CN111676440A - Preparation method of tantalum oxide in-situ composite tantalum-based nanocrystalline wear-resistant and anti-friction coating - Google Patents
Preparation method of tantalum oxide in-situ composite tantalum-based nanocrystalline wear-resistant and anti-friction coating Download PDFInfo
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- CN111676440A CN111676440A CN202010752610.2A CN202010752610A CN111676440A CN 111676440 A CN111676440 A CN 111676440A CN 202010752610 A CN202010752610 A CN 202010752610A CN 111676440 A CN111676440 A CN 111676440A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/134—Plasma spraying
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/06—Metallic material
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Abstract
The invention relates to a preparation method of a tantalum oxide in-situ composite tantalum-based nanocrystalline wear-resistant and anti-friction coating, which comprises the following steps: after the substrate is pretreated, Ta powder containing tantalum hydride is sprayed on the surface of the substrate after being melted by utilizing a plasma spraying technology, and Ta is obtained2O5And compounding the Ta-based nanocrystalline coating in situ. The preparation method is simple and easy to realize, and the obtained coating has the characteristics of high bonding strength, excellent friction-reducing and wear-resisting properties and the like, and is suitable for parts requiring high wear resistance and good friction-reducing property at the same time.
Description
Technical Field
The invention relates to the technical field of surface engineering, in particular to a preparation method of a tantalum oxide in-situ composite tantalum-based nanocrystalline wear-resistant and anti-friction coating.
Background
In the fields of aerospace, weaponry and the like, key parts of the aircraft usually run in extremely harsh environments and need to have the performances of wear resistance, friction reduction, long service life and the like. The friction and wear generally occur on the surface of a workpiece (for example, the surface of a shot blasting machine blade is eroded and worn by iron (steel) shots, the surface of a steel gun tube is eroded and worn by chemical corrosion of hot gas generated by burning of propellant, and a rubber sealing element is abraded by friction in the service process to form two-body abrasive wear of a rubber/metal matching pair). by adopting a surface strengthening technology, the friction and wear of surfaces which are in mutual contact or generate relative motion can be greatly reduced, so that the consumption of materials and energy is reduced, and the service life of the workpiece is prolonged. The surface coating technology is more and more emphasized by researchers, and the preparation of the protective coating with good friction-reducing and wear-resisting properties on the surface of the workpiece is a feasible method for solving the problem of friction and wear of the workpiece.
The metal tantalum (Ta) has high melting point, high density, low expansion coefficient, low thermal conductivity and good tribology and corrosion resistance, and can be used as a surface protection material. Because of the symbiosis of tantalum and niobium minerals, Ta is complex to refine and expensive in cost, and the direct use of Ta cannot meet the industrial requirements, so that Ta metal is more suitable for coating materials. The Ta-based coating can meet the requirements of various extreme working conditions due to unique performance and has wide application prospect. However, at present, both at home and abroad, it is about to target Ta-Ta2O5The tribological performance of the bulk nanocrystalline coating was almost none studied.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a tantalum oxide in-situ composite tantalum-based nanocrystalline wear-resistant antifriction coating, which has simple process and is suitable for industrial production.
In order to solve the problems, the preparation method of the tantalum oxide in-situ composite tantalum-based nanocrystalline wear-resistant and antifriction coating is characterized by comprising the following steps: after the substrate is pretreated, Ta powder containing tantalum hydride is sprayed on the surface of the substrate after being melted by utilizing a plasma spraying technology, and Ta is obtained2O5And compounding the Ta-based nanocrystalline coating in situ.
The base body is made of steel with different grades.
The pretreatment is that the base material is degreased by neutral or weak acid water-based degreaser, then washed by distilled water, polished and derusted, washed by acetone solution, and finally brown corundum (the main component is Al)2O3) And (4) sand blasting.
The Ta powder contains α -Ta phase and Ta2H phase of particle size<45 μm, purity > 99.9%.
The plasma spraying conditions include that the current is 360-420A, the voltage is 150-170V, the argon flow is 110-160 LPM, the hydrogen flow is 30-50 LPM, continuous spraying or intermittent spraying is adopted, the spraying frequency is 6-8 times, and the interval between the continuous spraying and the previous spraying and the next spraying is 2-3 s.
Compared with the prior art, the invention has the following advantages:
1. the invention contains α -Ta phase and Ta2H phase, particle size<Ta powder with the purity of more than 99.9 percent and the particle size of 45 mu m is taken as a raw material (shown in figure 1), and the Ta-based coating with the nanocrystalline structure is prepared by the atmospheric plasma spraying technology and the Ta is compounded in situ2O5The ceramic phase structure not only enhances the hardness of the coating, but also enhances the wear resistance of the coating under the boundary lubrication condition. Therefore, the coating has the characteristics of high hardness and toughness, high bonding strength, excellent antifriction and wear resistance and the like, and is suitable for parts requiring high wear resistance and good antifriction property at the same time.
2. The surface of the nanocrystalline coating obtained by the invention is uniform and flat, and the average grain size of alpha-Ta in the coating along the (110) crystal plane normal direction is 23-52 nm and the lattice distortion is 0.37-0.55 percent (as shown in figure 2) calculated by XRD analysis. The fine nano-crystalline grains enhance the scratch resistance of the coating under dry rubbing conditions.
3. The Ta obtained by the invention is subjected to fretting friction wear testing machine2O5And (3) carrying out performance evaluation on the in-situ compounded Ta-based nanocrystalline coating, wherein the friction condition adopts a ball-disk reciprocating mode.
The Ta-based coating was compared with commercially available Al having a diameter of 10mm2O3The ball is used as a dual ball to form a friction compatibility pair, the test environment is atmosphere, and the test conditions are as follows: dry friction conditions (load 10N, reciprocation frequency 6 Hz, amplitude 1 mm) and paraffin lubrication conditions (load 30N, reciprocation frequency 40 Hz, amplitude 1 mm).
The test results are shown in figures 3-4, and the lowest wear rate of the coating under the dry friction condition is 9.494 × 10-4mm3·N-1·m-1(ii) a Lowest average friction of coating under paraffin lubrication conditionsThe coefficient is 0.1811, and the wear rate is as low as 1.9749 × 10-8mm3·N-1·m-1. The Ta2O5The in-situ composite Ta-based nanocrystalline coating shows low friction coefficient and high wear resistance under the conditions of dry friction and paraffin lubrication.
4. The preparation method is simple and easy to realize, can be sprayed on the surfaces of different metal parts, is suitable for industrial production, and has potential application prospect in the environment of a mechanical motion system needing wear resistance and friction reduction.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is Ta according to the present invention2O5XRD pattern of raw material Ta powder for in-situ compounding Ta-based nanocrystalline coating spraying.
FIG. 2 is Ta according to the present invention2O5And compounding an XRD pattern of the Ta-based nanocrystalline coating in situ.
FIG. 3 is Ta according to the present invention2O5And (3) a curve graph of the change of the friction coefficient of the in-situ compounded Ta-based nanocrystalline coating along with time under the paraffin lubrication condition.
FIG. 4 is Ta according to the present invention2O5And (3) in-situ compounding a histogram of the lowest wear rate of the Ta-based nanocrystalline coating under dry friction and paraffin lubrication conditions.
Detailed Description
Embodiment 1 a method for preparing tantalum oxide in-situ composite tantalum-based nanocrystalline wear-resistant and anti-friction coating:
a45 # steel substrate is processed into a round block sample with the size of phi 24mm × 8mm, and then is pretreated, wherein the method comprises the following steps of firstly adopting a neutral or weakly acidic water-based degreasing agent to degrease the substrate, then sequentially carrying out distilled water washing, polishing and rust removal, acetone solution washing, and finally adopting brown corundum (the main component is Al)2O3) And (4) sand blasting. The whole washing process is carried out under ultrasonic oscillation.
After pretreatment, by utilizing a plasma spraying technology, a direct current is adopted to drive a plasma arc to reach a high temperature of more than 3000K, and hydrogenation is carried outMelting Ta powder containing α -Ta phase and Ta, and spraying onto the surface of substrate in atmosphere2H phase of particle size<45 μm, purity > 99.9% (see FIG. 1). Argon is used as main gas for spraying, and hydrogen is used as auxiliary gas; the purity of the introduced argon and hydrogen is more than 99.99 percent. The spraying current is 420A, the voltage is 161V, the argon flow is 115-117 LPM, the hydrogen flow is 30-40 LPM, continuous spraying or intermittent spraying is adopted, the spraying frequency is 6 times, and the interval between the continuous spraying and the two-time spraying is 2-3 s. After the spraying is finished, Ta is obtained2O5And compounding the Ta-based nanocrystalline coating in situ (shown in figure 2).
Embodiment 2 a method for preparing tantalum oxide in-situ composite tantalum-based nanocrystalline wear-resistant and anti-friction coating:
the substrate was pretreated in the same manner as in example 1.
After pretreatment, by utilizing a plasma spraying technology, a direct current is adopted to drive a plasma arc to reach a high temperature of more than 3000K, and Ta powder containing tantalum hydride is melted and sprayed on the surface of a substrate in an atmospheric environment. Ta powder as in example 1. Argon is used as main gas for spraying, and hydrogen is used as auxiliary gas; the purity of the introduced argon and hydrogen is more than 99.99 percent. The spraying current is 360A, the voltage is 150V, the argon flow is 110-115 LPM, the hydrogen flow is 40-50 LPM, continuous spraying or intermittent spraying is adopted, the spraying frequency is 7 times, and the interval between the continuous spraying and the two-time spraying is 2-3 s. After the spraying is finished, Ta is obtained2O5And compounding the Ta-based nanocrystalline coating in situ.
Embodiment 3 a method for preparing tantalum oxide in-situ composite tantalum-based nanocrystalline wear-resistant and anti-friction coating:
the substrate was pretreated in the same manner as in example 1.
After pretreatment, by utilizing a plasma spraying technology, a direct current is adopted to drive a plasma arc to reach a high temperature of more than 3000K, and Ta powder containing tantalum hydride is melted and sprayed on the surface of a substrate in an atmospheric environment. Ta powder as in example 1. Argon is used as main gas for spraying, and hydrogen is used as auxiliary gas; the purity of the introduced argon and hydrogen is more than 99.99 percent. The spraying current is 400A, the voltage is 170V, the argon flow is 160 LPM, the hydrogen flow is 35-45 LPM, continuous spraying or intermittent spraying is adopted, and the spraying frequency is 8 timesAnd continuously spraying or spraying twice before and after 2-3 s apart. After the spraying is finished, Ta is obtained2O5And compounding the Ta-based nanocrystalline coating in situ.
In the above examples 1 to 3, the material of the substrate was various grades of steel materials, such as 45 steel, 30CrMo, 1Cr18Ni9Ti, etc.
When the coating is applied, once the plasma spraying current, voltage, argon flow and hydrogen flow exceed the ranges of the invention, although the main structure of the obtained coating is kept unchanged, the fine structure characteristics such as pore distribution, grain size and lattice distortion in the coating and the wear resistance are greatly changed under the influence of the change of melting and cooling conditions, and under the same friction and wear test conditions, the wear rate of the coating is increased to 10-20 times or more of that of the coating obtained in the above embodiment.
Claims (5)
1. A preparation method of tantalum oxide in-situ composite tantalum-based nanocrystalline wear-resistant and anti-friction coating is characterized by comprising the following steps: after the substrate is pretreated, Ta powder containing tantalum hydride is sprayed on the surface of the substrate after being melted by utilizing a plasma spraying technology, and Ta is obtained2O5And compounding the Ta-based nanocrystalline coating in situ.
2. The method for preparing tantalum oxide in-situ composite tantalum-based nanocrystalline wear-resistant antifriction coating according to claim 1, characterized in that: the base body is made of steel with different grades.
3. The method for preparing tantalum oxide in-situ composite tantalum-based nanocrystalline wear-resistant antifriction coating according to claim 1, characterized in that: the pretreatment is to remove oil from the base material by using a neutral or weakly acidic water-based oil removal agent, then sequentially wash the base material by using distilled water, polish and remove rust, wash the base material by using an acetone solution, and finally sand blast by using brown corundum.
4. The method for preparing tantalum oxide in-situ composite tantalum-based nanocrystalline wear-resistant antifriction coating according to claim 1, characterized in that the Ta powder contains α -Ta phase and Ta2H phase of particle size<45 μm, purity > 99.9%.
5. The method for preparing tantalum oxide in-situ composite tantalum-based nanocrystalline wear-resistant antifriction coating according to claim 1, characterized in that: the plasma spraying conditions include that the current is 360-420A, the voltage is 150-170V, the argon flow is 110-160 LPM, the hydrogen flow is 30-50 LPM, continuous spraying or intermittent spraying is adopted, the spraying frequency is 6-8 times, and the interval between the continuous spraying and the previous spraying and the next spraying is 2-3 s.
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| CN202010752610.2A CN111676440A (en) | 2020-07-30 | 2020-07-30 | Preparation method of tantalum oxide in-situ composite tantalum-based nanocrystalline wear-resistant and anti-friction coating |
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| CN202010752610.2A CN111676440A (en) | 2020-07-30 | 2020-07-30 | Preparation method of tantalum oxide in-situ composite tantalum-based nanocrystalline wear-resistant and anti-friction coating |
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Citations (3)
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|---|---|---|---|---|
| WO2016181213A1 (en) * | 2015-05-13 | 2016-11-17 | Oerlikon Metco (Japan) Ltd. | Power for thermal spraying, thermal spraying method, and thermally sprayed coating |
| CN106947935A (en) * | 2017-05-09 | 2017-07-14 | 中国科学院兰州化学物理研究所 | A kind of method that thermal spraying prepares wear-resistant coating |
| CN110075354A (en) * | 2018-01-26 | 2019-08-02 | 中国科学院上海硅酸盐研究所 | A kind of tantalum base coating and its preparation method and application with significant rush cell Osteoblast Differentiation performance |
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- 2020-07-30 CN CN202010752610.2A patent/CN111676440A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016181213A1 (en) * | 2015-05-13 | 2016-11-17 | Oerlikon Metco (Japan) Ltd. | Power for thermal spraying, thermal spraying method, and thermally sprayed coating |
| CN106947935A (en) * | 2017-05-09 | 2017-07-14 | 中国科学院兰州化学物理研究所 | A kind of method that thermal spraying prepares wear-resistant coating |
| CN110075354A (en) * | 2018-01-26 | 2019-08-02 | 中国科学院上海硅酸盐研究所 | A kind of tantalum base coating and its preparation method and application with significant rush cell Osteoblast Differentiation performance |
Non-Patent Citations (1)
| Title |
|---|
| 李英: "微纳多级结构钽复合涂层的制备及生物性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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