CN 200610155616 CN200610155616 CN 200610155616 CN 200610155616 A CN200610155616 A CN 200610155616A CN 101016639 A CN101016639 A CN 101016639A
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Abstract
The invention discloses a craft to electroplate platinum coating with titanium basal body, which comprises the following steps: smoothing titanium basal body surface; degreasing; proceeding pretreatment to remove oxide layer; proceeding pre-deposition palladium catalytic layer craft treatment; getting the titanium basal body with palladium catalytic activity on the surface; electroplating platinum in the chloroplatinic acid solution at last. This electric pole material possesses good cohesion, which is a simple and competitive electroplate platinum craft.
Description
(1) technical field
The present invention relates to a kind of titanium basal body electric plating platinum coating technology, relate in particular to a kind of industrialization electroplatinizing technology.
(2) background technology
Platinum is as electrode materials, be widely used in fields such as plating, electrolytic synthesis, electrochemical treatment waste water and fuel cell, platinum electrode has that erosion resistance is strong, catalytic performance is high, oxygen evolution potential is high and characteristic such as hydrogen-evolution overpotential is low, being the anode material of excellent property, is again the cathode material of excellent property.Except that minority mixing acid, platinum all shows remarkable corrosion resistance nature in hydrochloric acid, nitric acid, sulfuric acid, hydrofluoric acid, phosphoric acid and most electrolyte solution.Many important electrochemical industries field, as hydrogen peroxide, ammonium persulphate, can platinum in the production of brine electrolysis etc. as anode material.But the platinum scarcity of resources, cost an arm and a leg, the electrode materials area of especially industrial application is very big, and directly making electrode with pure platinum is infeasible on producing, and has restricted platinum electrode applying in electrochemical industry.
For reducing the electrode cost, save the platinum resource, need to adopt the platinum plating material replace pure platinum goods, therefore how on the different matrix material electroplatinizing become the focus of people's research, wherein titanium base platinum electrode becomes the electrode materials of tool application prospect in the platinized electrode with its superior corrosion resistance.Titanium matrix electroplatinizing technology mainly adopts P salt electroplating technology at present, this technology subject matter is P salt preparation difficulty, loss is big, cost is high, and the titanium matrix generates semi-conductor titanium dioxide zone of oxidation easily simultaneously, and binding force of cladding material is poor, work-ing life is short, can not satisfy the electrochemical industry application request.
(3) summary of the invention
The objective of the invention is to solve that current titanium matrix platinum binding force of cladding material is poor, shortcoming such as electroplating technology complexity and cost height, a kind of technology of titanium matrix Direct Electroplating platinum is provided, good, the fine and close light of coating of titanium base platinum electrode binding force of cladding material of preparation, good, the long service life of chemical property can be applicable to industry such as brine electrolysis, electrolytic synthesis and electrochemical treatment waste water.
The technical solution used in the present invention is as follows:
A kind of technology of titanium basal body electric plating platinum coating, comprise with the titanium matrix surface flatten, oil removing, removing oxide layer pre-treatment, also comprise treated titanium matrix is carried out pre-deposition palladium Catalytic Layer art breading, obtain the titanium matrix that the surface has catalytic activity, at last Direct Electroplating platinum in platinum acid chloride solution.
Described titanium matrix surface pre-treating technology is that the sandblast of titanium matrix surface obtains the titanium matrix that the surface is the canescence micro-rough to the leveling of titanium matrix surface; At 50～80 ℃ of following alkaline degreasings, place etching solution etch 1～30min again under room temperature, remove surface and oil contaminant and zone of oxidation again, described etching solution consists of 0.5～12molL
-1HCl, saturated oxalic acid and 1～10gL
-1The HF volume ratio is 1: 1: 1 a mixed solution.
Further, described pre-deposition palladium Catalytic Layer technology is carried out pre-deposition palladium Catalytic Layer for adopting electrochemistry scanning method, palladium plating method or colloidal palladium activation method.
Further, described electrochemistry scanning method pre-deposition palladium Catalytic Layer technology is for being anode with platinum, and mercurous chloride electrode (SCE) is a reference electrode, and electrolytic solution is that volume ratio is 0.1～6molL of 1: 1
-1H
2SO
4With 0.1～1.0gL
-1PdCl
2Mixed solution, be 1～500mVs with scanning speed under the room temperature
-1, current potential scanned depositing Pd 1～30 minute for+0.3 to-1.5V (vs SCE).
Described palladium plating method pre-deposition palladium Catalytic Layer technology is for being supporting electrode with platinum, at 0.1～12molL of 1: 1 composition of volume ratio
-1H
2SO
4With 0.1～1.0gL
-1PdCl
2Electroplate liquid in, under 10～90 ℃ the temperature of electroplating solution, with 10～1000Am
-2Current density, the cathodic deposition palladium is 1～30 minute on the titanium matrix.
Described colloidal palladium activation method pre-deposition palladium Catalytic Layer technology is with colloidal palladium solution activation titanium matrix, passes through the dilute hydrochloric acid solution dispergation again, obtains the surface and be brown palladium Catalytic Layer on the titanium matrix.Described colloidal palladium solution can be prepared according to laxative remedy: among the 20mlHCl, add the 0.7g sodium stannate under stirring, it is standby to stir the emulsion B liquid that obtains white.In another container, the 0.1g Palladous chloride is added in the mixed solution of 10mlHCl and 20ml deionized water again, after the heating for dissolving, add the 0.25g tin protochloride down, stir and get A liquid after 12 minutes at 30 ± 2 ℃.Under agitation A liquid is poured in the B liquid immediately then, be diluted to 100ml, obtain brown colloidal palladium solution with deionized water.
In described three kinds of pre-deposition palladium Catalytic Layer technologies, more effective is electrochemistry scanning method and palladium plating method.
The method of Direct Electroplating platinum will be through the titanium matrix of pre-deposition palladium Catalytic Layer for being anode with platinum in the described platinum acid chloride solution, and 85～95 ℃ are carried out electrolysis in platinum acid chloride solution, and electrolysis density is 100～1000Am
-2, preferred 100～600Am
-2Further, described platinum acid chloride solution is 1～12molL of 1: 1 of volume ratio
-1HCl and 1～50gL
-1H
2PtCl
26H
2The mixed solution of O solution.
Concrete, the technology of described titanium basal body electric plating platinum coating for the titanium matrix surface is flattened, sandblast, oil removing, etch, be supplementary anode then with platinum, mercurous chloride electrode is a reference electrode, electrolytic solution is that volume ratio is 0.1～6molL of 1: 1
-1H
2SO
4With 0.1～1.0gL
-1PdCl
2Mixed solution, be 1～500mVs with scanning speed under the room temperature
-1, current potential scanned depositing Pd 1～30 minute for+0.3 to-1.5V (vs SCE); Be 1～12molL of 1: 1 then in volume ratio
-1HCl and 1～50gL
-1H
2PtCl
26H
2In the mixing electroplate liquid of O, with 100～1000Am
-2The electrolysis of electrolysis density, promptly get titanium base platinum electrode.
Perhaps to the titanium matrix surface flatten, sandblast, oil removing, etch, make supporting electrode with platinum then, the 0.1～12molL that forms at 1: 1 in volume ratio
-1H
2SO
4With 0.1～1.0gL
-1PdCl
2Electroplate liquid in, under 10～90 ℃ the temperature of electroplating solution, with 10～1000Am
-2Current density titanium substrate cathode deposition 1～30 minute.Be 1～12molL of 1: 1 then in volume ratio
-1HCl and 1～50gL
-1H
2PtCl
26H
2In the mixing electroplate liquid of O, with 100～600Am
-2The electrolysis of electrolysis density, promptly get titanium base platinum electrode.
The present invention compared with prior art, its beneficial effect is embodied in:
The present invention adopts palladium activation titanium matrix, and in platinum acid chloride solution Direct Electroplating platinum, avoided the complicated procedures of forming of the main salt of preparation in the P salt platinum plating technology, saved noble metal platinum, the more important thing is the problem that has solved titanium matrix platinum plating bonding force difference, good, the bright densification of coating of titanium base platinum electrode material bonding force of preparation is simple, the competitive electroplatinizing technology of a kind of technology.
(4) embodiment:
Below with specific embodiment technical scheme of the present invention is described, but protection scope of the present invention is not limited thereto:
Embodiment 1
With the leveling of titanium matrix surface, spray quartz sand, the sandblast rear surface is canescence, and has the micro-rough surface; The general alkaline degreasing solution of commercially available washing composition has been added in employing, handles 0.5 hour down to remove degreasing at 60 ℃, and after cleaning with flowing water, the oxide compound on surface is removed in etch at room temperature, and etching solution consists of 5molL
-1HCl, saturated oxalic acid and 5gL
-1HF liquor capacity ratio is 1: 1: 1 a mixture, 20 minutes etch time, carries out pre-deposition palladium Catalytic Layer immediately after cleaning.
Adopt electrochemistry scanning method pre-deposition palladium Catalytic Layer, technology is for being supplementary anode with platinum, and mercurous chloride electrode is a reference electrode, and electrolytic solution is 1molL
-1H
2SO
4+ 0.3gL
-1PdCl
2(volume ratio 1: 1), scanning speed are 5 0mYs
-1, the scanning potential range be+0.3 to arrive-1.5V (vs SCE), and temperature is a room temperature, and depositing time 5 minutes obtains the palladium Catalytic Layer of black.
Titanium matrix through electrochemistry scanning pre-deposition palladium Catalytic Layer carries out electroplatinizing in platinum acid chloride solution: be anode with platinum, 90 ℃ consist of 3molL at electroplate liquid
-1HCl+20gL
-1H
2PtCl
26H
2In 1: 1 the mixed solution of the volume ratio of O, be 300Am with the current density
-2, electroplated 20 minutes, obtain that bonding force is good, the titanium base platinum electrode material of the bright densification of coating.
Embodiment 2
The pre-treating technology of titanium matrix is with embodiment 1, and pre-deposition palladium Catalytic Layer process using palladium plating technology is made supporting electrode with platinum, is consisting of 1molL
-1H
2SO
4+ 02gL
-1PdCl
2In the electroplate liquid of (volume ratio is 1: 1), under 50 ℃ the temperature of electroplating solution, the titanium matrix is with 500Am
-2Current density cathodic deposition palladium 8 minutes, obtain black palladium catalytic film; Press embodiment 1 technology Direct Electroplating platinum in platinum acid chloride solution again, obtain that bonding force is good, the titanium base platinum electrode material of the bright densification of coating.
Embodiment 3
The pre-treating technology of titanium matrix adopts the colloidal palladium activation method to carry out pre-deposition palladium Catalytic Layer and handles with embodiment 1, and the activation solution manner of formulation is: among the 20mlHCl, add the 0.7g sodium stannate under stirring, it is standby to stir the emulsion B liquid that obtains white.In another container, the 0.1g Palladous chloride is added in the mixed solution of 10mlHCl and 20ml deionized water again, after the heating for dissolving, add the 0.25g tin protochloride down, stir and get A liquid after 12 minutes at 30 ± 2 ℃.Under agitation A liquid is poured in the B liquid immediately then, be diluted to 100ml, obtain brown colloidal pd activation solution, be incubated 5h down at 60 ± 5 ℃ again with deionized water.Under room temperature, the titanium matrix is placed colloidal pd activation solution, activate 5 minutes, pass through the dilute hydrochloric acid solution dispergation again, obtain to have the titanium matrix that the surface is brown palladium Catalytic Layer, press embodiment 1 technology Direct Electroplating platinum in platinum acid chloride solution, the bright platinum coating that obtains, bonding force is good.
Embodiment 4～8
According to embodiment 1 technology the titanium matrix is carried out pre-treatment, with palladium plating method pre-deposition Catalytic Layer, Direct Electroplating platinum in embodiment 1 described platinum acid chloride solution changes electroplating temperature again, and the result who obtains is as shown in table 1;
Titanium matrix electroplatinizing in platinum acid chloride solution under table 1 differing temps
| Embodiment | Temperature (℃) | Current density (Am -2) | The coating outward appearance | Bonding force |
| 4 5 6 7 8 | 80 85 90 92 95 | 300 300 300 300 300 | Black, smooth, fine and close silvery white, smooth, fine and close silvery white, smooth, fine and close light is smooth, fine and close greyish white, smooth, densification | Better good better carefully |
Embodiment 9～14
According to embodiment 1 technology the titanium matrix is carried out pre-treatment, with palladium plating method pre-deposition Catalytic Layer, Direct Electroplating platinum in embodiment 1 described platinum acid chloride solution changes the current density that adopts again, and the result who obtains is as shown in table 2;
Titanium matrix Platinic chloride electroplatinizing under the different current densities of table 2
| Embodiment | Current density (Am -2) | Temperature (℃) | The coating outward appearance | Bonding force |
| 9 10 11 12 13 14 | 100 200 400 600 800 900 | 90 90 90 90 90 90 | Silvery white, smooth, fine and close light, smooth, fine and close light, smooth, fine and close light, smooth, fine and close silver color, smooth, fine and close black, densification | Better good better poor carefully |
Claims (10)
1. the technology of a titanium basal body electric plating platinum coating, comprise with the titanium matrix surface flatten, oil removing, removing oxide layer pre-treatment, it is characterized in that described technology also comprises carries out pre-deposition palladium Catalytic Layer art breading with treated titanium matrix, obtain the titanium matrix that the surface has catalytic activity, at last Direct Electroplating platinum in platinum acid chloride solution.
2. the technology of titanium basal body electric plating platinum coating as claimed in claim 1 is characterized in that described pre-deposition palladium Catalytic Layer technology is to adopt electrochemistry scanning method, palladium plating method or colloidal palladium activation method to carry out pre-deposition palladium Catalytic Layer.
3. the technology of titanium basal body electric plating platinum coating as claimed in claim 2, it is characterized in that described electrochemistry scanning method pre-deposition palladium Catalytic Layer technology is: be supplementary anode with platinum, mercurous chloride electrode (SCE) is a reference electrode, and electrolytic solution is that volume ratio is 0.1～6molL of 1: 1
-1H
2SO
4With 0.1～1.0gL
-1PdCl
2Mixed solution, be 1～500mVs with scanning speed under the room temperature
-1, current potential scanned depositing Pd 1～30 minute for+0.3 to-1.5V (vs SCE).
4. the technology of titanium basal body electric plating platinum coating as claimed in claim 2 is characterized in that described palladium plating method pre-deposition palladium Catalytic Layer technology is: make supporting electrode with platinum, at 0.1～12mo1L of 1: 1 composition of volume ratio
-1H
2SO
4With 0.1～1.0gL
-1PdCl
2Electroplate liquid in, under 10～90 ℃ the temperature of electroplating solution, with 10～1000Am
-2Current density, the cathodic deposition palladium is 1～30 minute on the titanium matrix.
5. the technology of titanium basal body electric plating platinum coating as claimed in claim 2, it is characterized in that described colloidal palladium activation method pre-deposition palladium Catalytic Layer technology is: with colloidal palladium solution activation titanium matrix, pass through the dilute hydrochloric acid solution dispergation again, on the titanium matrix, obtain the surface and be brown palladium Catalytic Layer.
6. the technology of titanium basal body electric plating platinum coating as claimed in claim 2, it is characterized in that Direct Electroplating platinum technology is in the described platinum acid chloride solution: be anode with platinum, will be through the titanium matrix of pre-deposition palladium Catalytic Layer, 85～95 ℃ are carried out electrolysis in platinum acid chloride solution, and electrolysis density is 100～1000Am
-2
7. the technology of titanium basal body electric plating platinum coating as claimed in claim 6 is characterized in that described platinum acid chloride solution is 1～12molL of 1: 1 of volume ratio
-1HCl and 1～50gL
-1H
2PtCl
26H
2The mixed solution of O solution.
8. as the technology of the described titanium basal body electric plating platinum coating of one of claim 1～7, it is characterized in that described titanium matrix surface pre-treating technology for to the leveling of titanium matrix surface, the sandblast of titanium matrix surface, at 50～80 ℃ of following alkaline degreasings, at room temperature place etching solution etch 1～30min again, described etching solution consists of 0.5～12molL
-1HCl, saturated oxalic acid and 1～10gL
-1The HF volume ratio is 1: 1: 1 a mixed solution.
9. the technology of titanium basal body electric plating platinum coating as claimed in claim 1, it is characterized in that described technology for the titanium matrix surface is flattened, sandblast, oil removing, etch, be supplementary anode then with platinum, mercurous chloride electrode is a reference electrode, and electrolytic solution is that volume ratio is 0.1～6m01L of 1: 1
-1H
2SO
4With 0.1～1.0gL
-1PdCl
2Mixed solution, be 1～500mVs with scanning speed under the room temperature
-1, current potential scanned depositing Pd 1～30 minute for+0.3 to-1.5V (vs SCE); Be 1～12molL of 1: 1 then in volume ratio
-1HCl and 1～50gL
-1H
2PtCl
26H
2In the mixing electroplate liquid of O, with 100～1000Am
-2The electrolysis of electrolysis density, promptly get titanium base platinum electrode.
10. the technology of titanium basal body electric plating platinum coating as claimed in claim 1, it is characterized in that described technology for the titanium matrix surface is flattened, sandblast, oil removing, etch, make supporting electrode with platinum then, the 0.1～12molL that forms at 1: 1 in volume ratio
-1H
2SO
4With 0.1～1.0gL
-1PdCl
2Electroplate liquid in, under 10～90 ℃ the temperature of electroplating solution, with 10～1000Am
-2Current density titanium substrate cathode deposition 1～30 minute, be 1～12molL of 1: 1 then in volume ratio
-1HCl and 1～50gL
-1H
2PtCl
26H
2In 0 the mixing electroplate liquid, with 100～600Am
-2The electrolysis of electrolysis density, promptly get titanium base platinum electrode.
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- 2006-12-29 CN CN 200610155616 patent/CN101016639A/en active Pending
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| CN104055595A (en) * | 2014-07-05 | 2014-09-24 | 南宁越洋科技有限公司 | Artificial dental implant suitable for immediate tooth extraction and implantation, restoration and stress |
| CN105112954A (en) * | 2015-09-21 | 2015-12-02 | 无锡清杨机械制造有限公司 | Platinum electroplating liquid of potassium platinum (IV) chloride and electroplating method of platinum electroplating liquid |
| CN105386094A (en) * | 2015-09-21 | 2016-03-09 | 无锡清杨机械制造有限公司 | Acid diamminebis(nitrito-n)-platinu electroplating solution of electroplated platinum and electroplating method of acid diamminebis(nitrito-n)-platinu electroplating solution |
| CN107400910A (en) * | 2017-06-01 | 2017-11-28 | 中国南方电网有限责任公司超高压输电公司贵阳局 | A kind of electroplating technology for improving high voltage direct current converter valve screening electrodes detecting probe surface finish |
| 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 |
| 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 |
| CN109087902A (en) * | 2018-08-15 | 2018-12-25 | 京东方科技集团股份有限公司 | A kind of Wiring structure and preparation method thereof, display device |
| US11650637B2 (en) | 2018-08-15 | 2023-05-16 | Boe Technology Group Co., Ltd. | Wiring structure, preparation method thereof, and display device |
| CN111185158A (en) * | 2020-02-26 | 2020-05-22 | 左娟 | Composite photoelectric catalytic material and preparation method thereof |
| CN112048744A (en) * | 2020-09-12 | 2020-12-08 | 陕西泰安诺新材料科技有限公司 | Process for improving platinum plating uniformity on surface of titanium substrate |
| CN112048744B (en) * | 2020-09-12 | 2023-03-31 | 陕西泰安诺新材料科技有限公司 | Process for improving platinum plating uniformity on surface of titanium substrate |
| CN113897648A (en) * | 2021-11-22 | 2022-01-07 | 东莞中探探针有限公司 | Connector terminal electroplating process |
| CN114016097A (en) * | 2021-11-26 | 2022-02-08 | 湖南兴弘新材料科技有限公司 | Platinum plating solution and preparation method and application thereof |
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Open date: 20070815 |