CN114507893A - High-hardness wear-resistant micro-arc oxidation coating electrolyte for tantalum alloy surface and preparation method thereof - Google Patents
High-hardness wear-resistant micro-arc oxidation coating electrolyte for tantalum alloy surface and preparation method thereof Download PDFInfo
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- 229910001362 Ta alloys Inorganic materials 0.000 title claims abstract description 68
- 239000003792 electrolyte Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
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- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- 229910001388 sodium aluminate Inorganic materials 0.000 claims description 6
- 239000002562 thickening agent Substances 0.000 claims description 6
- 239000003112 inhibitor Substances 0.000 claims description 5
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- 239000000654 additive Substances 0.000 claims description 4
- 230000000996 additive effect Effects 0.000 claims description 4
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 4
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 4
- 150000003608 titanium Chemical class 0.000 claims description 4
- 150000003754 zirconium Chemical class 0.000 claims description 4
- 229910019985 (NH4)2TiF6 Inorganic materials 0.000 claims description 2
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 2
- 229910020491 K2TiF6 Inorganic materials 0.000 claims description 2
- 229910020264 Na2TiO3 Inorganic materials 0.000 claims description 2
- 229910010252 TiO3 Inorganic materials 0.000 claims description 2
- NMGYKLMMQCTUGI-UHFFFAOYSA-J diazanium;titanium(4+);hexafluoride Chemical compound [NH4+].[NH4+].[F-].[F-].[F-].[F-].[F-].[F-].[Ti+4] NMGYKLMMQCTUGI-UHFFFAOYSA-J 0.000 claims description 2
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/026—Anodisation with spark discharge
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
- Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
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Abstract
The invention belongs to the technical field of alloy surface treatment, and provides a high-hardness wear-resistant micro-arc oxidation coating electrolyte for a tantalum alloy surface and a preparation method thereof, which are used for effectively improving the hardness and wear resistance of a micro-arc oxidation coating. According to the invention, the hard phase decomposer is added into the electrolyte, and hard phase particles are obtained by decomposing the hard phase decomposer at high temperature and are fused into the coating, so that the hardness of the micro-arc oxidation coating is improved, and the tribological property of the coating is improved; meanwhile, the preparation method for obtaining the micro-arc oxidation coating based on the matching design of the electrolyte and the electrical parameters adopts a segmented pressurization mode to gradually increase the oxidation voltage so as to adjust the micro-arc oxidation reaction strength, control the growth rate of the micro-arc oxidation coating of the tantalum alloy and avoid the phenomenon that the structure and the compactness of the coating are damaged due to a large amount of micro-cracks generated by the coating due to the over-fast growth; the finally prepared micro-arc oxidation coating has small surface porosity, few cracks and compact structure, the hardness of the coating is higher than 800HV, and the dry friction coefficient of the coating and WC balls is reduced to 0.3-0.4 from 0.75.
Description
Technical Field
The invention belongs to the technical field of alloy surface treatment, relates to a tantalum alloy surface treatment technology, and particularly provides a high-hardness wear-resistant micro-arc oxidation coating electrolyte for a tantalum alloy surface and a preparation method thereof.
Background
Tantalum is a rare high melting metal among non-ferrous metals, having a melting point of 2996 ℃ second only to tungsten and rhenium metals. The chemical property of tantalum is very stable at normal temperature, and only reacts with hydrofluoric acid and acidic solution containing fluoride ions. The tantalum alloy has excellent performances such as high density, high strength, high temperature resistance, corrosion resistance and the like, and is widely applied in the fields of aerospace engines, chemical corrosion, atomic energy industry and the like, particularly high-temperature corrosion and the like and severe and complex environments thereof; however, the hardness of tantalum alloys is low, about 330HV, limiting the use of tantalum alloys in abrasive environments. When the tantalum alloy is used as a connecting piece, relative friction motion is inevitably generated between the tantalum alloy and an assembly contact material; the existing documents also mention that the phenomenon of high friction coefficient exists between tantalum alloy and assembly materials, the surface states of the tantalum alloy and an assembly workpiece are directly influenced, serious friction and abrasion are generated, and further the problems of energy waste, service life shortening and the like are caused.
In order to improve the service effect, the tantalum alloy needs to be subjected to surface modification treatment and then put into use; surface coating techniques can be used to improve the tribological properties of the tantalum alloy surface, resulting in low friction of the tantalum alloy piece with adjacent parts. The current tantalum alloy surface treatment technology comprises electroplating, vapor deposition, micro-arc oxidation and the like; the tantalum alloy has excellent corrosion resistance, difficult electroplating pretreatment and lower coating binding force; the vapor deposition process is complex and the cost is high; the micro-arc oxidation process mainly depends on matching and adjustment of electrolyte and electric parameters, and a modified ceramic coating mainly comprising matrix metal oxide and auxiliary electrolyte components grows on the surfaces of valve metals such as aluminum, magnesium, titanium and the like and alloys thereof under the action of instantaneous high temperature and high pressure generated by arc discharge; the micro-arc oxidation can carry out in-situ ceramic conversion on tantalum and the alloy thereof, the process is simple, and the coating has high hardness, good wear resistance, corrosion resistance and good insulating property.
At present, the coating prepared on the surface of the tantalum alloy by the common micro-arc oxidation technology is rough and porous in surface, has a large number of micro-cracks under the action of residual thermal stress, influences the binding force between the coating and a substrate, reduces the surface hardness of the coating, and shows high friction coefficient in the friction process, so that the application of the tantalum alloy micro-arc oxidation coating in a wear environment is greatly limited. The thickness, hardness and other properties of the micro-arc oxidation coating are influenced by factors such as energy parameters, matrix alloy elements, solution characteristics and the like, and the composition and proportion of the electrolyte are important to influence the surface appearance and coating properties of the micro-arc oxidation coating.
Disclosure of Invention
Aiming at various problems in the prior art, the invention provides the electrolyte of the high-hardness wear-resistant micro-arc oxidation coating on the surface of the tantalum alloy and the preparation method of the high-hardness wear-resistant micro-arc oxidation coating on the surface of the tantalum alloy based on the electrolyte; according to the invention, the hard phase decomposer dissolved in water is introduced into the electrolyte, and the hard phase decomposer is utilized to decompose and generate hard phase particles in the high-temperature micro-arc oxidation process and is fused into the micro-arc oxidation coating by depending on the configuration of the electrolyte and electrical parameters, so that the hardness and the wear resistance of the micro-arc oxidation coating are effectively improved.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the high-hardness wear-resistant micro-arc oxidation coating electrolyte for the tantalum alloy surface comprises: a main film forming agent, a pH regulator and an additive, wherein the main film forming agent is Na3PO4The pH regulator is NaOH; characterized in that the additive comprises: the film layer thickening agent, the arc inhibitor and the hard phase decomposer, wherein the hard phase decomposer is one or more of soluble aluminum salt, titanium salt, zirconium salt and fluorine salt which can be decomposed into hard phase particles.
Further, the concentration of the main film forming agent is 5-30 g/L, the concentration of the pH regulator is 5-10 g/L, the concentration of the film layer thickening agent is 1-10 g/L, the concentration of the arc inhibitor is 1-10 g/L, and the concentration of the hard phase decomposer is 5-30 g/L; the solvent is water.
Further, the aluminum salt is NaAlO2、KAlO2The titanium salt is Na2TiO3、K2TiO3The zirconium salt is Na2ZrO3、K2ZrO3The fluorine salt is Na2TiF6、K2TiF6、(NH4)2TiF6。
Further, the film layer thickening agent is NaF, KF and Na2One or more of S.
Further, the arc inhibitor is disodium ethylene diamine tetraacetate (EDTA-2Na) and hexamethylenetetramine (C)6H12N4) Glycerol (C)3H8O3) One or more of (a).
A preparation method of a high-hardness wear-resistant micro-arc oxidation coating on the surface of tantalum alloy is characterized by comprising the following steps: preparing the high-hardness wear-resistant micro-arc oxidation coating electrolyte on the surface of the tantalum alloy, placing the electrolyte in a stainless steel electrolytic tank, and setting electrical parameters as follows: the method comprises the steps of adopting a constant-voltage bipolar working mode, controlling the voltage to be 100-550V, the discharge frequency to be 400-1000 Hz, the positive-negative duty ratio to be 10-50%, and the oxidation time to be 10-60 min, controlling the temperature of an electrolyte to be lower than 40 ℃, connecting a tantalum alloy sample to a conducting rod, immersing the tantalum alloy sample into the electrolyte to serve as an anode, and using a stainless steel electrolytic tank as a cathode to perform micro-arc oxidation treatment, so as to obtain the high-hardness wear-resistant micro-arc oxidation coating on the surface of the tantalum alloy.
Further, the micro-arc oxidation treatment is performed by adopting a sectional pressurization mode: after micro-arc oxidation arcing, performing step increase by taking 10V as step increase, performing step increase for 1-5 times on the basis of initial voltage until the target voltage is reached, and oxidizing for 5-15 min at each voltage; it should be noted that: and setting the voltage value in the electrical parameter as the target voltage, and determining the initial voltage immediately after the target voltage and the step-up times are determined.
The invention has the beneficial effects that:
the invention provides a high-hardness wear-resistant micro-arc oxidation coating electrolyte for a tantalum alloy surface and a preparation method of a high-hardness wear-resistant micro-arc oxidation coating for the tantalum alloy surface based on the electrolyte, and the electrolyte has the following advantages:
1) according to the invention, the hard phase decomposer is added into the electrolyte, and hard phase particles are obtained by decomposing the hard phase decomposer at high temperature and are fused into the coating, so that the hardness of the micro-arc oxidation coating is improved, and the tribological property of the coating is improved; for example, NaAlO2Reacting with the tantalum alloy surface micro-arc oxidation product at high temperature to obtain hard phase AlTaO3Composite oxide and Al2O3By using KAlO2The same effect is also achieved; in addition, compared with the method of directly adding hard phase particles into the electrolyte, the method of the invention utilizes the thermal decomposition of the corresponding salt of the hard phase particles to generate the hard phase, thus avoiding the problem of uneven coating caused by particle agglomeration and sedimentation;
2) according to the method, the oxidation voltage is gradually increased in a mode of increasing the voltage by a specified voltage and sections, so that the micro-arc oxidation reaction strength is adjusted, the growth rate of the micro-arc oxidation coating of the tantalum alloy is controlled, and the phenomenon that the structure and compactness of the coating are damaged due to a large amount of micro-cracks generated by the coating due to too fast growth is avoided;
3) the micro-arc oxidation coating prepared by the method has the advantages of small surface porosity, few cracks and compact structure, the hardness of the coating is higher than 800HV, and the dry friction coefficient of the coating and WC balls is reduced to 0.3-0.4 from 0.75;
4) the tantalum alloy high-hardness wear-resistant coating prepared by the method is very uniform, is tightly combined with a substrate, has a simple preparation method, mild reaction conditions and low cost, and is beneficial to expanding the application of the tantalum alloy in a wear environment.
Drawings
FIG. 1 is an SEM photograph of the surface morphology of the high-hardness wear-resistant micro-arc oxidation coating on the surface of the tantalum alloy prepared in example 1.
FIG. 2 is an SEM photograph of the cross-sectional morphology of the high-hardness wear-resistant micro-arc oxidation coating on the surface of the tantalum alloy prepared in example 1.
FIG. 3 is a phase composition diagram of the cross-sectional morphology XRD of the high-hardness wear-resistant micro-arc oxidation coating on the surface of the tantalum alloy prepared in example 1.
Detailed Description
The following examples are given for the detailed implementation and specific operation procedures, but the scope of the present invention is not limited to the following examples.
Example 1
The embodiment provides an electrolyte and a preparation method of a high-hardness wear-resistant micro-arc oxidation coating on the surface of a tantalum alloy based on the electrolyte, and the preparation method comprises the following specific steps:
step 4, micro-arc oxidation: starting circulating cooling water, controlling the temperature of the electrolyte to be lower than 40 ℃, connecting the tantalum alloy sample to a conducting rod by using an aluminum wire, immersing the conducting rod into the electrolyte to serve as an anode, using a stainless steel electrolytic tank as a cathode, and starting a bidirectional pulse power supply to perform micro-arc oxidation treatment;
and step 5, post-treatment: washing the coating sample after the micro-arc oxidation treatment with distilled water, removing the residual electrolyte on the surface, and drying with cold air to obtain the high-hardness wear-resistant micro-arc oxidation coating on the surface of the tantalum alloy.
The high-hardness wear-resistant micro-arc oxidation coating on the surface of the tantalum alloy prepared by the embodiment is tested, the surface appearance SEM photo is shown in figure 1, the cross section appearance SEM photo is shown in figure 2, and the cross section appearance XRD phase composition diagram is shown in figure 3, and the micro-arc oxidation surface coating is very uniform, has no microcracks, no pores and no bare alloy as shown in figure 1, so that the effect of the micro-arc oxidation coating is ideal; FIG. 2 shows that the micro-arc oxidation coating is thin (about 20um), uniform in thickness, good in adhesion effect, high in compactness, high in strength, small in surface porosity, free of cracks and compact in structure; FIG. 3 shows the micro-arc oxidation coatingA trace amount of AlTaO was formed3Composite oxide and trace amount of Al2O3It is the formation of these two substances that provides the tantalum alloy surface with high hardness and wear resistance.
The thickness of the high-hardness wear-resistant micro-arc oxidation coating on the surface of the tantalum alloy obtained in the embodiment is about 21 microns, the hardness reaches 1200HV, and the dry friction coefficient between the tantalum alloy and WC balls under 4N load is 0.32.
Example 2
The embodiment provides an electrolyte and a preparation method of a high-hardness wear-resistant micro-arc oxidation coating on the surface of a tantalum alloy based on the electrolyte, and the preparation method comprises the following specific steps:
step 4, micro-arc oxidation: starting circulating cooling water, controlling the temperature of the electrolyte to be lower than 40 ℃, connecting the tantalum alloy sample to a conducting rod by using an aluminum wire, immersing the conducting rod into the electrolyte to serve as an anode, using a stainless steel electrolytic tank as a cathode, and starting a bidirectional pulse power supply to perform micro-arc oxidation treatment;
and step 5, post-treatment: washing the coating sample after the micro-arc oxidation treatment with distilled water, removing the residual electrolyte on the surface, and drying with cold air to obtain the high-hardness wear-resistant micro-arc oxidation coating on the surface of the tantalum alloy. The high-hardness wear-resistant micro-arc oxidation coating on the surface of the tantalum alloy has the effect similar to that of the embodiment 1.
The high-hardness wear-resistant micro-arc oxidation coating on the surface of the tantalum alloy obtained in the embodiment has thinner thickness of about 15 microns, hardness of about 900HV and dry friction coefficient of 0.35 between the coating and WC balls under 4N load.
Example 3
The embodiment provides an electrolyte and a preparation method of a high-hardness wear-resistant micro-arc oxidation coating on the surface of a tantalum alloy based on the electrolyte, and the preparation method comprises the following specific steps:
step 4, micro-arc oxidation: starting circulating cooling water, controlling the temperature of the electrolyte to be lower than 40 ℃, connecting the tantalum alloy sample to a conducting rod by using an aluminum wire, immersing the conducting rod into the electrolyte to serve as an anode, using a stainless steel electrolytic tank as a cathode, and starting a bidirectional pulse power supply to perform micro-arc oxidation treatment;
and step 5, post-treatment: washing the coating sample after the micro-arc oxidation treatment with distilled water, removing the residual electrolyte on the surface, and drying with cold air to obtain the high-hardness wear-resistant micro-arc oxidation coating on the surface of the tantalum alloy. The high-hardness wear-resistant micro-arc oxidation coating on the surface of the tantalum alloy still has the effect similar to that of the embodiment 1.
The thickness of the high-hardness wear-resistant micro-arc oxidation coating on the surface of the tantalum alloy obtained in the embodiment is about 23 μm, the hardness is about 860HV, and the dry friction coefficient between the coating and a WC ball under 4N load is 0.30.
While the invention has been described with reference to specific embodiments, any feature disclosed in this specification may be replaced by alternative features serving the same, equivalent or similar purpose, unless expressly stated otherwise; all of the disclosed features, or all of the method or process steps, may be combined in any combination, except mutually exclusive features and/or steps.
Claims (7)
1. The high-hardness wear-resistant micro-arc oxidation coating electrolyte for the tantalum alloy surface comprises: a main film forming agent, a pH regulator and an additive, wherein the main film forming agent is Na3PO4The pH regulator is NaOH; characterized in that the additive comprises: the film layer thickening agent, the arc suppression agent and the hard phase decomposing agent are one or more of soluble aluminum salt, titanium salt, zirconium salt and fluorine salt which can be decomposed into hard phase particles.
2. The electrolyte for the high-hardness wear-resistant micro-arc oxidation coating on the surface of the tantalum alloy according to claim 1, wherein the concentration of the main film forming agent is 5-30 g/L, the concentration of the pH regulator is 5-10 g/L, the concentration of the film layer thickening agent is 1-10 g/L, the concentration of the arc inhibitor is 1-10 g/L, and the concentration of the hard phase decomposer is 5-30 g/L; the solvent is water.
3. The electrolyte for high-hardness wear-resistant micro-arc oxidation coating on the surface of tantalum alloy according to claim 1, wherein the aluminum salt is NaAlO2、KAlO2The titanium salt is Na2TiO3、K2TiO3The zirconium salt is Na2ZrO3、K2ZrO3The fluorine salt is Na2TiF6、K2TiF6、(NH4)2TiF6。
4. The electrolyte for the high-hardness wear-resistant micro-arc oxidation coating on the surface of the tantalum alloy according to claim 1, wherein the film layer thickening agent is NaF, KF or Na2One or more of S.
5. The electrolyte for the high-hardness wear-resistant micro-arc oxidation coating on the surface of the tantalum alloy as claimed in claim 1, wherein the arc inhibitor is disodium ethylene diamine tetraacetate (EDTA-2Na) and hexamethylenetetramine (C)6H12N4) Glycerol (C)3H8O3) One or more of (a).
6. A preparation method of a high-hardness wear-resistant micro-arc oxidation coating on the surface of tantalum alloy is characterized by comprising the following steps: preparing the high-hardness wear-resistant micro-arc oxidation coating electrolyte on the surface of the tantalum alloy of claim 1, placing the electrolyte in a stainless steel electrolytic tank, and setting electrical parameters as follows: the method comprises the steps of adopting a constant-voltage bipolar working mode, controlling the voltage to be 100-550V, the discharge frequency to be 400-1000 Hz, the positive-negative duty ratio to be 10-50%, and the oxidation time to be 10-60 min, controlling the temperature of an electrolyte to be lower than 40 ℃, connecting a tantalum alloy sample to a conducting rod, immersing the tantalum alloy sample into the electrolyte to serve as an anode, and using a stainless steel electrolytic tank as a cathode to perform micro-arc oxidation treatment, so as to obtain the high-hardness wear-resistant micro-arc oxidation coating on the surface of the tantalum alloy.
7. The method for preparing the high-hardness wear-resistant micro-arc oxidation coating on the surface of the tantalum alloy according to claim 6, wherein the micro-arc oxidation treatment is performed in a segmented pressurization mode: after micro-arc oxidation arcing, stepping up by taking 10V as step-up, stepping up for 1-5 times on the basis of initial voltage until the target voltage is reached, and oxidizing for 5-15 min at each voltage.
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Citations (9)
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