CN102220582A - Platinum-plated titanium palladium alloy plate and preparation method thereof - Google Patents
Platinum-plated titanium palladium alloy plate and preparation method thereof Download PDFInfo
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- CN102220582A CN102220582A CN2010101472410A CN201010147241A CN102220582A CN 102220582 A CN102220582 A CN 102220582A CN 2010101472410 A CN2010101472410 A CN 2010101472410A CN 201010147241 A CN201010147241 A CN 201010147241A CN 102220582 A CN102220582 A CN 102220582A
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Abstract
The invention discloses a platinum-plated titanium palladium alloy plate and a preparation method thereof, which belong to the technical field of preparation of corrosion resistant electrode. The preparation method comprises: plating a nickel layer on the surface of the titanium palladium alloy plate and plating platinum, wherein the thickness of the titanium palladium alloy plate is 2 to 3 millimeters, the thickness of the nickel layer is 1 to 1.5 micrometers, and the thickness of the platinum plating is 5 to 8 micrometers; and subjecting the titanium palladium alloy plate to sand blast, oil removal and oxide film removal treatment to remove oil stains and oxide films on surface, plating nickel by using a chemical nickel plating process, placing in clean water for washing after nickel plating, plating platinum by using a platinum plating process, placing in clean water for washing after platinum plating, and placing in a vacuum heat treatment furnace in protection of argon to perform heat treatment. In the invention, the thickness of the platinum plating of the platinum-plated titanium palladium alloy plate is 5 to 8 micrometers, a thick platinum layer is plated on the titanium palladium alloy plate, the bonding force between the titanium palladium alloy plate substrate and the platinum plating is 22 to 28MPa, the surface state is observed by a scanning electron microscope, and according to result of observation after amplification by 2,500 times, the platinum plating has no needle holes.
Description
Technical field
The invention belongs to the corrosion-resistant electrode preparing technical field, particularly a kind of platinized titanium palldium alloy plate and preparation method thereof.
Background technology
In material surface modifying was handled, the electrochemical surface processing treatment was a kind of technology commonly used, as adopting electrolysis or electro-plating method, made material surface form special functional coating, to satisfy its service requirements.The material that in corrosive medium, uses, perhaps as electrolysis or galvanized insoluble anode (dimensional stabilizing electrode, DSA) material generally will use inert material or corrosion-resistant strong material, as graphite, corrosion resisting stainless steel, lead alloy, nickelalloy, titanium and titanium alloy etc.Noble coatings (gold, platinum and rhodium etc.) material has superior corrosion resistance, is widely used in contact material and metallide anode.Electrolysis/plating generally is to use in acidity or basic solution, solution corrosion is strong, electrode itself will have good electrochemical catalysis reactive behavior and conductivity, require electrode will have superior corrosion resistance and stability simultaneously, when guaranteeing electrolysis and Electroplating Production quality, reduce the energy consumption of electrochemical reaction process as far as possible.
Titanium palldium alloy (Ti-0.2%Pd) to cause blunt current potential more negative, the surface 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.The titanium palldium alloy has superior corrosion resistance in many media (as acid, neutrality, week reduction and Oxidant etc.), have good performances such as anti-spot corrosion, crevice corrosion, intergranular corrosion, abrasion, fatigue corrosion and stress corrosion.
Titanium palldium alloy surface-coated platinum can be used as electrolysis or galvanic anode, and kind electrode can keep good electrochemical catalysis reactive behavior and electroconductibility, has very strong erosion resistance and stability again.Even use in strong acid solution, still have good solidity to corrosion.If make titanium palldium alloy and platinum coating mortise, platinum coating is fine and close and have a certain thickness, such platinum coated electrode has good electrochemical catalysis activity, electroconductibility and stability in electrochemistry Working environment (electrolysis, electrophoresis, electric osmose and plating etc.), can satisfy the needs of high-voltage, big electric current and long-time steady operation.
Summary of the invention
The purpose of this invention is to provide a kind of platinized titanium palldium alloy plate and preparation method thereof.
A kind of platinized titanium palldium alloy plate is characterized in that, is matrix with titanium palldium alloy plate, electroplates platinum layer behind the titanium palldium alloy plate plating nickel on surface layer, and titanium palldium alloy plate thickness is 2～3mm, and nickel layer thickness is 1～1.5 μ m, and the platinum thickness of coating is 5～8 μ m.
Bonding force between titanium palldium alloy board substrate and the platinum coating is 22～28MPa.
Weight percent 〉=99.9% of platinum in the described platinum coating.
A kind of preparation method of platinized titanium palldium alloy plate is characterized in that, this method steps is as follows:
(1) titanium palldium alloy plate is shaped: choosing thickness is the titanium palldium alloy plate of 2～3mm, and cutting;
(2) titanium palldium alloy plate surface treatment: after the sandblasting of titanium palldium alloy plate, oil removing is also removed oxide film;
(3) chemical nickel plating: surface treated titanium palldium alloy plate carries out chemical nickel plating, and nickel layer thickness is 1～1.5 μ m, puts into clear water after the nickel plating and cleans;
(4) electroplatinizing: with the titanium palldium alloy plate behind the chemical nickel plating of step (3) is negative electrode, electroplates the platinum of a bed thickness 5～8 μ m thereon, puts into clear water after the platinum plating and cleans;
(5) thermal treatment: place the vacuum heat treatment furnace of argon shield to carry out, thermal treatment temp is 500 ℃, and the time is 2.5 hours, and furnace cooling gets platinized titanium palldium alloy plate.
The described chemical nickel-plating plating solution of step (3) consists of: NiSO
47H
2O:40g/L, NaH
2PO
2H
2O:20g/L, NH
4Cl:40g/L, Na
3C
6H
5O
72H
2O, 80g/L, plating bath pH are 9.0, temperature: 85～90 ℃, the electroless plating time is 8～15 minutes.
The described electroplatinizing of step (4) is an anode with the platinum guaze, and the control cathode current density is 2A/dm during plating
2, cathode and anode spacing 0.5～1cm, bath voltage 2.6～3.5V, electroplate liquid pH value 9～12,90～95 ℃ of temperature, electroplating time 5～60 hours.
Described electroplate liquid consists of: P salt [(NH
3)
2Pt (NO
2)
22H
2O]: 25g/L, ammonium nitrate (NH
4NO
3): 100g/L, Sodium Nitrite (NaNO
2): 10g/L, ammonium hydroxide (NH
4OH): 55g/L, sodium laurylsulfonate: 0.02g/L, asccharin: 0.02g/L, 1,4-butynediol: 0.05g/L.
Press the thick titanium palldium alloy plate of certain size cutting 2～3mm; handle through sandblast, oil removing and oxide film dissolving; remove surface and oil contaminant and oxide film; adopt above-mentioned nickel chemical plating technology nickel plating; putting into clear water after the nickel plating cleans; by the platinum plating of above-mentioned electroplatinizing technology, put into clear water after the platinum plating and clean then, place the vacuum heat treatment furnace of argon shield to heat-treat.After thermal treatment finishes, with the thickness of thickness tester measurement platinum coating, measure binding force of cladding material, with the condition of surface of scanning electron microscopic observation platinum coating with stretching method.
Beneficial effect of the present invention is: platinized titanium palldium alloy plate thickness of the present invention is 2～3mm, matrix titanium palldium alloy plate thickness is 2～3mm, the platinum thickness of coating is 5～8 μ m, on titanium palldium alloy plate, electroplated a bed thickness platinum layer, bonding force between titanium palldium alloy board substrate and the platinum coating is 22～28MPa, use the scanning electron microscopic observation condition of surface, amplify and observe free of pinholes more than 2500 times.Made platinized titanium palldium alloy plate can be used as corrosion-resistant electrode as electrolysis or galvanic anode, is specially adapted to electrolysis and plating in the nuclear industry.
Embodiment
The invention will be further described below in conjunction with embodiment:
Embodiment 1
A kind of platinized titanium palldium alloy plate is a matrix with titanium palldium alloy plate, electroplates platinum layer behind the titanium palldium alloy plate plating nickel on surface layer, and titanium palldium alloy plate thickness is 2.5mm, and nickel layer thickness is 1.1 μ m, and the platinum thickness of coating is 5.8 μ m.Weight percent 〉=99.9% of described platinum coating platinum.
The preparation method of above-mentioned platinized titanium palldium alloy plate is characterized in that, this method steps is as follows:
(1) titanium palldium alloy plate is shaped: choosing thickness is the titanium palldium alloy plate of 2.5mm, and by long 150mm, wide 150mm carries out cutting;
(2) titanium palldium alloy plate surface treatment: after the sandblasting of titanium palldium alloy plate, oil removing is also removed oxide film; Specific as follows:
Sandblast: remove machining marks by sandblasting, increase roughness, obtain the surface of comparatively fresh, help improving the bonding force of coating;
Oil removing: remove the greasy dirt on titanium palldium alloy plate surface, adopt ultrasonic cleaning and matting to remove surface and oil contaminant, matting employing massfraction is 40% NaOH heat alkali liquid cleaning, and cleaning temperature is 50 ℃;
Oxide film dissolving: the 10%HF-20%HCl (the hydrofluoric acid massfraction is 10% in the mixed acid solution, and the hydrochloric acid massfraction is 20%) and the 10%HF-20%HNO that adopt heat
3(the hydrofluoric acid massfraction is 10% in the mixed acid solution, and the nitric acid massfraction is 20%) two kinds of mixed acid solutions are the etch substrate respectively, removes the oxide film of substrate surface;
(3) chemical nickel plating: surface treated titanium palldium alloy plate carries out chemical nickel plating, and nickel layer thickness is 1～1.5 μ m; Chemical nickel-plating plating solution consists of: NiSO
47H
2O:40g/L, NaH
2PO
2H
2O:20g/L, NH
4Cl:40g/L, Na
3C
6H
5O
72H
2O, 80g/L, plating bath pH are 9.0, temperature: 85～90 ℃, the electroless plating time is 8 minutes; The chemical nickel plating purpose is to prevent that titanium palldium alloy unsalted surface from forming blocked up oxide passivation film before plating, and electroplatinizing is carried out smoothly, and platinum guarantees that at titanium palldium alloy surface uniform deposition platinum binding force of cladding material and density are qualified;
(4) electroplatinizing: clean with clear water after the nickel plating, electroplate the platinum of a bed thickness 5～8 μ m thereon; With the titanium palldium alloy plate behind the chemical nickel plating of step (3) is negative electrode, is anode with the platinum guaze, and the control cathode current density is 2A/dm during plating
2, cathode and anode spacing 0.5～1cm, bath voltage 2.6～3.5V, electroplate liquid pH value 9～12,90～95 ℃ of temperature, electroplating time 36 hours;
Described electroplate liquid consists of: P salt [(NH
3)
2Pt (NO
2)
22H
2O]: 25g/L, ammonium nitrate (NH
4NO
3): 100g/L, Sodium Nitrite (NaNO
2): 10g/L, ammonium hydroxide (NH
4OH, massfraction are 25%): 55g/L, sodium laurylsulfonate: 0.02g/L, asccharin: 0.02g/L, 1,4-butynediol: 0.05g/L;
Adopt continuous current platinum plating technology, anode uses power supply to adopt and electroplates power source special, electroplate liquid is realized circulating by filtration pump, electrolyzer places constant temperature water bath to electroplate to realize constant temperature, in electroplate liquid, added special additive of joining during plating, comprise the moistened surface agent, electroplate leveling agent and brightening agent, these additives evenly are adsorbed on the negative electrode (titanium palldium alloy plate), make platinum ion uniform deposition in the electroplate liquid on negative electrode, form fine and closely woven crystallization, thereby guarantee that coating is even, densification, tight with matrix bond, firmly, make the heatproof of coating, wear-resisting, welding, toughness, anticorrosion, electric conductivity, performance index such as smooth finish are improved;
(5) thermal treatment: thermal treatment is carried out in the vacuum heat treatment furnace of argon shield is arranged, and thermal treatment temp is 500 ℃, and the time is 2.5 hours, and furnace cooling gets platinized titanium palldium alloy plate; Thermal treatment can make the bonding force between titanium palldium alloy plate and the platinum coating reliably be guaranteed.
After thermal treatment finished, the thickness of measuring platinum coating with thickness tester was 5.8 μ m, and the bonding force of measuring between titanium palldium alloy board substrate and the platinum coating with stretching method is 26.8MPa, with scanning electron microscopic observation platinum coating surface state, amplified 2500 times of observations and did not find pin hole.
Embodiment 2
A kind of platinized titanium palldium alloy plate is a matrix with titanium palldium alloy plate, electroplates platinum layer behind the titanium palldium alloy plate plating nickel on surface layer, and titanium palldium alloy plate thickness is 3mm, and nickel layer thickness is 1.1 μ m, and the platinum thickness of coating is 6.6 μ m.Weight percent 〉=99.9% of described platinum coating platinum.
The preparation method: except titanium palldium alloy plate thickness is 3mm, by long 150mm, wide 150mm carries out cutting; Electroplate outside 48 hours in the electroplatinizing step, other are identical with embodiment 1.
After thermal treatment finishes, the thickness of measuring platinum coating with thickness tester is 6.6 μ m, and the bonding force of measuring between titanium palldium alloy board substrate and the platinum coating with stretching method is 25.6MPa, with scanning electron microscopic observation platinum coating surface state, amplify 3000 times of observations, do not find pin hole.
Embodiment 3
A kind of platinized titanium palldium alloy plate is a matrix with titanium palldium alloy plate, electroplates platinum layer behind the titanium palldium alloy plate plating nickel on surface layer, and titanium palldium alloy plate thickness is 2mm, and nickel layer thickness is 1.1 μ m, and the platinum thickness of coating is 7.3 μ m.Weight percent 〉=99.9% of described platinum coating platinum.
The preparation method: except titanium palldium alloy plate thickness is 2mm, by long 200mm, wide 200mm carries out cutting; Electroplate outside 56 hours in the electroplatinizing step, other are identical with embodiment 1.
After thermal treatment finishes, the thickness of measuring platinum coating with thickness tester is 7.3 μ m, and the bonding force of measuring between titanium palldium alloy board substrate and the platinum coating with stretching method is 24.5MPa, with scanning electron microscopic observation platinum coating surface state, amplify 3000 times of observations, do not find pin hole.
Claims (7)
1. a platinized titanium palldium alloy plate is characterized in that, is matrix with titanium palldium alloy plate, electroplates platinum layer behind the titanium palldium alloy plate plating nickel on surface layer, and titanium palldium alloy plate thickness is 2～3mm, and nickel layer thickness is 1～1.5 μ m, and the platinum thickness of coating is 5～8 μ m.
2. a kind of platinized titanium palldium alloy plate according to claim 1 is characterized in that the bonding force between titanium palldium alloy board substrate and the platinum coating is 22～28MPa.
3. a kind of platinized titanium palldium alloy plate according to claim 1 and 2 is characterized in that weight percent 〉=99.9% of platinum in the described platinum coating.
4. the preparation method of a platinized titanium palldium alloy plate is characterized in that, this method steps is as follows:
(1) titanium palldium alloy plate is shaped: choosing thickness is the titanium palldium alloy plate of 2～3mm, and cutting;
(2) titanium palldium alloy plate surface treatment: after the sandblasting of titanium palldium alloy plate, oil removing is also removed oxide film;
(3) chemical nickel plating: surface treated titanium palldium alloy plate carries out chemical nickel plating, and nickel layer thickness is 1～1.5 μ m, puts into clear water after the nickel plating and cleans;
(4) electroplatinizing: with the titanium palldium alloy plate behind the chemical nickel plating of step (3) is negative electrode, electroplates the platinum of a bed thickness 5～8 μ m thereon, puts into clear water after the platinum plating and cleans;
(5) thermal treatment: place the vacuum heat treatment furnace of argon shield to carry out, thermal treatment temp is 500 ℃, and the time is 2.5 hours, and furnace cooling gets platinized titanium palldium alloy plate.
5. the preparation method of a kind of platinized titanium palldium alloy plate according to claim 4 is characterized in that, the described chemical nickel-plating plating solution of step (3) consists of: NiSO
47H
2O:40g/L, NaH
2PO
2H
2O:20g/L, NH
4Cl:40g/L, Na
3C
6H
5O
72H
2O, 80g/L, plating bath pH are 9.0, temperature: 85～90 ℃, the electroless plating time is 8～15 minutes.
6. the preparation method of a kind of platinized titanium palldium alloy plate according to claim 4 is characterized in that, the described electroplatinizing of step (4) is an anode with the platinum guaze, and the control cathode current density is 2A/dm during plating
2, cathode and anode spacing 0.5～1cm, bath voltage 2.6～3.5V, electroplate liquid pH value 9～12,90～95 ℃ of temperature, electroplating time 5～60 hours.
7. the preparation method of a kind of platinized titanium palldium alloy plate according to claim 4 is characterized in that, described electroplate liquid consists of: P salt [(NH
3)
2Pt (NO
2)
22H
2O]: 25g/L, ammonium nitrate (NH
4NO
3): 100g/L, Sodium Nitrite (NaNO
2): 10g/L, ammonium hydroxide (NH
4OH): 55g/L, sodium laurylsulfonate: 0.02g/L, asccharin: 0.02g/L, 1,4-butynediol: 0.05g/L.
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| CN105112956A (en) * | 2015-09-21 | 2015-12-02 | 无锡清杨机械制造有限公司 | Acidic dinitrodiammineplatinum ammoniacal plating solution and plating method of Pt |
| CN105132963A (en) * | 2015-09-21 | 2015-12-09 | 无锡清杨机械制造有限公司 | Alkaline P salt plating solution for electroplating platinum and electroplating method thereof |
| CN105386095A (en) * | 2015-09-21 | 2016-03-09 | 无锡清杨机械制造有限公司 | Alkaline platinum plating P salt electroplating bath and electroplating method thereof |
| CN105386093A (en) * | 2015-09-21 | 2016-03-09 | 无锡清杨机械制造有限公司 | Pt alkaline P salt electroplating bath and electroplating method thereof |
| CN105386092A (en) * | 2015-09-21 | 2016-03-09 | 无锡清杨机械制造有限公司 | Barium-salt-contained alkaline plating Pt P salt electroplating bath and electroplating method thereof |
| CN105886983A (en) * | 2016-06-01 | 2016-08-24 | 洛阳双瑞精铸钛业有限公司 | Roll type production method of titanium and palladium alloy |
| CN108130566A (en) * | 2018-01-31 | 2018-06-08 | 西北有色金属研究院 | For the electroplate liquid and its electro-plating method of nickel base superalloy electroplating surface platinum layer |
| CN113514528A (en) * | 2021-03-10 | 2021-10-19 | 首钢集团有限公司 | Method for measuring compactness of hot-dip galvanized sheet inhibition layer |
| CN113897648A (en) * | 2021-11-22 | 2022-01-07 | 东莞中探探针有限公司 | Connector terminal electroplating process |
| CN114134545A (en) * | 2021-10-21 | 2022-03-04 | 中国科学院金属研究所 | Plating solution for electroplating platinum on bright metal surface and electroplating method thereof |
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| CN105112956A (en) * | 2015-09-21 | 2015-12-02 | 无锡清杨机械制造有限公司 | Acidic dinitrodiammineplatinum ammoniacal plating solution and plating method of Pt |
| CN105132963A (en) * | 2015-09-21 | 2015-12-09 | 无锡清杨机械制造有限公司 | Alkaline P salt plating solution for electroplating platinum and electroplating method thereof |
| CN105386095A (en) * | 2015-09-21 | 2016-03-09 | 无锡清杨机械制造有限公司 | Alkaline platinum plating P salt electroplating bath and electroplating method thereof |
| CN105386093A (en) * | 2015-09-21 | 2016-03-09 | 无锡清杨机械制造有限公司 | Pt alkaline P salt electroplating bath and electroplating method thereof |
| CN105386092A (en) * | 2015-09-21 | 2016-03-09 | 无锡清杨机械制造有限公司 | Barium-salt-contained alkaline plating Pt P salt electroplating bath and electroplating method thereof |
| CN105886983A (en) * | 2016-06-01 | 2016-08-24 | 洛阳双瑞精铸钛业有限公司 | Roll type production method of titanium and palladium alloy |
| CN108130566A (en) * | 2018-01-31 | 2018-06-08 | 西北有色金属研究院 | For the electroplate liquid and its electro-plating method of nickel base superalloy electroplating surface platinum layer |
| CN108130566B (en) * | 2018-01-31 | 2019-08-27 | 西北有色金属研究院 | Electroplate liquid and its electro-plating method for nickel base superalloy electroplating surface platinum layer |
| CN113514528A (en) * | 2021-03-10 | 2021-10-19 | 首钢集团有限公司 | Method for measuring compactness of hot-dip galvanized sheet inhibition layer |
| CN114134545A (en) * | 2021-10-21 | 2022-03-04 | 中国科学院金属研究所 | Plating solution for electroplating platinum on bright metal surface and electroplating method thereof |
| CN113897648A (en) * | 2021-11-22 | 2022-01-07 | 东莞中探探针有限公司 | Connector terminal electroplating process |
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Application publication date: 20111019 |