CN103014793A - Method for preparing titanium carbide coating through pulse electrodeposition - Google Patents
Method for preparing titanium carbide coating through pulse electrodeposition Download PDFInfo
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- CN103014793A CN103014793A CN2012105359280A CN201210535928A CN103014793A CN 103014793 A CN103014793 A CN 103014793A CN 2012105359280 A CN2012105359280 A CN 2012105359280A CN 201210535928 A CN201210535928 A CN 201210535928A CN 103014793 A CN103014793 A CN 103014793A
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- titanium carbide
- carbide coating
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- pulse electrodeposition
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Abstract
The invention discloses a method for preparing a titanium carbide coating through pulse electrodeposition. The method comprises the following steps: through taking a substrate as a cathode, taking graphite as an anode and a carbon source and taking nickel as a reference electrode, melting a titanium source into a salt mixture; reacting for 0.5-2h under the protection of inert gas, at a temperature of 800-950 DEG C and under a pulse voltage of 2.5-3V, thus forming a titanium carbide coating on the substrate. According to the invention, deposition is performed by using a molten salt electro-deposition method without use of large equipment and precious materials, therefore, the method is low in cost and simple in operation; and in the reaction process, no harmful gas is required, and no harmful substance is produced, therefore, the method is environment-friendly; and a titanium carbide coating prepared by using the method disclosed by the invention is dense and good in performances.
Description
Technical field
The invention belongs to technical field of surface, particularly relate to the method that a kind of pulse electrodeposition prepares titanium carbide coating.
Background technology
Therefore the transition group carbide is called as refractory carbide owing to have very high fusing point.The titanium carbide conduct is one of most important refractory carbide wherein, has the advantages such as high-melting-point (3067 ℃), high-modulus (410-450GPa), high rigidity (28-35GPa) and good chemical stability.Therefore be widely used in cutting tool and industrial wear parts etc.Titanium carbide has low chemically reactive, so lower of room temperature is contained concentrated acid and the concentrated base corrosion of oxygenant, at high temperature still has good solidity to corrosion.The industrial the most frequently used method for preparing titanium carbide coating has chemical vapour deposition, physical vapor deposition and thermospray.Physical vapor deposition is lower than the used depositing temperature of chemical vapour deposition, but just because of low base material and the coating layering of causing of temperature, reduces adhesivity.Thermospray can prepare thicker titanium carbide coating, yet porosity is high.In addition, also useful titanium valve as reagent fused salt synthesizing titanium carbide.
The molten salt electrochemistry method also is used to prepare some carbide coatings such as TaC, NbC, WC, SiC etc.In these researchs, the required carbon source of electrosynthesis carbide is carbonate.With respect to other refractory carbide, the electrolytic synthesis of titanium carbide is much more difficult, and its reason is that the titanium source is (such as K
2TiF
6) product that easily is difficult to be reduced with carbonate reaction formation is (such as K
2TiO
3).
Summary of the invention
Based on this, the purpose of this invention is to provide the method that a kind of pulse electrodeposition prepares titanium carbide coating.
Concrete technical scheme is as follows:
A kind of pulse electrodeposition prepares the method for titanium carbide coating; comprise the steps: take substrate as negative electrode; graphite is anode and carbon source; nickel is reference electrode; the titanium source is melted in the mixing salt, and reaction conditions is: in protection of inert gas, and 800-950 ℃; 2.5-3V react 0.5-2h under the pulse potential, namely generate one deck titanium carbide coating at substrate.
Among some embodiment, described titanium source is K therein
2TiF
6
Therein among some embodiment, described mixing salt composition and molar content be: 40-41%NaCl, 50-51%KCl and 9-10%NaF.
Therein among some embodiment, described mixing salt composition and molar content be: 40.25%NaCl, 50.5%KCl and 9.25%NaF.
Among some embodiment, the weight percentage of described titanium source in mixing salt is 5-10% therein.
Among some embodiment, the weight percentage of described titanium source in mixing salt is 7% therein.
Among some embodiment, described reaction conditions is therein: 900 ℃, react 1h under the 2.8V pulse potential.
Among some embodiment, depositing time is 2-4:1 with the stand-by time ratio in the described pulse potential therein.
Among some embodiment, the thickness of described titanium carbide coating is 0.5-1 μ m therein.
Among some embodiment, described substrate is stainless steel plate therein.
Principle of the present invention: relate to three processes in stainless steel surface electrochemical synthesis TiC coating, namely as the K in titanium source
2TiF
6Be reduced into Ti, produce C and Ti and C reaction formation TiC.Ti (K
2TiF
6) electro-reduction process in molten fluoride or fluorochemical-muriate comprises following two steps:
Ti
4++e=Ti
3+ (1)
Ti
3++3e=Ti (2)
In reduction process, do not observe and relate to Ti
2+Intermediate reaction.Carbanion is often used as the carbon source of fused salt galvanic deposit carbide.In the present invention, owing to do not have carbonate in the fused salt, therefore forming the required carbon source of titanium carbide can only be from graphite anode.Experimental result shows that graphite anode has suffered comparatively serious corrosion in the pulse electrodeposition process, and obviously, graphite can form some carbonaceous products with molten salt react ion in this process.These carbonaceous products are reduced into carbon at stainless steel surface, and form titanium carbide with the titanium reaction.
Beneficial effect of the present invention:
The industrial the most frequently used method of carbide coating for preparing has chemical vapour deposition, physical vapor deposition and thermospray.Physical vapor deposition can carry out under the condition more much lower than chemical vapour deposition temperature, but lower substrate temperature also may cause the bonding force of coating and matrix to descend; Thermospray can prepare thicker carbide coating, but coating porosity is high.The present invention adopts the method for fused salt galvanic deposit to deposit, and does not need main equipment and precious materials, and is with low cost, simple to operate.Without the need for evil gas, do not produce objectionable impurities, so present method is environmentally friendly in the reaction process yet.Fine and close with the titanium carbide coating that present method obtains, performance is good.
Description of drawings
Fig. 1 is the XRD figure (1 is titanium carbide, and 2 is stainless steel substrate) of the titanium carbide coating for preparing of pulse electrodeposition of the present invention;
Fig. 2 is the surface topography of the titanium carbide coating for preparing of pulse electrodeposition of the present invention.
Embodiment
By the following examples the present invention is further elaborated.
The method that the present embodiment pulse electrodeposition prepares titanium carbide coating is as follows:
Adopt the line cutting that 304 stainless steel materials lines are cut into the sheet sample, and through grinding, cleaning and drying treatment.The end that the Fe-Cr silk is spot welded to sample is as contact conductor, and three-electrode system is adopted in galvanic deposit, and namely take the stainless steel plate sample as negative electrode, Graphite Electrodes is supporting electrode and carbon source (anode), and nickel electrode is reference electrode.With K
2TiF
6Be the titanium source, take ternary eutectic (mixing salt) 40.25mol%NaCl-50.5mol%KCl--9.25mol%NaF salt as active substance K
2TiF
6Solvent, K
2TiF
6Content in solvent is 7wt%.The above-mentioned mixing salt for preparing and titanium source are put into alumina crucible, under the protection of argon gas, be warmed up to 900 ℃.Adopt the PAR2273 electrochemical workstation to carry out the constant potential pulsed deposition.The applying pulse current potential is 2.8V, deposits 2.4 seconds and stops 0.6 second afterwards, and total pulsed deposition time is 1 hour, is the titanium carbide coating of 0.8 μ m in stainless steel plate deposition a layer thickness namely.
The XRD figure of described titanium carbide coating and surface topography map are referring to Fig. 1 and Fig. 2.
Can find out that from Fig. 1, Fig. 2 pulse electrodeposition method of the present invention is continuously fine and close at the titanium carbide coating that stainless steel base prepares, good with the combination of stainless steel base.
Titanium carbide is a kind of high-hardness ceramic material, has excellent wear resisting property and chemical stability in room temperature environment.Titanium carbide has low chemically reactive, so can only be contained concentrated acid and the concentrated base corrosion of oxygenant under the room temperature, at high temperature still has good solidity to corrosion, and the prospect that is widely used is such as cutting tool, industrial wear parts and electrode materials etc.
Stainless steel is used to the bipolar plates of Proton Exchange Membrane Fuel Cells owing to the advantage with high strength, low cost, excellent machinability, good ductility and electroconductibility, but in the environment of Proton Exchange Membrane Fuel Cells, bipolar plate of stainless steel is corrosion and passivation (causing electroconductibility to reduce) easily, so need to be in its surface-coated last layer corrosion-resistant conductive coating.Adopt the method for pulse electrodeposition of the present invention at bipolar plate of stainless steel deposition one deck titanium carbide coating, can guarantee that bipolar plates has good electroconductibility, can greatly improve again the erosion resistance of bipolar plates.
The method that the present embodiment pulse electrodeposition prepares titanium carbide coating is as follows:
Adopt the line cutting that 304 stainless steel materials lines are cut into the sheet sample, and through grinding, cleaning and drying treatment.The end that the Fe-Cr silk is spot welded to sample is as contact conductor, and three-electrode system is adopted in galvanic deposit, and namely take the stainless steel plate sample as negative electrode, graphite is supporting electrode and carbon source (anode), and nickel electrode is reference electrode.With K
2TiF
6Be the titanium source, take ternary eutectic (mixing salt) 40.25mol%NaCl-50.5mol%KCl--9.25mol%NaF salt as active substance K
2TiF
6Solvent, K
2TiF
6Content in behind solvent is 5wt%.The above-mentioned mixing salt for preparing and titanium source are put into alumina crucible, under the protection of argon gas, be warmed up to 850 ℃.Adopt the PAR2273 electrochemical workstation to carry out the constant potential pulsed deposition.The applying pulse current potential is that the 3V deposition stopped 0.6 second afterwards in 1.2 seconds, and total pulsed deposition time is 2 hours, is the titanium carbide coating of 1 μ m in stainless steel plate deposition a layer thickness namely.
XRD figure and the surface topography map of described titanium carbide coating are similar to Example 1, so omit.
Embodiment 3
The method that the present embodiment pulse electrodeposition prepares titanium carbide coating is as follows:
Adopt the line cutting that 304 stainless steel materials lines are cut into the sheet sample, and through grinding, cleaning and drying treatment.The end that the Fe-Cr silk is spot welded to sample is as contact conductor, and three-electrode system is adopted in galvanic deposit, and namely the stainless steel plate sample is negative electrode, and take graphite as supporting electrode with carbon source (anode), nickel electrode is reference electrode.With K
2TiF
6Be the titanium source, take ternary eutectic (mixing salt) 40.25mol%NaCl-50.5mol%KCl--9.25mol%NaF salt as active substance K
2TiF
6Solvent, K
2TiF
6Content 10wt% in solvent.The above-mentioned mixing salt for preparing and titanium source are put into alumina crucible, under the protection of argon gas, be warmed up to 950 ℃.Adopt the PAR2273 electrochemical workstation to carry out the constant potential pulsed deposition.The applying pulse current potential is that the 2.5V deposition stopped 0.6 second afterwards in 1.8 seconds, and total pulsed deposition time is 0.5 hour, is the titanium carbide coating of 1 μ m in stainless steel plate deposition a layer thickness namely.
XRD figure and the surface topography map of described titanium carbide coating are similar to Example 1, so omit.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to claim of the present invention.Should be pointed out that for the person of ordinary skill of the art without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a pulse electrodeposition prepares the method for titanium carbide coating; it is characterized in that; comprise the steps: take substrate as negative electrode; graphite is anode and carbon source, and nickel is reference electrode, and the titanium source is melted in the mixing salt; reaction conditions is: in protection of inert gas; 800-950 ℃, react 0.5-2h under the 2.5-3V pulse potential, namely generate one deck titanium carbide coating at substrate.
2. pulse electrodeposition according to claim 1 prepares the method for titanium carbide coating, it is characterized in that, described titanium source is K
2TiF
6
3. pulse electrodeposition according to claim 1 prepares the method for titanium carbide coating, it is characterized in that, described mixing salt composition and molar content be: 40-41%NaCl, 50-51%KCl and 9-10%NaF.
4. pulse electrodeposition according to claim 3 prepares the method for titanium carbide coating, it is characterized in that, described mixing salt composition and molar content be: 40.25%NaCl, 50.5%KCl and 9.25%NaF.
5. pulse electrodeposition according to claim 1 and 2 prepares the method for titanium carbide coating, it is characterized in that, the weight percentage of described titanium source in mixing salt is 5-10%.
6. pulse electrodeposition according to claim 5 prepares the method for titanium carbide coating, it is characterized in that, the weight percentage of described titanium source in mixing salt is 7%.
7. pulse electrodeposition according to claim 1 prepares the method for titanium carbide coating, it is characterized in that, described reaction conditions is: 900 ℃, react 1h under the 2.8V pulse potential.
8. pulse electrodeposition according to claim 1 prepares the method for titanium carbide coating, it is characterized in that, depositing time is 2-4:1 with the stand-by time ratio in the described pulse potential.
9. pulse electrodeposition according to claim 1 prepares the method for titanium carbide coating, it is characterized in that, the thickness of described titanium carbide coating is 0.5-1 μ m.
10. pulse electrodeposition according to claim 1 prepares the method for titanium carbide coating, it is characterized in that, described substrate is stainless steel plate.
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Cited By (11)
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CN103409774A (en) * | 2013-07-09 | 2013-11-27 | 中国船舶重工集团公司第七二五研究所 | Method for preparing titanium or titanium alloy in molten salt by use of pulse power supply |
CN103972528A (en) * | 2014-05-30 | 2014-08-06 | 长沙理工大学 | Preparation method of metal bipolar plate protective coating of proton exchange membrane fuel cell |
CN104233424A (en) * | 2014-09-30 | 2014-12-24 | 长沙理工大学 | Carbonitriding method for metal surface |
CN105845551A (en) * | 2015-02-03 | 2016-08-10 | 朗姆研究公司 | Metal doping of amorphous carbon and silicon films used as hardmasks in substrate processing systems |
CN109207960A (en) * | 2017-07-04 | 2019-01-15 | 宁波晨鑫维克工业科技有限公司 | A kind of carbonization titanium nanocrystals coating and its preparation method and application being compound in M42 steel surface |
CN110512233A (en) * | 2019-09-25 | 2019-11-29 | 武汉大学 | A kind of porous carbide hydrogen-precipitating electrode and one one-step preparation method with honeycomb microstructure |
CN110983393A (en) * | 2019-12-27 | 2020-04-10 | 广东电网有限责任公司电力科学研究院 | Silver-niobium carbide composite coating and preparation method thereof |
CN111282586A (en) * | 2020-03-24 | 2020-06-16 | 福州大学 | Preparation method and application of in-situ alumina coated titanium carbide catalyst |
CN114122422A (en) * | 2021-09-30 | 2022-03-01 | 哈尔滨工业大学(威海) | Preparation method of surface microstructure of bipolar plate of fuel cell |
CN114808068A (en) * | 2022-03-01 | 2022-07-29 | 季华实验室 | Graphite cavity inner surface treatment method, graphite cavity sheet and graphite cavity |
CN115491675A (en) * | 2022-09-22 | 2022-12-20 | 广西大学 | Preparation method of titanium carbide coating on surface of metal bipolar plate of proton exchange membrane fuel cell |
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CN110512233A (en) * | 2019-09-25 | 2019-11-29 | 武汉大学 | A kind of porous carbide hydrogen-precipitating electrode and one one-step preparation method with honeycomb microstructure |
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CN111282586A (en) * | 2020-03-24 | 2020-06-16 | 福州大学 | Preparation method and application of in-situ alumina coated titanium carbide catalyst |
CN111282586B (en) * | 2020-03-24 | 2022-07-08 | 福州大学 | Preparation method and application of in-situ alumina coated titanium carbide catalyst |
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