CN112048741B - Si3N4Preparation method and application of/Ni titanium alloy blade tip protective coating - Google Patents
Si3N4Preparation method and application of/Ni titanium alloy blade tip protective coating Download PDFInfo
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- CN112048741B CN112048741B CN201910487507.7A CN201910487507A CN112048741B CN 112048741 B CN112048741 B CN 112048741B CN 201910487507 A CN201910487507 A CN 201910487507A CN 112048741 B CN112048741 B CN 112048741B
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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
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
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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
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
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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
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/38—Pretreatment of metallic surfaces to be electroplated of refractory metals or nickel
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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
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
- C25D5/505—After-treatment of electroplated surfaces by heat-treatment of electroplated tin coatings, e.g. by melting
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/70—Wind energy
- Y02E10/72—Wind turbines with rotation axis in wind direction
Abstract
The invention belongs to the technical field of protective coating deposition on the surface of a metal material, and particularly relates to Si3N4A preparation method and application of a/Ni titanium alloy blade tip protective coating. Firstly, preparing a nickel activation layer on a titanium alloy matrix through a process of preactivating and charging a base material into a groove; then preparing Si on the active layer by utilizing a composite electrodeposition technology3N4Ni coating and finally subjecting the coating to vacuum heat treatment. Mixing Si3N4the/Ni titanium alloy blade tip protective coating is applied to surface protection of a titanium alloy blade tip and is used for improving the sealing performance of a gas turbine engine. The titanium alloy blade tip protective coating related by the invention is successfully synthesized, and the coating has higher film-base bonding strength and wear resistance, and has important significance for theoretical research and practical application of the wear-resistant sealing coating.
Description
The technical field is as follows:
the invention belongs to the technical field of protective coating deposition on the surface of a metal material, and particularly relates to Si3N4A preparation method and application of a/Ni titanium alloy blade tip protective coating.
Background art:
the titanium alloy has the characteristics of high specific strength, low density, good elasticity resistance, good molding processability and the like, and also has better corrosion resistance and heat resistance, so the titanium alloy is applied to the aviation industry from the beginning of birth. Today, titanium alloy blades and parts are used in large numbers in the compressor sector of aircraft engines. However, when the engine is running, the linear speed of the blade tip of the airplane blade is high, and usually reaches more than 300m/s, and the blade tip and the sealing coating are subjected to severe friction. The method not only leads the blade to be greatly worn and greatly shortens the service life of the airplane blade, but also easily causes titanium fire due to severe friction because of poor thermal conductivity of the titanium alloy. Therefore, the preparation of hard wear-resistant coatings on the tips of titanium alloy blades is an effective way to solve the above problems.
The composite electroplating technology has the characteristics of low synthesis temperature, convenience in operation, small limitation on the size and the shape of a workpiece and the like, and is suitable for processing the compressor blade with a complex shape. However, titanium is a very active metal and is easily oxidized in air and aqueous solutions to form a titania ceramic film. This oxide film not only inhibits further electroplating, but also causes poor interface matching between the coating and the metal, making it difficult to obtain a coating having good adhesion. Currently, the most used method for this problem is pre-plating the surface of the titanium alloy substrate, and the key to the pre-treatment is to form a suitable "active film" on the surface. However, when the use temperature of the active film is higher, the active film is slowly decomposed, and the coating is easy to fall off, so that the method can not meet the requirement of the titanium alloy blade in a middle-temperature service environment. Therefore, there is a need to invent a pretreatment method suitable for electroplating titanium alloy blades to obtain higher film-based bonding strength and titanium alloy blade tip protective coating to prevent titanium fire and prolong the service life of the blades.
Disclosure of Invention
The invention aims to provide Si3N4The preparation method and the application of the/Ni titanium alloy blade tip protective coating are characterized in that the Si is prepared by combining a composite electroplating technology with a process of preactivation, charged groove and heat treatment3N4The protective coating for the/Ni titanium alloy blade tip effectively solves the problems of a titanium alloy matrix and Si3N4The poor interface matching of the/Ni coating ensures that the sealing protective coating deposited by electroplating has higher wear resistance and film-base bonding strength.
The technical scheme of the invention is as follows:
si3N4Firstly, preparing a pure nickel activation layer on a substrate by utilizing a process of preactivation and charged groove entering; then preparing Si by utilizing composite electrodeposition technology3N4Ni coating and finally subjecting the as-deposited coating to vacuum heat treatment.
Said Si3N4A preparation method of a/Ni titanium alloy blade tip protective coating is provided, wherein a substrate is a titanium alloy.
Said Si3N4Preparation method of/Ni titanium alloy blade tip protective coating, Si3N4The particle size range of the particles is 40-70 mu m.
Said Si3N4The preparation method of the protective coating of the/Ni titanium alloy blade tip comprises the steps of testing the binding force of the protective coating by adopting a tensile test method, and testing the binding force of the protective coating by adopting a tensile test method3N4The binding force of the/Ni coating reaches more than 50 MPa.
Said Si3N4Preparation method of/Ni titanium alloy blade tip protective coating and deposited Si3N4The Ni coating is subjected to heat treatment to obtain wear-resistant Si3N4The protective coating for the/Ni titanium alloy blade tip has a friction coefficient of 0.3-0.5 at normal temperature.
Said Si3N4The preparation method of the/Ni titanium alloy blade tip protective coating specifically comprises the following steps:
(1) the pretreatment process comprises the following steps: the titanium alloy base material is required to be pretreated before deposition, and the specific process comprises the following steps: firstly, sequentially polishing a matrix by using 240#, 400#, 600# and 800# sandpaper, then carrying out dry spraying treatment on the surface of the matrix by using 300-mesh aluminum oxide, then respectively carrying out ultrasonic cleaning for 10-30 min by using acetone and alcohol, and drying;
(2) the method adopts a process of preactivation and charged entry to deposit the nickel activation layer, and comprises the following specific processes: before plating, etching and cleaning the titanium alloy substrate for 30-90 s by using 15-25 vol% hydrochloric acid; then connecting the substrate to the negative electrode of a power supply, putting the substrate into a watt liquid plating tank after electrifying to deposit a pure nickel activation layer with the thickness of 3-5 mu m; wherein the current is denseThe degree is 1 to 5A/dm2The temperature of the watt liquid in the plating tank is 30-50 ℃;
(3) fixing Si by composite electroplating technology3N4The hard particles comprise the following specific processes: uniformly arranging a layer of Si on the surface of the workpiece deposited with the nickel activation layer3N4Hard particles are put into the watt liquid for composite electroplating, the temperature of the watt liquid in the electroplating bath is 30-50 ℃, and the current density is 0.5-2A/dm2The time is 0.1-1 h; taking out the workpiece after a specified time, brushing off the unfixed hard particles on the surface layer, putting the workpiece into the watt liquid again for thickening, wherein the workpiece is a cathode, and the anode is a pure nickel plate;
(4) and after deposition, washing and drying by distilled water, and carrying out vacuum annealing at 400-500 ℃ for 20-50 h.
Said Si3N4The preparation method of the/Ni titanium alloy blade tip protective coating comprises the step (2) and the step (3), wherein the deposition time is set according to the thickness of a required coating.
Said Si3N4The preparation method of the/Ni titanium alloy blade tip protective coating comprises the following steps of (2) and (3) and the watt liquid comprises the following components: 240-250 g/L of nickel sulfate, 35-50 g/L of nickel chloride, 35-40 g/L of boric acid, 0.4-0.6 g/L of saccharin sodium, 0.1-0.2 g/L of sodium dodecyl sulfate and the balance of water.
Said Si3N4The preparation method of the/Ni titanium alloy blade tip protective coating comprises the following steps of (3) thickening electroplating technological parameters: the temperature of the watt liquid in the electroplating bath is 30-50 ℃, and the current density is 0.5-2A/dm2The time is 3-5 h.
Said Si3N4Use of a/Ni titanium alloy blade tip protective coating, Si3N4the/Ni titanium alloy blade tip protective coating is applied to surface protection of a titanium alloy blade tip and is used for improving the sealing performance of a gas turbine engine.
The design idea of the invention is as follows:
the invention adopts the composite electrodeposition technology to prepare Si on the titanium alloy substrate3N4a/Ni protective coating. "Pre-activation + Charge incorporation" as referred to in the present inventionThe process of groove and heat treatment solves the problem of poor electroplating binding force on the titanium alloy base material, and the final binding force can reach more than 50 MPa. Si added to the coating3N4The hard particles not only have better lubricating effect, but also can endow the coating with excellent cutting performance so as to achieve the effect of protecting the tip of the titanium alloy blade. The coating base material is Ni, has better oxidation resistance and other performances at the temperature of below 500 ℃, has strong heat conductivity, can avoid titanium fire in the high-speed scraping process, and can meet the service environment of the existing titanium alloy blade.
The invention has the following advantages and beneficial effects:
1. the titanium alloy blade tip protective coating prepared by the invention has the advantages that the binding force between the coating and the base material is more than 50MPa, the average friction coefficient of the coating is about 0.4, and the coating has excellent wear resistance.
2. The invention provides a process of preactivation, charged slot and heat treatment, which solves the problems of titanium alloy matrix and Si3N4The problem that the interface matching performance of the Ni coating is poor is solved, and technical support is provided for the application of the sealing coating deposited by adopting an electroplating technology to the titanium alloy blade of the aeroengine.
3. The titanium alloy blade tip protection protective coating related by the invention can be applied to surface protection of the titanium alloy blade tip of an aircraft engine, can prevent titanium fire and can effectively prolong the service life of the titanium alloy blade.
4. The titanium alloy blade tip protective coating related by the invention is successfully synthesized, and the coating has higher film-base bonding strength and wear resistance, and has important significance for theoretical research and practical application of the wear-resistant sealing coating.
Description of the drawings:
FIG. 1 is Si3N4And the sectional appearance diagram of the/Ni titanium alloy blade tip protective coating.
FIG. 2 is Si3N4The X-ray diffraction pattern of the/Ni titanium alloy blade tip protective coating. In the figure, the abscissa 2 θ represents the diffraction angle (°), and the ordinate Intensity represents the relative Intensity (a.u ℃).
FIG. 3 is Si3N4The friction coefficient of the/Ni titanium alloy blade tip protective coating changes along with time. In the figure, the abscissa Time represents the Time (min) and the ordinate Friction coeffient represents the Friction coefficient.
The specific implementation mode is as follows:
in the concrete implementation process, the Si of the invention3N4The preparation method of the/Ni titanium alloy blade tip protective coating comprises the following process flows of: firstly, preparing a nickel activation layer on a titanium alloy matrix through a process of preactivating and charging a base material into a groove; then preparing Si on the active layer by utilizing a composite electrodeposition technology3N4a/Ni coating, finally subjecting the coating to a vacuum heat treatment, Si3N4The total thickness of the/Ni titanium alloy blade tip protective coating is 40-50 mu m.
The present invention will be described in further detail below by way of examples.
Example 1
The base material adopts TC6 titanium alloy, the titanium alloy base material needs to be pretreated before deposition, and the specific process is as follows: firstly, sequentially grinding a matrix by using 240#, 400#, 600# and 800# sandpaper, then carrying out dry spraying treatment on the surface of the matrix by using 300-mesh aluminum oxide, then respectively carrying out ultrasonic cleaning for 20min by using acetone and alcohol, and drying.
Preparing a nickel activation layer by adopting a process of preactivating and charging into a groove: putting the pretreated TC6 titanium alloy substrate into 20 vol% hydrochloric acid to be soaked for 60-90 s, and performing pre-activation before plating; then connecting the substrate to the negative electrode of a power supply, putting the substrate into a watt liquid plating tank after electrifying to deposit a pure nickel activation layer. Wherein, the specific technological parameters of the preplating Ni are as follows: the cathode-anode distance is 3cm, and the current density is 3A/dm2The temperature of the watt liquid is 45 ℃, the workpiece is used as a cathode, the anode is a pure nickel target, the time is 5min, and the thickness of the pure nickel activation layer is 5 mu m.
(II) preparing Si by composite electrodeposition3N4The protective coating of the/Ni titanium alloy blade tip: uniformly arranging a layer of Si on the surface of the workpiece plated with the pure nickel activation layer3N4Placing the hard particles into a watt liquid for composite electroplating, wherein Si3N4The particle size of the hard particles is 40-70 mu m, and the specific electroplating process parameters are as follows: the distance between the anode and the cathode is 3cm, and the current density is 0.6A/dm2The temperature of the watt liquid is 45 ℃ for 1 h. Taking out the workpiece after 1 hour, brushing off the unfixed hard particles on the surface of the workpiece, and then putting the workpiece into a watt liquid for thickening, wherein the electroplating technological parameters are as follows: the distance between the anode and the cathode is 3cm, and the current density is 0.6A/dm2The time is 5h, the temperature of the watt liquid is 45 ℃, and the Si in a deposition state is formed3N4the/Ni composite coating.
The watt liquid comprises the following components: 240g/L of nickel sulfate, 35g/L of nickel chloride, 40g/L of boric acid, 0.6g/L of saccharin sodium, 0.2g/L of sodium dodecyl sulfate and the balance of water.
After the composite electrodeposition is finished, washing and drying by distilled water, and then carrying out Si deposition3N4the/Ni composite coating is annealed for 24 hours in vacuum at 400 ℃.
Plating of Si on one side of TC6 substrate3N4the/Ni composite coating is measured by a tensile test method, and the bonding force between the coating and a substrate is 52 MPa.
As shown in FIG. 1, Si3N4Cross-sectional morphology of the/Ni coating, Si3N4The particles are uniformly distributed, and are partially embedded in the coating, and partially exposed outside; the coating has compact structure and uniform thickness distribution. The total thickness of the coating was about 45 μm.
As shown in figure 2, the phase composition in the coating is detected by XRD, and the surface structure of the coating is mainly Ni phase and Si phase3N4And (4) forming.
Example 2
The base material adopts TC4 titanium alloy, the titanium alloy base material needs to be pretreated before deposition, and the specific process is as follows: firstly, sequentially grinding a matrix by using 240#, 400#, 600# and 800# sandpaper, then carrying out dry spraying treatment on the surface of the matrix by using 300-mesh aluminum oxide, then respectively carrying out ultrasonic cleaning for 20min by using acetone and alcohol, and drying.
Preparing a nickel activation layer by adopting a process of preactivating and charging into a groove: putting the pretreated TC4 titanium alloy substrate into 20 vol% hydrochloric acid for preactivation for 30-60 s; then connecting the substrate to the negative pole of a power supply, putting the substrate into watt liquid after electrifyingDepositing pure nickel activation layer in the plating bath. Wherein, the specific technological parameters of the preplating Ni are as follows: the cathode-anode distance is 3cm, and the current density is 2A/dm2The temperature of the watt liquid is 40 ℃, the workpiece is used as a cathode, the anode is a pure nickel target, the time is 3min, and the thickness of the pure nickel activation layer is 3 mu m.
(II) preparing Si by composite electrodeposition3N4The protective coating of the/Ni titanium alloy blade tip: then a layer of Si is uniformly arranged on the surface of the workpiece plated with the pure nickel activation layer3N4Placing the hard particles into a watt liquid for composite electroplating, wherein Si3N4The particle size of the hard particles is 40-70 mu m, and the specific electroplating process parameters are as follows: the cathode-anode distance is 3cm, and the current density is 0.8A/dm2The time is 1h, and the temperature of the watt liquid is 40 ℃. Taking out the workpiece after 1 hour, brushing off the unfixed hard particles on the surface of the workpiece, and then putting the workpiece into a watt liquid for thickening, wherein the electroplating technological parameters are as follows: the distance between the anode and the cathode is 3cm, and the current density is 0.8A/dm2At a watt temperature of 40 ℃ for 5h, forming Si in a deposited state with a total thickness of about 40 mu m3N4the/Ni composite coating. Si3N4The particles are uniformly distributed, and are partially embedded in the coating, and partially exposed outside; the coating has compact structure and uniform thickness distribution.
The watt liquid comprises the following components: 250g/L of nickel sulfate, 40g/L of nickel chloride, 40g/L of boric acid, 0.6g/L of saccharin sodium, 0.2g/L of sodium dodecyl sulfate and the balance of water.
After the composite electrodeposition is finished, washing and drying by distilled water, and then carrying out Si deposition3N4the/Ni composite coating is annealed for 48 hours in vacuum at 400 ℃.
Adopting an MS-T3000 type ball disc type friction wear testing machine to carry out treatment on TC4 matrix, as-deposited Si and as-annealed Si3N4The tribological behavior of the/Ni composite coatings was tested. FIG. 3 shows that the counter grinding pair is Al2O3And the friction factor under the working conditions of load 250g, rotating speed 500r/min, radius 3mm and friction time 2 min. After the test, no obvious grinding mark is seen on the surface of the workpiece, which shows that the coating has excellent wear resistance. As shown in FIG. 3, the coating had a coefficient of friction curve with time of friction having an average coefficient of friction of 0.36 and a wear ofLow loss rate and excellent wear resistance.
The results of the examples show that the invention successfully prepares Si by a composite electrodeposition process3N4The coating has good film-substrate binding force and excellent frictional wear, can obviously improve the low wear resistance of the titanium alloy blade, and has important significance for protecting the titanium alloy blade, prolonging the service life of the blade, reducing the occurrence probability of titanium fire and improving the thrust-weight ratio of an engine.
Claims (5)
1. Si3N4The preparation method of the/Ni titanium alloy blade tip protective coating is characterized in that firstly, a pure nickel activation layer is prepared on a matrix by utilizing a process of preactivation and charged groove entering; then preparing Si by utilizing composite electrodeposition technology3N4a/Ni coating, and finally carrying out vacuum heat treatment on the deposition-state coating;
the matrix is titanium alloy, Si3N4The particle size range of the particles is 40-70 mu m;
the method specifically comprises the following steps:
(1) the pretreatment process comprises the following steps: the titanium alloy base material is required to be pretreated before deposition, and the specific process comprises the following steps: firstly, sequentially polishing a matrix by using 240#, 400#, 600# and 800# sandpaper, then carrying out dry spraying treatment on the surface of the matrix by using 300-mesh aluminum oxide, then respectively carrying out ultrasonic cleaning for 10-30 min by using acetone and alcohol, and drying;
(2) the nickel activation layer is deposited by adopting a process of preactivating and charging into a groove, and the specific process comprises the following steps: before plating, etching and cleaning the titanium alloy substrate for 30-90 s by using 15-25 vol% hydrochloric acid; then connecting the substrate to the negative electrode of a power supply, putting the substrate into a watt liquid plating tank after electrifying to deposit a pure nickel activation layer with the thickness of 3-5 mu m; wherein the current density is 1-5A/dm2The temperature of the watt liquid in the plating tank is 30-50 ℃;
(3) fixing Si by composite electroplating technology3N4The hard particles comprise the following specific processes: uniformly arranging a layer of Si on the surface of the workpiece deposited with the nickel activation layer3N4Hard particles are put into watt liquid for composite electroplating and electroplating bathThe temperature of the medium watt liquid is 30-50 ℃, and the current density is 0.5-2A/dm2The time is 0.1-1 h; taking out the workpiece after a specified time, brushing off the unfixed hard particles on the surface layer, putting the workpiece into the watt liquid again for thickening, wherein the workpiece is a cathode, and the anode is a pure nickel plate;
(4) after deposition, washing and drying by distilled water, and carrying out vacuum annealing at 400-500 ℃ for 20-50 h;
Si3N4the particles are uniformly distributed, and are partially embedded in the coating and partially exposed outside; compact coating structure, uniform thickness distribution, Si3N4The total thickness of the/Ni titanium alloy blade tip protective coating is 40-50 mu m;
the bonding force of the protective coating is tested by adopting a tensile test method, and Si3N4The bonding force of the/Ni coating reaches more than 50 MPa;
as-deposited Si3N4The Ni coating is subjected to heat treatment to obtain wear-resistant Si3N4The protective coating for the/Ni titanium alloy blade tip has a friction coefficient of 0.3-0.5 at normal temperature.
2. Si according to claim 13N4The preparation method of the/Ni titanium alloy blade tip protective coating is characterized in that in the step (2) and the step (3), the deposition time is set according to the thickness of the required coating.
3. Si according to claim 13N4The preparation method of the/Ni titanium alloy blade tip protective coating is characterized in that in the step (2) and the step (3), the watt liquid comprises the following components: 240-250 g/L of nickel sulfate, 35-50 g/L of nickel chloride, 35-40 g/L of boric acid, 0.4-0.6 g/L of saccharin sodium, 0.1-0.2 g/L of sodium dodecyl sulfate and the balance of water.
4. Si according to claim 13N4The preparation method of the/Ni titanium alloy blade tip protective coating is characterized in that in the step (3), thickened electroplating technological parameters are as follows: the temperature of the watt liquid in the electroplating bath is 30-50 DEG CThe current density is 0.5-2A/dm2The time is 3-5 h.
5. Si according to any one of claims 1 to 43N4The application of the/Ni titanium alloy blade tip protective coating is characterized in that Si3N4the/Ni titanium alloy blade tip protective coating is applied to surface protection of a titanium alloy blade tip and is used for improving the sealing performance of a gas turbine engine.
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