CN104790001A - Method for preparing tantalum coating plated on medium-carbon CrNiMo steel surface using fused salt - Google Patents
Method for preparing tantalum coating plated on medium-carbon CrNiMo steel surface using fused salt Download PDFInfo
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- CN104790001A CN104790001A CN201510173706.2A CN201510173706A CN104790001A CN 104790001 A CN104790001 A CN 104790001A CN 201510173706 A CN201510173706 A CN 201510173706A CN 104790001 A CN104790001 A CN 104790001A
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Abstract
The invention discloses a tantalum coating plated on the medium-carbon CrNiMo steel surface using fused salt and a preparation method of the tantalum coating. The preparation method includes the following steps: an activate fluid containing rare earth is used to perform activation treatment on the surface to be plated of the steel, the treated steel is used as a cathode, and a 99.97% high-purity tantalum sheet is used as an anode; the tantalum source is melted into a salt mixture, and the reaction conditions are as follows: a coarse vacuum condition of 0.02-0.1 MPa is required, the temperature is 700-950 DEG C; the plating is carried out under 70-100 mA/cm2 for 3-5 hours in a constant-current mode with a constant current power supply, so as to obtain the tantalum coating on the steel subjected to activation treatment. According to the invention, the method of using rare earth to activate fused salt and plating tantalum through electro-deposition can be carried out in coarse vacuum and atmospheric environments; the requirement on equipment is relaxed, the cost is low, the operation is simple, and during reaction process, harmful gases are not required, and no harmful gas is produced; the method is environment-friendly; the tantalum coating prepared by using the method is dense, the coating is in well combination with a substrate, and the thickness of the coating is uniform.
Description
Technical field
The present invention relates to a kind of Heavy Carriage Wheel surface Electroplating from Molten Salts tantalum coating and preparation method thereof, melting salt can be utilized on the Heavy Carriage Wheel surface of activated process under rough vacuum condition to electroplate and to obtain tantalum coating, its resistance to erosion and wear and corrosion resistance nature can be improved, extend its service life.
Background technology
Tantalum has excellent corrosion resistance nature; the erosion of all mineral acids (comprising chloroazotic acid) except hydrofluoric acid can be resisted at ambient temperature; and hydrofluoric acid to its corrosion also slowly, is often used to manufacture the equipment such as multiple senior acid-resistant system and the heat exchanger under corrosive medium environment, well heater.Tantalum is extremely stable in vivo, does not all dissolve and corrodes, also chemical reaction does not occur in normal temperature and various biological fluid environment, and biological tissue is easy in the growth of tantalum implant surface, and therefore, tantalum is also referred to as " close biological metal ".In addition, tantalum is famous with high-melting-point, and its fusing point is widely used in the multiple civilian and military fields such as superalloy, Wimet, pressure vessels for the chemical industry up to 3000 ° of C.The corrosion resistance nature that tantalum coating is good and high-melting-point characteristic and good mechanical property, the High Temperature Tribological Behavior that steel are as good in PCrNi3Mo, 25Cr3Mo3NiNb etc. can be given, can be applicable to the device under high temperature friction operating mode, as rocket nozzle, gun barrel, piston ring etc., to improve the performance of its surface oxidation-resistant and resistance to ablation.
The method preparing tantalum coating at present mainly contains: magnetron sputtering, chemical vapour deposition, plasma spraying, ion implantation.Magnetron sputtering equipment is expensive, complex process and tantalum thin layer due to sputter temperature lower, the combination of tantalum film and matrix belongs to physical bond, and bonding strength is not high; Tantalum coating quality prepared by chemical vapour deposition is not good, and when depositing temperature is higher, larger on the impact of body material; The made coating of plasma spraying is fine and close not, more or less all there is certain hole; Ion implantation made coat-thickness is too thin, cannot meet the requirement of resistance to erosion and wear structure.Therefore be necessary to propose a kind of method that preparation technology of coating is simple, coat-thickness, bonding strength meet engineer applied.
Melting salt plating is often used to prepare refractory metal, but because melting salt plating is at high temperature carried out, the surface of steel is easily oxidized under the high temperature conditions, makes interface especially easily form comparatively loose zone of oxidation, is difficult to obtain the tantalum coating with better interface.
Summary of the invention
The object of the present invention is to provide a kind of Heavy Carriage Wheel melt surface salt plating tantalum method of activated process, the tantalum coating of acquisition combines well, thickness is uniform, and the resistance to erosion and wear of steel and corrosion resistance nature are improved.
Concrete technical scheme is as follows:
The preparation method of a kind of Heavy Carriage Wheel surface Electroplating from Molten Salts tantalum coating, comprise the steps: with the steel curved beam through activation treatment as negative electrode, high-purity tantalum piece of more than 99.9% is anode, in tantalum source is melted in mixing salt, reaction conditions is rough vacuum 0.02 ~ 0.09MPa, 700 ~ 950 ° of C, under the constant current mode of constant current power supply, at 70 ~ 100mA/cm
2lower plating 3 ~ 5h, namely obtain tantalum coating, wherein activation treatment 5min, the activation solution component of employing is: 10mL/LH
2sO
4with 1-2g/LCe (NO
3)
3mixed solution.
In preferred version of the present invention, tantalum source is K
2taF
7.
In preferred version of the present invention, mixing salt composition and molar content be 46% ~ 47%KF, 10% ~ 11%NaF and 42% ~ 44%LiF.
In more preferably scheme of the present invention, mixing salt composition and molar content be: 46.5%KF, 11.5%NaF and 42%LiF.
In preferred version of the present invention, the weight percentage of tantalum source in mixing salt is 10% ~ 15%.
In more preferably scheme of the present invention, the weight percentage of tantalum source in mixing salt is 11.5%.
In preferred version of the present invention, reaction conditions is: 0.05MPa, 850 ° of C, under the constant current mode of constant current power supply, under 80mA/cm2, electroplates 4h.
In preferred version of the present invention, the thickness of tantalum coating is 10 ~ 25 μm.
Principle of the present invention: relate to 2 processes, namely as the K in tantalum source in Heavy Carriage Wheel surface electrochemistry deposition of tantalum coating
2taF
7be reduced into Ta, generation Ta atom in the process of unplated piece surface deposition.The electro-reduction process of Ta in fluorochemical low melting point eutectic fused salt comprises following two steps:
The first step [TaF
7]
-2+ 3e=TaF
2(s)+5F
-, (1)
Second reaction is TaF
2(s)+2e=Ta+2F
-, (2)
The first step is the reversible reaction of diffusion control, the irreversible reaction that second step controls for non-diffusing.In the present invention, solubility tantalum anode is subject to comparatively serious corrosion in electrodeposition process, and the Ta atom that tantalum anode discharges makes the massfraction of Ta atom in electroplate liquid maintain a comparatively stable level.This also makes in the process of electroplating, and can obtain comparatively uniform coating.
Beneficial effect of the present invention:
(1) the present invention adopts the method for melting salt galvanic deposit, does not need main equipment and precious materials, with low cost, simple to operate.
(2) in reaction process without the need for evil gas, also do not produce objectionable impurities, so present method is environmentally friendly.
(3) that tantalum coating is combined with matrix is better in the activation of rare earth-activated liquid.
(4) process of tantalum coating deposition is also the process of diffusion, and coating adhesion can be good.
(5) tantalum coating can better protecting steel matrix under momentary impulse high temperature and mechanical wear effect.
Accompanying drawing explanation
Fig. 1 is the SEM figure (wherein 1 is tantalum, and 2 is Heavy Carriage Wheel substrate) of the tantalum coating that the melting salt electro-plating method of the embodiment of the present invention 1 tantalum coating prepares;
Fig. 2 is the line sweep EDS composition analysis of tantalum coating prepared by the melting salt electro-plating method of the embodiment of the present invention 1 tantalum coating.
Embodiment
Below by way of embodiments and drawings the present invention is further elaborated.
Embodiment 1
The melting salt electro-plating method of the present embodiment tantalum coating is as follows:
Adopt Linear cut by middle carbon PCrNi3Mo steel board Linear cut slabbing sample, specification is φ 30 × 4mm, and through grinding, cleaning and drying treatment.Fe-Cr-Al silk is spot welded to one end of sample as contact conductor, galvanic deposit adopts two electrode systems, namely with middle carbon PCrNi3Mo steel curved beam for negative electrode, solubility tantalum electrode is anode, K
2taF
7as tantalum source, be tantalum source K with ternary eutectic (mixing salt) 40.25mol%NaCl-50.5mol%KCl-9.25mol%NaF
2taF
7solvent, K
2taF
7content is in a solvent 11.5wt%.The above-mentioned mixing salt for preparing and tantalum source are put into alumina crucible, is first evacuated to 0.05MPa, is then warmed up to 850 ° of C.The H of the activated liquid 10mL/L of middle carbon PCrNi3Mo steel
2sO
4, 1.5g/L Ce (NO
3)
3activation 5min, adopt constant current power supply to carry out galvanic deposit, current density is 80mA/cm
2deposition 4h, namely deposits the tantalum coating that a layer thickness is about 16 μm on middle carbon PCrNi3Mo steel.
The section S EM figure of described tantalum coating and the line sweep EDS composition analysis of tantalum coating are see Fig. 1 and Fig. 2.
As seen from Figure 1, Figure 2, the melting salt electro-plating method of tantalum coating of the present invention is at middle carbon PCrNi
3the tantalum coating that Mo steel obtains is combined with matrix well, thickness is comparatively even.
Embodiment 2
Adopt Linear cut by middle carbon PCrNi3Mo steel board Linear cut slabbing sample, specification is φ 30 × 4mm, and through grinding, cleaning and drying treatment.Fe-Cr-Al silk is spot welded to one end of sample as contact conductor, galvanic deposit adopts two electrode systems, namely with middle carbon PCrNi3Mo steel curved beam for negative electrode, solubility tantalum electrode is anode, K
2taF
7as tantalum source, be tantalum source K with ternary eutectic (mixing salt) 40.25mol%NaCl-50.5mol%KCl-9.25mol%NaF
2taF
7solvent, K
2taF
7content is in a solvent 10wt%.The above-mentioned mixing salt for preparing and tantalum source are put into alumina crucible, is first evacuated to 0.09MPa, is then warmed up to 700 ° of C.The H of the activated liquid 10mL/L of middle carbon PCrNi3Mo steel
2sO
4, 1g/L Ce (NO
3)
3activation 5min, adopt constant current power supply to carry out galvanic deposit, current density is 70mA/cm
2deposition 3h, namely deposits the tantalum coating that a layer thickness is about 10 μm on middle carbon PCrNi3Mo steel.
Cross-sectional scans figure and the EDS line sweep of described tantalum coating are similar to Example 1.
Embodiment 3
Adopt Linear cut by middle carbon 32Cr2Mo1VA steel board Linear cut slabbing sample, specification is φ 30 × 4mm, and through grinding, cleaning and drying treatment.Fe-Cr-Al silk is spot welded to one end of sample as contact conductor, galvanic deposit adopts two electrode systems, namely with middle carbon 32Cr2Mo1VA steel curved beam for negative electrode, solubility tantalum electrode is anode, K
2taF
7as tantalum source, be tantalum source K with ternary eutectic (mixing salt) 40.25mol%NaCl-50.5mol%KCl-9.25mol%NaF
2taF
7solvent, K
2taF
7content is in a solvent 15wt%.The above-mentioned mixing salt for preparing and tantalum source are put into alumina crucible, is first evacuated to 0.02MPa, is then warmed up to 950 ° of C.The H of the activated liquid 10mL/L of middle carbon 32Cr2Mo1VA steel
2sO
4, 2g/L Ce (NO
3)
3activation 5min, adopt constant current power supply to carry out galvanic deposit, current density is 100mA/cm
2deposition 5h, namely deposits the tantalum coating that a layer thickness is about 25 μm on middle carbon 32Cr2Mo1VA steel.
Cross-sectional scans figure and the EDS line sweep of described tantalum coating are similar to Example 1.
Embodiment 4
Adopt Linear cut by middle carbon 25Cr3Mo3NiNb steel board Linear cut slabbing sample, specification is φ 30 × 4mm, and through grinding, cleaning and drying treatment.Fe-Cr-Al silk is spot welded to one end of sample as contact conductor, galvanic deposit adopts two electrode systems, namely with middle carbon 25Cr3Mo3NiNb steel curved beam for negative electrode, solubility tantalum electrode is anode, K
2taF
7as tantalum source, be tantalum source K with ternary eutectic (mixing salt) 40.25mol%NaCl-50.5mol%KCl-9.25mol%NaF
2taF
7solvent, K
2taF
7content is in a solvent 12.5wt%.The above-mentioned mixing salt for preparing and tantalum source are put into alumina crucible, is first evacuated to 0.07MPa, is then warmed up to 900 ° of C.The H of the activated liquid 10mL/L of middle carbon 25Cr3Mo3NiNb steel
2sO
4, 1.7g/L Ce (NO
3)
3activation 5min, adopt constant current power supply to carry out galvanic deposit, current density is 90mA/cm
2deposition 4.5h, namely deposits the tantalum coating that a layer thickness is about 18 μm on middle carbon 25Cr3Mo3NiNb steel.
Cross-sectional scans figure and the EDS line sweep of described tantalum coating are similar to Example 1.
Claims (8)
1. the preparation method of a Heavy Carriage Wheel surface Electroplating from Molten Salts tantalum coating, it is characterized in that, comprise the steps: with the steel curved beam through activation treatment as negative electrode, high-purity tantalum piece of more than 99.9% is anode, in tantalum source is melted in mixing salt, reaction conditions is rough vacuum 0.02 ~ 0.09MPa, 700 ~ 950 ° of C, under the constant current mode of constant current power supply, at 70 ~ 100mA/cm
2lower plating 3 ~ 5h, namely obtain tantalum coating, wherein activation treatment 5min, the activation solution component of employing is: 10mL/LH
2sO
4with 1-2g/LCe (NO
3)
3mixed solution.
2. the preparation method of Heavy Carriage Wheel surface as claimed in claim 1 Electroplating from Molten Salts tantalum coating, it is characterized in that, tantalum source is K
2taF
7.
3. the preparation method of Heavy Carriage Wheel surface as claimed in claim 1 Electroplating from Molten Salts tantalum coating, is characterized in that, mixing salt composition and molar content be 46% ~ 47%KF, 10% ~ 11%NaF and 42% ~ 44%LiF.
4. the preparation method of Heavy Carriage Wheel surface as claimed in claim 1 Electroplating from Molten Salts tantalum coating, is characterized in that, mixing salt composition and molar content be 46.5%KF, 11.5%NaF and 42%LiF.
5., as the preparation method according to Heavy Carriage Wheel surface according to claim 1 Electroplating from Molten Salts tantalum coating, it is characterized in that, the weight percentage of tantalum source in mixing salt is 10% ~ 15%.
6. the preparation method of Heavy Carriage Wheel surface as claimed in claim 1 Electroplating from Molten Salts tantalum coating, it is characterized in that, the weight percentage of tantalum source in mixing salt is 11.5%.
7. the preparation method of Heavy Carriage Wheel surface as claimed in claim 1 Electroplating from Molten Salts tantalum coating, it is characterized in that, reaction conditions is: 0.05MPa, and 850 ° of C, under the constant current mode of constant current power supply, at 80mA/cm
2lower plating 4h.
8. the preparation method of Heavy Carriage Wheel surface as claimed in claim 1 Electroplating from Molten Salts tantalum coating, it is characterized in that, the thickness of the tantalum coating of acquisition is 10 ~ 25 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510173706.2A CN104790001A (en) | 2015-04-13 | 2015-04-13 | Method for preparing tantalum coating plated on medium-carbon CrNiMo steel surface using fused salt |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510173706.2A CN104790001A (en) | 2015-04-13 | 2015-04-13 | Method for preparing tantalum coating plated on medium-carbon CrNiMo steel surface using fused salt |
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|---|---|
| CN104790001A true CN104790001A (en) | 2015-07-22 |
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ID=53555183
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|---|---|---|---|
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3814673A (en) * | 1969-07-02 | 1974-06-04 | Gen Electric | Process for tantalliding and niobiding base metal compositions |
| JP2001279486A (en) * | 2000-03-30 | 2001-10-10 | Japan Science & Technology Corp | Method for plating tantalum |
| CN101638804A (en) * | 2008-07-30 | 2010-02-03 | 宝山钢铁股份有限公司 | Chromium-free passivation solution for tin plate and method for using same |
| CN102330095A (en) * | 2011-08-29 | 2012-01-25 | 中国科学院合肥物质科学研究院 | Preparation method of Al2O3 coating on surface of steel-matrix material |
| CN103060863A (en) * | 2013-01-18 | 2013-04-24 | 沈阳瑞康达科技有限公司 | Method for preparing Ni-Ti surface tantalum plating layer with halide fused salt electro-deposition |
-
2015
- 2015-04-13 CN CN201510173706.2A patent/CN104790001A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3814673A (en) * | 1969-07-02 | 1974-06-04 | Gen Electric | Process for tantalliding and niobiding base metal compositions |
| JP2001279486A (en) * | 2000-03-30 | 2001-10-10 | Japan Science & Technology Corp | Method for plating tantalum |
| CN101638804A (en) * | 2008-07-30 | 2010-02-03 | 宝山钢铁股份有限公司 | Chromium-free passivation solution for tin plate and method for using same |
| CN102330095A (en) * | 2011-08-29 | 2012-01-25 | 中国科学院合肥物质科学研究院 | Preparation method of Al2O3 coating on surface of steel-matrix material |
| CN103060863A (en) * | 2013-01-18 | 2013-04-24 | 沈阳瑞康达科技有限公司 | Method for preparing Ni-Ti surface tantalum plating layer with halide fused salt electro-deposition |
Non-Patent Citations (1)
| Title |
|---|
| 王升 等: "熔盐电镀钽及其耐磨损烧蚀性能", 《中国表面工程》 * |
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Application publication date: 20150722 |
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