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CN101016639A - Process of titanium basal body electric plating platinum coating - Google Patents

Process of titanium basal body electric plating platinum coating Download PDF

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Publication number
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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platinum
electroplating
titanium substrate
palladium
solution
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黄辉
甘永平
张文魁
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Zhejiang University of Technology ZJUT
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Zhejiang University of Technology ZJUT
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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

A kind of technology of titanium basal body electric plating platinum coating
(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)

1.一种钛基体电镀铂镀层的工艺，包括将钛基体表面进行整平、除油、除氧化层前处理，其特征在于所述的工艺还包括将经处理的钛基体进行预沉积钯催化层工艺处理，得到表面具有催化活性的钛基体，最后在氯铂酸溶液中直接电镀铂。1. A process for electroplating a platinum coating on a titanium substrate, comprising leveling the surface of the titanium substrate, degreasing, and pre-treating the oxide layer, characterized in that the process also includes pre-depositing palladium catalysis on the treated titanium substrate Layer process treatment to obtain a titanium substrate with catalytic activity on the surface, and finally electroplating platinum directly in chloroplatinic acid solution. 2.如权利要求1所述的钛基体电镀铂镀层的工艺，其特征在于所述的预沉积钯催化层工艺为采用电化学扫描法、电镀钯法或胶体钯活化法进行预沉积钯催化层。2. the technique of titanium substrate electroplating platinum coating as claimed in claim 1 is characterized in that described pre-deposited palladium catalytic layer technology is to adopt electrochemical scanning method, electroplating palladium method or colloidal palladium activation method to carry out pre-deposited palladium catalytic layer . 3.如权利要求2所述的钛基体电镀铂镀层的工艺，其特征在于所述的电化学扫描法预沉积钯催化层工艺为：以铂为辅助阳极，甘汞电极(SCE)为参比电极，电解液为体积比为1∶1的0.1～6mol·L-1 H2SO4和0.1～1.0g·L-1 PdCl2的混合液，室温下以扫描速率为1～500mV·s-1、电位为+0.3到-1.5V(vs SCE)进行扫描沉积钯1～30分钟。3. the technique of titanium substrate electroplating platinum coating as claimed in claim 2 is characterized in that described electrochemical scanning method pre-deposition palladium catalytic layer technique is: take platinum as auxiliary anode, and calomel electrode (SCE) is reference Electrode, the electrolyte is a mixture of 0.1~6mol·L -1 H 2 SO 4 and 0.1~1.0g·L -1 PdCl 2 with a volume ratio of 1:1, at room temperature with a scan rate of 1~500mV·s - 1. The potential is +0.3 to -1.5V (vs SCE) to scan and deposit palladium for 1 to 30 minutes. 4.如权利要求2所述的钛基体电镀铂镀层的工艺，其特征在于所述的电镀钯法预沉积钯催化层工艺为：以铂作辅助电极，在体积比1∶1组成的0.1～12mo1·L-1 H2SO4和0.1～1.0g·L-1PdCl2的电镀液中，10～90℃的电镀液温度下，以10～1000A·m-2的电流密度，于钛基体上阴极沉积钯1～30分钟。4. the technique of titanium substrate electroplating platinum coating as claimed in claim 2 is characterized in that described electroplating palladium method pre-deposited palladium catalytic layer technique is: make auxiliary electrode with platinum, in volume ratio 1: 1 composition 0.1～ In the electroplating solution of 12mo1·L -1 H 2 SO 4 and 0.1～1.0g·L -1 PdCl 2 , at the temperature of the electroplating solution of 10～90℃, with the current density of 10～1000A·m -2 , on the titanium substrate Palladium is deposited on the upper cathode for 1 to 30 minutes. 5.如权利要求2所述的钛基体电镀铂镀层的工艺，其特征在于所述的胶体钯活化法预沉积钯催化层工艺为：以胶体钯溶液活化钛基体，再经过稀盐酸溶液解胶，在钛基体上获得表面呈棕色的钯催化层。5. the technique of electroplating platinum coating on titanium substrate as claimed in claim 2, it is characterized in that described colloidal palladium activation method pre-deposition palladium catalyst layer process is: activate titanium substrate with colloidal palladium solution, then degel through dilute hydrochloric acid solution , a palladium catalytic layer with a brown surface was obtained on the titanium substrate. 6.如权利要求2所述的钛基体电镀铂镀层的工艺，其特征在于所述的氯铂酸溶液中直接电镀铂工艺为：以铂为阳极，将经过预沉积钯催化层的钛基体，在氯铂酸溶液中85～95℃进行电解，电解密度为100～1000A·m-2。6. the technique of titanium substrate electroplating platinum coating as claimed in claim 2 is characterized in that in the described chloroplatinic acid solution, direct electroplating platinum process is: take platinum as anode, will pass through the titanium substrate of pre-deposited palladium catalytic layer, The electrolysis is carried out in chloroplatinic acid solution at 85-95°C, and the electrolysis density is 100-1000A·m -2 . 7.如权利要求6所述的钛基体电镀铂镀层的工艺，其特征在于所述的氯铂酸溶液为体积比1∶1的1～12mol·L-1 HCl和1～50g·L-1H2PtCl2·6H2O溶液的混合液。7. The process of electroplating a platinum coating on a titanium substrate as claimed in claim 6, characterized in that the chloroplatinic acid solution is 1 to 12mol L -1 HCl and 1 to 50g L-1 with a volume ratio of 1: 1 The mixture of H 2 PtCl 2 ·6H 2 O solution. 8.如权利要求1～7之一所述的钛基体电镀铂镀层的工艺，其特征在于所述的钛基体表面前处理工艺为对钛基体表面整平、钛基体表面喷砂、在50～80℃下碱性除油、再在室温下置于浸蚀液中浸蚀1～30min，所述浸蚀液组成为0.5～12mol·L-1 HCl、饱和草酸和1～10g·L-1HF体积比为1∶1∶1的混合液。8. The process of electroplating a platinum coating on a titanium substrate as claimed in any one of claims 1 to 7, characterized in that the surface pretreatment process of the titanium substrate is to level the surface of the titanium substrate, sandblast the surface of the titanium substrate, and Alkaline degreasing at 80°C, and then etched in an etching solution for 1 to 30 minutes at room temperature. The composition of the etching solution is 0.5 to 12mol·L -1 HCl, saturated oxalic acid and HF volume ratio of 1:1:1 mixture. 9.如权利要求1所述的钛基体电镀铂镀层的工艺，其特征在于所述的工艺为对钛基体表面进行整平、喷砂、除油、浸蚀，然后以铂为辅助阳极，甘汞电极为参比电极，电解液为体积比为1∶1的0.1～6m01·L-1 H2SO4和0.1～1.0g·L-1 PdCl2的混合液，室温下以扫描速率为1～500mV·s-1、电位为+0.3到-1.5V(vs SCE)进行扫描沉积钯1～30分钟；然后在体积比为1∶1的1～12mol·L-1 HCl与1～50g·L-1 H2PtCl2·6H2O的混合电镀液中，以100～1000A·m-2的电解密度电解，即得钛基铂电极。9. the technique of electroplating platinum coating on titanium substrate as claimed in claim 1 is characterized in that described technology is to carry out leveling, sand blasting, degreasing, etching to the surface of titanium substrate, then take platinum as auxiliary anode, Gan The mercury electrode is the reference electrode, and the electrolyte is a mixture of 0.1~6m01·L -1 H 2 SO 4 and 0.1~1.0g·L -1 PdCl 2 with a volume ratio of 1:1. ~500mV·s -1 , the potential is +0.3 to -1.5V (vs SCE) for scanning deposition of palladium for 1 ~ 30 minutes; In the mixed electroplating solution of L -1 H 2 PtCl 2 ·6H 2 O, electrolyze with the electrolytic density of 100～1000A·m -2 to obtain the titanium-based platinum electrode. 10.如权利要求1所述的钛基体电镀铂镀层的工艺，其特征在于所述的工艺为对钛基体表面进行整平、喷砂、除油、浸蚀，然后以铂作辅助电极，在体积比1∶1组成的0.1～12mol·L-1 H2SO4和0.1～1.0g·L-1PdCl2的电镀液中，10～90℃的电镀液温度下，以10～1000A·m-2的电流密度钛基体阴极沉积1～30分钟，然后在体积比为1∶1的1～12mol·L-1 HCl与1～50g·L-1 H2PtCl2·6H20的混合电镀液中，以100～600A·m-2的电解密度电解，即得钛基铂电极。10. The process of electroplating a platinum coating on a titanium substrate as claimed in claim 1, characterized in that the process is to level the surface of the titanium substrate, sandblast, degrease, etch, then use platinum as an auxiliary electrode, and then use platinum as an auxiliary electrode. In the electroplating solution composed of 0.1～12mol·L -1 H 2 SO 4 and 0.1～1.0g·L -1 PdCl 2 with a volume ratio of 1:1, at the temperature of the electroplating solution of 10～90℃, at 10～1000A·m Cathodic deposition of titanium substrate at a current density of -2 for 1 to 30 minutes, and then mixed electroplating with 1 to 12mol·L -1 HCl and 1 to 50g·L -1 H 2 PtCl 2 ·6H 2 0 at a volume ratio of 1:1 solution, electrolysis at an electrolytic density of 100-600A·m -2 to obtain a titanium-based platinum electrode.
CN 200610155616 2006-12-29 2006-12-29 Process of titanium basal body electric plating platinum coating Pending CN101016639A (en)

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CN101831666A (en) * 2010-05-28 2010-09-15 上海交通大学 Preparation method of nickel-based or titanium-based catalytic electrode for electrically catalyzing ammonia oxides
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
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