CN113122844A - Method for preparing composite coating on surface of nickel-based alloy through micro-arc oxidation and plasma sputtering - Google Patents
Method for preparing composite coating on surface of nickel-based alloy through micro-arc oxidation and plasma sputtering Download PDFInfo
- Publication number
- CN113122844A CN113122844A CN202110457355.3A CN202110457355A CN113122844A CN 113122844 A CN113122844 A CN 113122844A CN 202110457355 A CN202110457355 A CN 202110457355A CN 113122844 A CN113122844 A CN 113122844A
- Authority
- CN
- China
- Prior art keywords
- micro
- arc oxidation
- nickel
- based alloy
- plasma sputtering
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
- C23C28/321—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer with at least one metal alloy layer
- C23C28/3215—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer with at least one metal alloy layer at least one MCrAlX layer
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
-
- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
- C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
-
- 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
-
- 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
- C25D11/34—Anodisation of metals or alloys not provided for in groups C25D11/04 - C25D11/32
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Inorganic Chemistry (AREA)
- Electrochemistry (AREA)
- Physical Vapour Deposition (AREA)
- Coating By Spraying Or Casting (AREA)
Abstract
The invention provides a method for preparing a composite coating on the surface of a nickel-based alloy by micro-arc oxidation-plasma sputtering, which comprises the following steps: (1) firstly, placing a nickel-based alloy matrix in electrolyte for micro-arc oxidation to form a micro-arc oxidation ceramic film layer on the surface of the nickel-based alloy; (2) and then carrying out plasma sputtering on the nickel-based alloy subjected to micro-arc oxidation to form a NiCrAlY coating on the surface of the micro-arc oxidation ceramic coating. The preparation method provided by the invention has the advantages of simple and convenient operation, low energy consumption, low cost and good environment-friendly effect, and the NiCrAlY coating in the prepared composite coating has good combination with the micro-arc oxidation ceramic coating, good chemical stability, high mechanical strength and high temperature resistance, not only can solve the phenomenon that the protective coating and the matrix in a high-temperature environment for a long time generate element mutual diffusion, but also has good combination with the matrix, and improves the mechanical strength and the high-temperature stability of the nickel-based high-temperature alloy part.
Description
Technical Field
The invention relates to the technical field of alloy surface treatment, in particular to a method for preparing a composite coating on the surface of a nickel-based alloy by micro-arc oxidation-plasma sputtering.
Background
The nickel-based alloy has excellent performances of stable structure, strong oxidation resistance, high working temperature and the like, and can still maintain higher strength and good oxidation resistance at the melting point temperature of 85 percent (up to 650-1000 ℃) of the alloy, so that the nickel-based alloy is widely applied to hot end parts of aero-engines, industrial gas turbines and the like. In modern aircraft engines, the amount of nickel-based alloy used is about 80% of the total mass of the engine. Because the nickel-based alloy part is in service in severe working environments such as high temperature, high fuel gas corrosion, cyclic load, vibration, high thrust-weight ratio and the like for a long time, the nickel-based alloy part is easy to damage, the normal use and the service safety of the equipment are severely limited, and great loss is brought to the national economic development.
How to increase the service temperature and prolong the service life of the nickel-based alloy has been a hot point of research. The high-temperature protective coating can generate larger temperature drop between the nickel-based alloy and high-temperature fuel gas and is similar to an isolation layer, so that the high-temperature protective coating can not directly act on the surface of a part substrate under a high-temperature working medium, and the substrate is effectively protected. The high-temperature protective coating which is in a high-temperature environment for a long time can generate mutual diffusion of elements with the substrate, on one hand, Kirkendall holes formed near the interface of the coating/the substrate reduce the performance of the coating, and on the other hand, the high-temperature creep resistance of the substrate can be degraded.
Micro-arc oxidation, also known as plasma oxidation or anodic spark deposition, is different from ordinaryThe method is a new technology for growing a ceramic oxide film in situ by carrying out spark discharge on the surface of metal such as Al, Mg, Ti and the like in a non-stretching region. In brief, plasma discharge is generated under the action of high voltage and pulse power supply, so that a thin oxide layer is generated on the surface of a substrate. The micro-arc oxidation under an aluminate system can generate Al with the performance similar to that of cemented carbide2O3The film has the characteristics of good wear resistance and high hardness, but the surface of the film is rough. At present, micro-arc oxidation is widely applied to medical machinery, dies, aviation Al, Mg and other parts due to unique advantages, but a method for preparing a ceramic film layer serving as a high-temperature protective coating barrier layer on the surface of a nickel-based alloy through micro-arc oxidation is rarely reported at home and abroad.
Disclosure of Invention
In order to solve the behavior of element mutual diffusion between the protective coating and the matrix in a high-temperature environment for a long time, the invention provides a method for preparing a composite coating on the surface of a nickel-based alloy by micro-arc oxidation-plasma sputtering, which comprises the following steps:
(1) firstly, placing a nickel-based alloy matrix in electrolyte for micro-arc oxidation to form a micro-arc oxidation ceramic film layer on the surface of the nickel-based alloy;
(2) and then carrying out plasma sputtering on the nickel-based alloy subjected to micro-arc oxidation to form a NiCrAlY coating on the surface of the micro-arc oxidation ceramic coating.
Before micro-arc oxidation, the nickel-based alloy is firstly polished by metallographic abrasive paper until the surface of the nickel-based alloy is free of scratches, and then is subjected to acid cleaning and drying.
Wherein the electrolyte is aluminum nitrate alcohol solution.
Wherein, in the electrolyte, the concentration of the aluminum nitrate is 0.05-0.11 mol/L.
Wherein the process parameters of the micro-arc oxidation are as follows: the frequency of the pulse power supply is 500HZ, the dead time is 5%, and the positive duty ratio and the negative duty ratio are 45% and-45% respectively.
The adjustable range of the voltage is 400V-500V, when the nickel-based alloy is broken down, violent arc discharge occurs in the reaction tank, the adjustable reaction time of micro-arc oxidation is 20min-120min, the voltage and the current are adjusted to 0 after the reaction is finished, a closing button on a micro-arc oxidation pulse power supply touch screen is clicked, the sample is cooled to the room temperature along with the reaction tank, and a micro-arc oxidation ceramic film layer is formed on the surface of the nickel-based alloy.
And slowly increasing the voltage in the micro-arc oxidation process until the voltage is kept unchanged after arc discharge.
The method comprises the following steps of putting a sample subjected to micro-arc oxidation into a plasma sputtering instrument, and putting a NiCrAlY target above the sample, wherein in the plasma sputtering process, parameters of a cathode pulse power supply are as follows: the voltage regulation range is 400-600V, the current regulation range is 1-2A, and the duty ratio is 80%.
In the plasma sputtering process, the parameters of the anode pulse power supply are as follows: the voltage regulation range is 700-900V, the current regulation range is 1-2A, and the duty ratio is 80%.
Wherein, the plasma sputtering is carried out in a vacuum environment, and the adjustable range of the working air pressure is 15-50 Pa.
The invention has the beneficial effects that:
the preparation method of the composite coating provided by the invention has the advantages of simple and convenient operation, low energy consumption, low cost and good environment-friendly effect, and the NiCrAlY coating and the micro-arc oxidation ceramic coating in the prepared composite coating are well combined, have good chemical stability, high mechanical strength and high temperature resistance, can not only solve the behavior that elements are mutually diffused between the protective coating and a matrix in a high-temperature environment for a long time, but also be well combined with the matrix, and improve the mechanical strength and the high-temperature stability of the nickel-based high-temperature alloy part.
Drawings
In order to more clearly illustrate the technical solution of the present invention, the drawings used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it should be obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a sectional SEM image of a composite coating prepared by the method provided in example 3 of the invention;
fig. 2 is an XRD spectrum of the composite coating prepared by the method provided in example 3 of the present invention.
Detailed Description
The following is a preferred embodiment of the present invention, and it should be noted that it is obvious to those skilled in the art that various modifications and improvements can be made without departing from the principle of the present invention, and these modifications and improvements are also considered to be within the scope of the present invention.
Example 1
The invention provides a method for preparing a composite coating on the surface of a nickel-based alloy by micro-arc oxidation-plasma sputtering, which comprises the following steps:
(1) grinding the Inconel718 nickel-based alloy plate with the size of 12mm multiplied by 4mm multiplied by 2mm after wire cutting to W10 (800 meshes) by using metallographic abrasive paper until the surface has no scratch, and carrying out acid washing and drying to obtain an experimental sample;
(2) firstly, weighing 28g of aluminum nitrate by using an electronic balance, dissolving the aluminum nitrate in alcohol, and then fixing the volume by using a 1L volumetric flask to obtain 0.074mol/L aluminum nitrate alcohol electrolytic solution;
(3) pouring the electrolytic solution prepared in the step (2) into a reaction tank, opening a stirring blade switch, fixing the sample obtained in the step (1) at a position 1-2cm below the liquid level of the electrolytic solution in the reaction tank by using a sample clamp, opening cooling water communicated with the reaction tank to reduce the temperature during reaction, connecting an anode jaw with the reaction tank, and connecting a cathode jaw with the sample clamp;
(4) opening a WH-10 type micro-arc oxidation pulse power supply, setting the frequency of 500HZ, the dead zone time of 5 percent and the positive and negative duty ratios of 45 percent and-45 percent respectively on a touch screen in the middle of the pulse power supply, and screwing a current knob below the touch screen to the maximum current of 4.5A by adopting a constant current method to regulate and control the voltage to obtain experimental parameters;
(5) clicking a start button on a touch screen to gradually increase the voltage until the voltage is 430V, when the nickel-based alloy is broken down, generating violent arc discharge in a reaction tank, keeping the voltage micro-arc oxidation for 90min, adjusting the voltage and the current to 0, and clicking a close button on a micro-arc oxidation pulse power supply touch screen to cool a sample to room temperature along with the reaction tank, so as to form a micro-arc oxidation ceramic film layer on the surface of the nickel-based alloy;
(6) placing the sample after micro-arc oxidation into a plasma sputtering instrument, placing a NiCrAlY target material above the sample, and performing the process under vacuum with the vacuum degree of 1 x 10-4And adjusting parameters of the cathode pulse power supply as follows: voltage 423V, current 1.59A, duty cycle 80%, frequency 45.1HZ, and anode pulse power supply parameters were adjusted as follows: the voltage 839V, the current of 1.28A, the duty ratio of 80 percent and the frequency of 45.2HZ form a NiCrAlY coating on the surface of the micro-arc oxidation ceramic coating.
Example 2
The invention provides a method for preparing a composite coating on the surface of a nickel-based alloy by micro-arc oxidation-plasma sputtering, which comprises the following steps:
(1) grinding the Inconel718 nickel-based alloy plate with the size of 12mm multiplied by 4mm multiplied by 2mm after wire cutting to W10 (800 meshes) by using metallographic abrasive paper until the surface has no scratch, and carrying out acid washing and drying to obtain an experimental sample;
(2) firstly, weighing 28g of aluminum nitrate by using an electronic balance, dissolving the aluminum nitrate in alcohol, and then fixing the volume by using a 1L volumetric flask to obtain 0.074mol/L aluminum nitrate alcohol electrolytic solution;
(3) pouring the electrolytic solution prepared in the step (2) into a reaction tank, opening a stirring blade switch, fixing the sample obtained in the step (1) at a position 1-2cm below the liquid level of the electrolytic solution in the reaction tank by using a sample clamp, opening cooling water communicated with the reaction tank to reduce the temperature during reaction, connecting an anode jaw with the reaction tank, and connecting a cathode jaw with the sample clamp;
(4) opening a WH-10 type micro-arc oxidation pulse power supply, setting the frequency of 500HZ, the dead zone time of 5 percent and the positive and negative duty ratios of 45 percent and-45 percent respectively on a touch screen in the middle of the pulse power supply, and screwing a current knob below the touch screen to the maximum current of 4.5A by adopting a constant current method to regulate and control the voltage to obtain experimental parameters;
(5) clicking a start button on a touch screen, gradually increasing the voltage until the voltage is 430V, when the nickel-based alloy is broken down, generating violent arc discharge in a reaction tank, continuously and slowly increasing the voltage to 450V, keeping the voltage for microarc oxidation for 90min, adjusting the voltage and the current to 0, clicking a close button on a microarc oxidation pulse power supply touch screen, cooling a sample to room temperature along with the reaction tank, and forming a microarc oxidation ceramic film layer on the surface of the nickel-based alloy;
(6) placing the sample after micro-arc oxidation into a plasma sputtering instrument, placing a NiCrAlY target material above the sample, and performing the process under vacuum with the vacuum degree of 1 x 10-4And adjusting parameters of the cathode pulse power supply as follows: voltage 423V, current 1.59A, duty cycle 80%, frequency 45.1HZ, and anode pulse power supply parameters were adjusted as follows: the voltage 839V, the current of 1.28A, the duty ratio of 80 percent and the frequency of 45.2HZ form a NiCrAlY coating on the surface of the micro-arc oxidation ceramic coating.
Example 3
The invention provides a method for preparing a composite coating on the surface of a nickel-based alloy by micro-arc oxidation-plasma sputtering, which comprises the following steps:
(1) grinding the Inconel718 nickel-based alloy plate with the size of 12mm multiplied by 4mm multiplied by 2mm after wire cutting to W10 (800 meshes) by using metallographic abrasive paper until the surface has no scratch, and carrying out acid washing and drying to obtain an experimental sample;
(2) firstly, weighing 28g of aluminum nitrate by using an electronic balance, dissolving the aluminum nitrate in alcohol, and then fixing the volume by using a 1L volumetric flask to obtain 0.074mol/L aluminum nitrate alcohol electrolytic solution;
(3) pouring the electrolytic solution prepared in the step (2) into a reaction tank, opening a stirring blade switch, fixing the sample obtained in the step (1) at a position 1-2cm below the liquid level of the electrolytic solution in the reaction tank by using a sample clamp, opening cooling water communicated with the reaction tank to reduce the temperature during reaction, connecting an anode jaw with the reaction tank, and connecting a cathode jaw with the sample clamp;
(4) opening a WH-10 type micro-arc oxidation pulse power supply, setting the frequency of 500HZ, the dead zone time of 5 percent and the positive and negative duty ratios of 45 percent and-45 percent respectively on a touch screen in the middle of the pulse power supply, and screwing a current knob below the touch screen to the maximum current of 4.5A by adopting a constant current method to regulate and control the voltage to obtain experimental parameters;
(5) clicking a start button on a touch screen, gradually increasing the voltage until the voltage is 430V, when the nickel-based alloy is broken down, generating violent arc discharge in a reaction tank, continuously and slowly increasing the voltage to 470V, keeping the voltage for microarc oxidation for 90min, adjusting the voltage and the current to 0, and clicking a close button on a microarc oxidation pulse power supply touch screen, so that a sample is cooled to room temperature along with the reaction tank, and forming a microarc oxidation ceramic film layer on the surface of the nickel-based alloy;
(6) placing the sample after micro-arc oxidation into a plasma sputtering instrument, placing a NiCrAlY target material above the sample, and performing the process under vacuum with the vacuum degree of 1 x 10-4And adjusting parameters of the cathode pulse power supply as follows: voltage 423V, current 1.59A, duty cycle 80%, frequency 45.1HZ, and anode pulse power supply parameters were adjusted as follows: the voltage 839V, the current of 1.28A, the duty ratio of 80 percent and the frequency of 45.2HZ form a NiCrAlY coating on the surface of the micro-arc oxidation ceramic coating.
Fig. 1 is a cross-sectional SEM image of a composite coating prepared by the method provided in example 3 of the present invention, as is apparent from the figure: micro-arc oxidized Al with clear interface2O3The ceramic coating and the NiCrAlY coating, the NiCrAlY coating and the micro-arc oxidation ceramic coating are combined tightly without obvious defects.
Fig. 2 is an XRD spectrum of the composite coating prepared by the method provided in example 3 of the present invention, and it can be seen from the graph: the phase of the composite coating is AlNi and Cr2Ni3The intermetallic compound and the micro-arc oxidation ceramic layer are mainly composed of alpha-Al2O3Phase and small amount of gamma-Al2O3Phase composition, alpha-Al2O3The phase performance is stable, the catalyst belongs to low-activity alumina, almost has no catalytic activity, and is insoluble in water, strong acid and strong alkali solutions.
Example 4
The invention provides a method for preparing a composite coating on the surface of a nickel-based alloy by micro-arc oxidation-plasma sputtering, which comprises the following steps:
(1) grinding the Inconel718 nickel-based alloy plate with the size of 12mm multiplied by 4mm multiplied by 2mm after wire cutting to W10 (800 meshes) by using metallographic abrasive paper until the surface has no scratch, and carrying out acid washing and drying to obtain an experimental sample;
(2) firstly, weighing 24g of aluminum nitrate by using an electronic balance, dissolving the aluminum nitrate in alcohol, and then fixing the volume by using a 1L volumetric flask to obtain 0.064mol/L aluminum nitrate alcohol electrolytic solution;
(3) pouring the electrolytic solution prepared in the step (2) into a reaction tank, opening a stirring blade switch, fixing the sample obtained in the step (1) at a position 1-2cm below the liquid level of the electrolytic solution in the reaction tank by using a sample clamp, opening cooling water communicated with the reaction tank to reduce the temperature during reaction, connecting an anode jaw with the reaction tank, and connecting a cathode jaw with the sample clamp;
(4) opening a WH-10 type micro-arc oxidation pulse power supply, setting the frequency of 500HZ, the dead zone time of 5 percent and the positive and negative duty ratios of 45 percent and-45 percent respectively on a touch screen in the middle of the pulse power supply, and screwing a current knob below the touch screen to the maximum current of 4.5A by adopting a constant current method to regulate and control the voltage to obtain experimental parameters;
(5) clicking a start button on a touch screen to gradually increase the voltage until the voltage is 420V, when the nickel-based alloy is broken down, generating violent arc discharge in a reaction tank, keeping the voltage micro-arc oxidation for 60min, adjusting the voltage and the current to 0, and clicking a close button on a micro-arc oxidation pulse power supply touch screen to cool a sample to room temperature along with the reaction tank, so as to form a micro-arc oxidation ceramic film layer on the surface of the nickel-based alloy;
(6) placing the sample after micro-arc oxidation into a plasma sputtering instrument, placing a NiCrAlY target material above the sample, and performing the process under vacuum with the vacuum degree of 1 x 10-4And adjusting parameters of the cathode pulse power supply as follows: the voltage is 450V, the current is 1.2A, the duty ratio is 80%, the frequency is 45.1HZ, and the parameters of the anode pulse power supply are regulated as follows: the voltage is 750V, the current is 1.68A, the duty ratio is 80%, the frequency is 45.2HZ, and a NiCrAlY coating is formed on the surface of the micro-arc oxidation ceramic coating.
Example 5
The invention provides a method for preparing a composite coating on the surface of a nickel-based alloy by micro-arc oxidation-plasma sputtering, which comprises the following steps:
(1) grinding the Inconel718 nickel-based alloy plate with the size of 12mm multiplied by 4mm multiplied by 2mm after wire cutting to W10 (800 meshes) by using metallographic abrasive paper until the surface has no scratch, and carrying out acid washing and drying to obtain an experimental sample;
(2) firstly, weighing 20g of aluminum nitrate by using an electronic balance, dissolving the aluminum nitrate in alcohol, and then using a 1L volumetric flask to fix the volume to obtain 0.064mol/L aluminum nitrate alcohol electrolytic solution;
(3) pouring the electrolytic solution prepared in the step (2) into a reaction tank, opening a stirring blade switch, fixing the sample obtained in the step (1) at a position 1-2cm below the liquid level of the electrolytic solution in the reaction tank by using a sample clamp, opening cooling water communicated with the reaction tank to reduce the temperature during reaction, connecting an anode jaw with the reaction tank, and connecting a cathode jaw with the sample clamp;
(4) opening a WH-10 type micro-arc oxidation pulse power supply, setting the frequency of 500HZ, the dead zone time of 5 percent and the positive and negative duty ratios of 45 percent and-45 percent respectively on a touch screen in the middle of the pulse power supply, and screwing a current knob below the touch screen to the maximum current of 4.5A by adopting a constant current method to regulate and control the voltage to obtain experimental parameters;
(5) clicking a start button on a touch screen to gradually increase the voltage until the voltage is 450V, when the nickel-based alloy is broken down, generating violent arc discharge in a reaction tank, keeping the voltage micro-arc oxidation for 60min, adjusting the voltage and the current to 0, and clicking a close button on a micro-arc oxidation pulse power supply touch screen to cool a sample to room temperature along with the reaction tank, so as to form a micro-arc oxidation ceramic film layer on the surface of the nickel-based alloy;
(6) placing the sample after micro-arc oxidation into a plasma sputtering instrument, placing a NiCrAlY target material above the sample, and performing the process under vacuum with the vacuum degree of 1 x 10-4And adjusting parameters of the cathode pulse power supply as follows: the voltage is 500V, the current is 1.55A, the duty ratio is 80%, the frequency is 45.1HZ, and the parameters of the anode pulse power supply are adjusted as follows: the voltage is 800V, the current is 1.4A, the duty ratio is 80%, the frequency is 45.2HZ, and a NiCrAlY coating is formed on the surface of the micro-arc oxidation ceramic membrane layer.
Example 6
The invention provides a method for preparing a composite coating on the surface of a nickel-based alloy by micro-arc oxidation-plasma sputtering, which comprises the following steps:
(1) grinding the Inconel718 nickel-based alloy plate with the size of 12mm multiplied by 4mm multiplied by 2mm after wire cutting to W10 (800 meshes) by using metallographic abrasive paper until the surface has no scratch, and carrying out acid washing and drying to obtain an experimental sample;
(2) firstly, weighing 32g of aluminum nitrate by using an electronic balance, dissolving the aluminum nitrate in alcohol, and then using a 1L volumetric flask to fix the volume to obtain 0.085mol/L aluminum nitrate alcohol electrolytic solution;
(3) pouring the electrolytic solution prepared in the step (2) into a reaction tank, opening a stirring blade switch, fixing the sample obtained in the step (1) at a position 1-2cm below the liquid level of the electrolytic solution in the reaction tank by using a sample clamp, opening cooling water communicated with the reaction tank to reduce the temperature during reaction, connecting an anode jaw with the reaction tank, and connecting a cathode jaw with the sample clamp;
(4) opening a WH-10 type micro-arc oxidation pulse power supply, setting the frequency of 500HZ, the dead zone time of 5 percent and the positive and negative duty ratios of 45 percent and-45 percent respectively on a touch screen in the middle of the pulse power supply, and screwing a current knob below the touch screen to the maximum current of 4.5A by adopting a constant current method to regulate and control the voltage to obtain experimental parameters;
(5) clicking a start button on a touch screen, gradually increasing the voltage until the voltage is 470V, when the nickel-based alloy is broken down, generating violent arc discharge in a reaction tank, keeping the voltage micro-arc oxidation for 60min, adjusting the voltage and the current to 0, clicking a close button on a micro-arc oxidation pulse power supply touch screen, cooling a sample to room temperature along with the reaction tank, and forming a micro-arc oxidation ceramic film layer on the surface of the nickel-based alloy;
(6) placing the sample after micro-arc oxidation into a plasma sputtering instrument, placing a NiCrAlY target material above the sample, and performing the process under vacuum with the vacuum degree of 1 x 10-4And adjusting parameters of the cathode pulse power supply as follows: the voltage is 600V, the current is 1.48A, the duty ratio is 80%, the frequency is 45.1HZ, and the parameters of the anode pulse power supply are regulated as follows: the voltage is 850V, the current is 1.4A, the duty ratio is 80%, the frequency is 45.2HZ, and a NiCrAlY coating is formed on the surface of the micro-arc oxidation ceramic coating.
Example 7
The invention provides a method for preparing a composite coating on the surface of a nickel-based alloy by micro-arc oxidation-plasma sputtering, which comprises the following steps:
(1) grinding the Inconel718 nickel-based alloy plate with the size of 12mm multiplied by 4mm multiplied by 2mm after wire cutting to W10 (800 meshes) by using metallographic abrasive paper until the surface has no scratch, and carrying out acid washing and drying to obtain an experimental sample;
(2) firstly, 41g of aluminum nitrate is weighed by an electronic balance and dissolved in alcohol, and then a 1L volumetric flask is used for constant volume to obtain 0.11mol/L aluminum nitrate alcohol electrolytic solution;
(3) pouring the electrolytic solution prepared in the step (2) into a reaction tank, opening a stirring blade switch, fixing the sample obtained in the step (1) at a position 1-2cm below the liquid level of the electrolytic solution in the reaction tank by using a sample clamp, opening cooling water communicated with the reaction tank to reduce the temperature during reaction, connecting an anode jaw with the reaction tank, and connecting a cathode jaw with the sample clamp;
(4) opening a WH-10 type micro-arc oxidation pulse power supply, setting the frequency of 500HZ, the dead zone time of 5 percent and the positive and negative duty ratios of 45 percent and-45 percent respectively on a touch screen in the middle of the pulse power supply, and screwing a current knob below the touch screen to the maximum current of 4.5A by adopting a constant current method to regulate and control the voltage to obtain experimental parameters;
(5) clicking a start button on a touch screen to gradually increase the voltage until the voltage is 490V, when the nickel-based alloy is broken down, generating violent arc discharge in a reaction tank, keeping the voltage for micro-arc oxidation for 60min, adjusting the voltage and the current to 0, clicking a close button on a micro-arc oxidation pulse power supply touch screen to cool a sample to room temperature along with the reaction tank, and forming a micro-arc oxidation ceramic film layer on the surface of the nickel-based alloy;
(6) placing the sample after micro-arc oxidation into a plasma sputtering instrument, placing a NiCrAlY target material above the sample, and performing the process under vacuum with the vacuum degree of 1 x 10-4And adjusting parameters of the cathode pulse power supply as follows: the voltage is 550V, the current is 1.6A, the duty ratio is 80%, the frequency is 45.1HZ, and the parameters of the anode pulse power supply are regulated as follows: the voltage is 850V, the current is 1.8A, the duty ratio is 80%, the frequency is 45.2HZ, and a NiCrAlY coating is formed on the surface of the micro-arc oxidation ceramic coating.
The above examples only express the specific embodiments of the present invention, and the description thereof is more specific and detailed, but not to be construed as limiting the scope of the present invention. It should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the spirit of the present invention, and these changes and modifications are all within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A method for preparing a composite coating on the surface of a nickel-based alloy by micro-arc oxidation-plasma sputtering is characterized by comprising the following steps:
(1) firstly, placing a nickel-based alloy matrix in electrolyte for micro-arc oxidation to form a micro-arc oxidation ceramic film layer on the surface of the nickel-based alloy;
(2) and then carrying out plasma sputtering on the nickel-based alloy subjected to micro-arc oxidation to form a NiCrAlY coating on the surface of the micro-arc oxidation ceramic coating.
2. The method for preparing the composite coating on the surface of the nickel-based alloy by the micro-arc oxidation-plasma sputtering method according to claim 1, wherein the method comprises the following steps: before the micro-arc oxidation of the nickel-based alloy, firstly, the surface of the nickel-based alloy is polished by metallographic abrasive paper until no scratch is formed on the surface, and then, the nickel-based alloy is subjected to acid cleaning and drying.
3. The method for preparing the composite coating on the surface of the nickel-based alloy by the micro-arc oxidation-plasma sputtering method according to claim 1, wherein the method comprises the following steps: the electrolyte is aluminum nitrate alcohol solution.
4. The method for preparing the composite coating on the surface of the nickel-based alloy by the micro-arc oxidation-plasma sputtering method according to claim 3, wherein the method comprises the following steps: in the electrolyte, the concentration of the aluminum nitrate is 0.05-0.11 mol/L.
5. The method for preparing the composite coating on the surface of the nickel-based alloy by the micro-arc oxidation-plasma sputtering according to any one of claims 1 to 4, wherein the process parameters of the micro-arc oxidation are as follows: the frequency of the pulse power supply is 500HZ, the dead time is 5%, and the positive duty ratio and the negative duty ratio are 45% and-45% respectively.
6. The method for preparing the composite coating on the surface of the nickel-based alloy by the micro-arc oxidation-plasma sputtering method according to claim 5, wherein the method comprises the following steps: the adjustable range of the voltage is 400V-500V, when the nickel-based alloy is broken down, violent arc discharge occurs in the reaction tank, the adjustable reaction time of the micro-arc oxidation is 20min-120min, the voltage and the current are adjusted to 0 after the reaction is finished, and a closing button on a micro-arc oxidation pulse power supply touch screen is clicked, so that the sample is cooled to the room temperature along with the reaction tank, and a micro-arc oxidation ceramic film layer is formed on the surface of the nickel-based alloy.
7. The method for preparing the composite coating on the surface of the nickel-based alloy by the micro-arc oxidation-plasma sputtering method according to claim 6, wherein the method comprises the following steps: and slowly increasing the voltage in the micro-arc oxidation process until the voltage is kept unchanged after arc discharge.
8. The method for preparing the composite coating on the surface of the nickel-based alloy by the micro-arc oxidation-plasma sputtering according to any one of claims 1 to 4, which is characterized in that: placing the sample subjected to micro-arc oxidation into a plasma sputtering instrument, and placing a NiCrAlY target material above the sample, wherein in the plasma sputtering process, parameters of a cathode pulse power supply are as follows: the voltage regulation range is 400-600V, the current regulation range is 1-2A, and the duty ratio is 80%.
9. The method for preparing the composite coating on the surface of the nickel-based alloy by the micro-arc oxidation-plasma sputtering according to any one of claims 1 to 4, wherein in the plasma sputtering process, the parameters of an anode pulse power supply are as follows: the voltage regulation range is 700-900V, the current regulation range is 1-2A, and the duty ratio is 80%.
10. The method for preparing the composite coating on the surface of the nickel-based alloy by the micro-arc oxidation-plasma sputtering according to any one of claims 1 to 4, which is characterized in that: the plasma sputtering is carried out in a vacuum environment, and the adjustable range of working air pressure is 15-50 Pa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110457355.3A CN113122844A (en) | 2021-04-27 | 2021-04-27 | Method for preparing composite coating on surface of nickel-based alloy through micro-arc oxidation and plasma sputtering |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110457355.3A CN113122844A (en) | 2021-04-27 | 2021-04-27 | Method for preparing composite coating on surface of nickel-based alloy through micro-arc oxidation and plasma sputtering |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113122844A true CN113122844A (en) | 2021-07-16 |
Family
ID=76780300
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110457355.3A Pending CN113122844A (en) | 2021-04-27 | 2021-04-27 | Method for preparing composite coating on surface of nickel-based alloy through micro-arc oxidation and plasma sputtering |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113122844A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115852367A (en) * | 2022-12-06 | 2023-03-28 | 西北有色金属研究院 | Method for preparing high-corrosion-resistance conductive composite coating on surface of magnesium alloy |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020037220A1 (en) * | 2000-09-25 | 2002-03-28 | Snecma Moteurs | Method of making a protective coating forming a thermal barrier with a bonding underlayer on a superalloy substrate, and a part obtained thereby |
| RU2007146968A (en) * | 2007-12-20 | 2009-06-27 | Федеральное государственное унитарное предприятие "Московское машиностроительное производственное предприятие "Салют" (RU) | METHOD FOR PRODUCING MULTILAYER HEAT PROTECTIVE COATING ON PARTS FROM HEAT-RESISTANT ALLOYS |
| CN102925841A (en) * | 2012-11-07 | 2013-02-13 | 天津大学 | Ceramic thermal barrier coating with allitic diffusion layer bonding layer and preparation method thereof |
| CN103590008A (en) * | 2013-11-28 | 2014-02-19 | 铜陵学院 | Preparation method for Al2O3 diffusion barrier between TiAl alloy and MCrAlY coating |
| CN105401147A (en) * | 2015-11-04 | 2016-03-16 | 西安交通大学 | High-temperature corrosion-resistant coating containing aluminum oxide diffusion barriers and preparation method for high-temperature corrosion-resistant coating |
| CN111593394A (en) * | 2020-07-15 | 2020-08-28 | 南昌航空大学 | Preparation method and application of nickel-based alloy nickel-rhenium-aluminum oxide diffusion barrier |
| CN112342592A (en) * | 2020-10-23 | 2021-02-09 | 南昌航空大学 | Method for preparing ceramic film layer on surface of nickel-based alloy through micro-arc oxidation |
-
2021
- 2021-04-27 CN CN202110457355.3A patent/CN113122844A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020037220A1 (en) * | 2000-09-25 | 2002-03-28 | Snecma Moteurs | Method of making a protective coating forming a thermal barrier with a bonding underlayer on a superalloy substrate, and a part obtained thereby |
| RU2007146968A (en) * | 2007-12-20 | 2009-06-27 | Федеральное государственное унитарное предприятие "Московское машиностроительное производственное предприятие "Салют" (RU) | METHOD FOR PRODUCING MULTILAYER HEAT PROTECTIVE COATING ON PARTS FROM HEAT-RESISTANT ALLOYS |
| CN102925841A (en) * | 2012-11-07 | 2013-02-13 | 天津大学 | Ceramic thermal barrier coating with allitic diffusion layer bonding layer and preparation method thereof |
| CN103590008A (en) * | 2013-11-28 | 2014-02-19 | 铜陵学院 | Preparation method for Al2O3 diffusion barrier between TiAl alloy and MCrAlY coating |
| CN105401147A (en) * | 2015-11-04 | 2016-03-16 | 西安交通大学 | High-temperature corrosion-resistant coating containing aluminum oxide diffusion barriers and preparation method for high-temperature corrosion-resistant coating |
| CN111593394A (en) * | 2020-07-15 | 2020-08-28 | 南昌航空大学 | Preparation method and application of nickel-based alloy nickel-rhenium-aluminum oxide diffusion barrier |
| CN112342592A (en) * | 2020-10-23 | 2021-02-09 | 南昌航空大学 | Method for preparing ceramic film layer on surface of nickel-based alloy through micro-arc oxidation |
Non-Patent Citations (8)
| Title |
|---|
| J. MULLER ET AL.: ""Chemical vapor deposition of smooth α-Al2O3 films on nickel base superalloys as diffusion barriers"", 《SURFACE AND COATINGS TECHNOLOGY》 * |
| S.H.HOSSEINI ET AL.: ""Investigating efficiency of a-Al2O3 diffusion barrier layer in oxidation of EB-PVD NiCrAlY coatings"", 《SURFACE ENGINEERING》 * |
| U. ERITT WT AL.: ""Investigations on the Deposition and the Efficiency of a Multilayer High Temperature Coating System for Gas Turbine Blades"", 《MAT.-WISS. U. WERKSTOFFTECH》 * |
| 于萍等: "镍基单晶高温合金扩散阻挡层的研究进展", 《材料导报》 * |
| 孙可为等: "镍基合金高温扩散阻挡层的研究进展", 《材料导报》 * |
| 廖健等: "《铝合金挤压材生产与应用》", 31 March 2018, 冶金工业出版社 * |
| 张晓囡等: "热障涂层界面扩散阻挡层研究进展", 《材料导报》 * |
| 戴永年等: "《有色金属材料的真空冶金》", 31 March 2000, 冶金工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115852367A (en) * | 2022-12-06 | 2023-03-28 | 西北有色金属研究院 | Method for preparing high-corrosion-resistance conductive composite coating on surface of magnesium alloy |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104562128B (en) | A kind of method for preparing thermal protection ceramic layer on metal or metallic composite surface | |
| CN102174704B (en) | Preparation method for tantalum-contained interlayer metallic oxide electrode | |
| US11572627B2 (en) | Molten Al—Si alloy corrosion resistant composite coating and preparation method and application thereof | |
| CN106637071B (en) | A kind of method that multisection type pack cementation aluminizing combination differential arc oxidation prepares composite coating | |
| CN103590008B (en) | One is coated with interlayer in TiAl alloy and MCrAlY and prepares Al 2o 3the method of diffusion barrier | |
| CN102154673A (en) | Method for preparing environment-friendly micro-arc oxidation black ceramic film on aluminum alloy surface | |
| CN106252682A (en) | Fuel battery metal pole plate multiple phase coating of suppression column crystal and preparation method thereof | |
| CN106637354A (en) | Preparation method of micro-arc oxidation film layer on surface of beryllium and beryllium-aluminum alloy | |
| CN110055477A (en) | A kind of nanoporous ni-based amorphous alloy material and its application in water electrolysis hydrogen production | |
| CN113122844A (en) | Method for preparing composite coating on surface of nickel-based alloy through micro-arc oxidation and plasma sputtering | |
| CN107937874B (en) | A method of Pt-Al high-temperature protection coating is prepared on niobium alloy surface | |
| CN108707922A (en) | A kind of flexible nano is porous/amorphous composite material and preparation method thereof | |
| CN103147112B (en) | A kind of electrolytic solution and for the preparation of the purposes of nuclear fuel rod zirconium alloy cladding micro-arc oxidation films and method | |
| CN114481048A (en) | High-conductivity corrosion-resistant amorphous/nanocrystalline composite coexistent coating and preparation method and application thereof | |
| CN100486007C (en) | Process for preparing integrated renewable fuel double effect oxygen electrode diffusion layer | |
| Wang et al. | Investigation of commercial aluminum alloys as anode materials for alkaline aluminum–air batteries | |
| Chai et al. | Effect of electrical parameters on the growth and properties of 7075 aluminum alloy film based on scanning micro-arc oxidation with mesh electrode | |
| CN112048752A (en) | Preparation method and application of cBN/Ni-Mo titanium alloy blade tip protective coating | |
| CN112342592A (en) | Method for preparing ceramic film layer on surface of nickel-based alloy through micro-arc oxidation | |
| CN111394771B (en) | Method for preparing coating on surface of copper and copper alloy and copper product | |
| CN109136981A (en) | A kind of FeCo base metal glass film elctro-catalyst and the preparation method and application thereof | |
| CN103469278B (en) | A kind of electrolyte of preparing for zirconium alloy cladding diaphragm and micro-arc oxidation process | |
| CN105967740B (en) | A kind of laser melting coating and the chemical de- compound method for preparing micro nano structure block silicon materials of alloy | |
| CN104611679B (en) | Nanocrystalline ZrC/Zr composite coatings of one proton exchanging film fuel battery titanium alloy bipolar plates and preparation method thereof | |
| CN106544627B (en) | A kind of thermophilic corrosion-resistance composite coating and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |