CN108265292A - A kind of titanium alloy surface composite coating and its preparation method and application - Google Patents

A kind of titanium alloy surface composite coating and its preparation method and application Download PDF

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Publication number
CN108265292A
CN108265292A CN201810172242.7A CN201810172242A CN108265292A CN 108265292 A CN108265292 A CN 108265292A CN 201810172242 A CN201810172242 A CN 201810172242A CN 108265292 A CN108265292 A CN 108265292A
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China
Prior art keywords
coating
titanium alloy
flame retardant
heat insulating
present
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CN201810172242.7A
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Inventor
汪瑞军
马小斌
詹华
王亦奇
鲍曼雨
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Beijing Golden Wheel Special Machine C Ltd
Chinese Academy of Agricultural Mechanization Sciences
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Beijing Golden Wheel Special Machine C Ltd
Chinese Academy of Agricultural Mechanization Sciences
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Priority to CN201810172242.7A priority Critical patent/CN108265292A/en
Publication of CN108265292A publication Critical patent/CN108265292A/en
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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
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    • 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
    • C23C28/343—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 DLC or an amorphous carbon based layer, the layer being doped or not
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
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    • 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
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • C23C16/27—Diamond only
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    • 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
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
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    • 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
    • C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
    • C23C26/02—Coating not provided for in groups C23C2/00 - C23C24/00 applying molten material to the substrate
    • 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
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    • 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
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    • 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
    • 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
    • C23C28/3455—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 with a refractory ceramic layer, e.g. refractory metal oxide, ZrO2, rare earth oxides or a thermal barrier system comprising at least one refractory oxide 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
    • 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
    • C23C4/073—Metallic material containing MCrAl or MCrAlY alloys, where M is nickel, cobalt or iron, with or without non-metal elements
    • 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
    • C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
    • C23C4/11—Oxides
    • 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
    • C23C4/129—Flame spraying
    • 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

Abstract

The present invention provides a kind of titanium alloy surface composite coating, including being arranged on the flame retardant coating on titanium alloy substrate surface, being arranged on the heat insulating coat of the flame retardant coating upper surface and being arranged on the infrared stealth coating of the heat insulating coat upper surface；Wherein, the flame retardant coating is by Ti40Zr25Ni3Cu12Be20It is formed；The heat insulating coat is by ZrO2‑Y2O3It is formed；The infrared stealth coating is diamond-like DLC coatings.The composite coating has had both fire-retardant, heat-insulated and infrared stealth function, meanwhile, the composite coating also shows excellent thermal shock resistance.Preparation method and its application in aerospace parts the present invention also provides the titanium alloy surface composite coating.

Description

A kind of titanium alloy surface composite coating and its preparation method and application
Technical field
The present invention relates to titanium alloy surfaces to be modified field more particularly to a kind of titanium alloy surface composite coating and its preparation side Method and application.
Background technology
Titanium alloy is since specific strength and specific modulus are high, density is low, survivability is strong, in calming the anger for advanced aero engine There is huge application prospect on the aerospace parts such as machine casing, blade.But it due to titanium alloy under high temperature environment, is acutely rubbed Meeting catching fire during wiping, and can spread rapidly, titanium fire accident occurs, seriously constrains titanium alloy in advanced aero engine Application.Meanwhile in recent years, infrared acquisition and guidance technology are developed rapidly, such as airborne Infrared Search and Track System (IRST) it is close with the operating distance of airborne radar to the forward detection of fighter plane distance up to 185 kms or so, to aircraft The threat of getting worse is constituted, there is an urgent need to have infrared stealth function for titanium alloy surface coating.
In the prior art, the technology relative maturity of heat insulating coat is prepared using plasma spraying, but does not have flame retardant property And infrared stealth function, can not meet the needs of it is in aviation field.
Invention content
The purpose of the present invention is to provide a kind of titanium alloy surface composite coatings and its preparation method and application, existing to solve There is the problem of titanium alloy surface modification can not meet fire-retardant, heat-insulated and infrared stealth complex function in technology.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical scheme：
A kind of titanium alloy surface composite coating, described in being arranged on the flame retardant coating on titanium alloy substrate surface, being arranged on The heat insulating coat of flame retardant coating upper surface and the infrared stealth coating for being arranged on the heat insulating coat upper surface；
Wherein, the flame retardant coating is by Ti40Zr25Ni3Cu12Be20It is formed；
The heat insulating coat is by ZrO2-Y2O3It is formed；
The infrared stealth coating is diamond-like DLC coatings.
Preferably, the thickness of the flame retardant coating is 0.1~0.15mm.
Preferably, the thickness of the heat insulating coat is 0.20~0.25mm.
Preferably, the thickness of the infrared stealth coating is 0.004~0.008mm.
Preferably, NiCrAlY tie coats, the NiCrAlY mistakes are further included between the flame retardant coating and heat insulating coat The thickness for crossing coating is 0.08~0.10mm.
The present invention also provides the preparation methods of the titanium alloy surface composite coating, include the following steps：
Using electric spark deposition method titanium alloy substrate surface depositing Ti40Zr25Ni3Cu12Be20, form flame retardant coating；
Using plasma spraying method the flame retardant coating surface spraying ZrO2-Y2O3, form heat insulating coat；
Diamond-like DLC coatings are prepared on the surface of the heat insulating coat using plasma reinforced chemical vapour deposition method, As infrared stealth coating, titanium alloy surface composite coating is obtained.
Preferably, the voltage during the electric spark deposition method be 60~100V, discharge frequency be 1000~2000Hz, Discharge capacity is 40~120 μ F.
Preferably, in the surface depositing Ti of titanium alloy substrate40Zr25Ni3Cu12Be20It is further included after forming flame retardant coating：It adopts With supersonic flame spraying method NiCrAlY tie coats are prepared on the surface of the flame retardant coating.
Preferably, the plasma reinforced chemical vapour deposition method is gradient transition method.
The present invention also provides the titanium alloy surface composite coating or the titanium alloys being prepared by above-mentioned preparation method Application of the surface composite coating in aerospace parts.
The present invention provides a kind of titanium alloy surface composite coating, the fire-retardant painting including being arranged on titanium alloy substrate surface Layer is arranged on the heat insulating coat of the flame retardant coating upper surface and is arranged on the infrared stealth painting of the heat insulating coat upper surface Layer；Wherein, the flame retardant coating is by Ti40Zr25Ni3Cu12Be20It is formed；The heat insulating coat is by ZrO2-Y2O3It is formed；It is described red Outer camouflage coating is diamond-like DLC coatings.In titanium alloy surface composite coating of the present invention Ti40Zr25Ni3Cu12Be20Flame retardant coating has good titanium fire preventing performance, ZrO2-Y2O3Heat insulating coat has excellent thermal insulation Can, diamond-like DLC coatings have excellent infrared stealth performance；The composite coating had both it is fire-retardant, heat-insulated with it is infrared hidden Body function, the initiation temperature of the titanium alloy surface composite coating is 600 DEG C or more, and 600 DEG C of heat insulation is 90 DEG C, Room temperature, the infrared emittance of 200 DEG C, 400 DEG C 8~14 μm of wave bands are respectively：0.42nd, 0.585,0.577, it is infrared hidden less than existing The infrared emittance of body coating.Meanwhile the composite coating also shows excellent thermal shock resistance, is subjected to 75 thermal shocks and follows Ring, complex function disbonding is less than 10%.
The present invention also provides the preparation method of the titanium alloy surface composite coating, the present invention uses electric spark deposition method The Ti being prepared40Zr25Ni3Cu12Be20Flame retardant coating not only has titanium fire preventing flame retarding function, is also formed with titanium alloy substrate micro- Metallurgical binding has ensured that complex function coating has the bond strength of up to 30MPa, what plasma spraying method was prepared ZrO2-Y2O3Heat insulating coat has excellent heat-proof quality, the DLC coatings that plasma reinforced chemical vapour deposition method is prepared With excellent infrared stealth performance, and so that its infrared emittance is minimum.Can preferably it be applied in aerospace parts.
Description of the drawings
Fig. 1 is the structure diagram of the titanium alloy surface composite coating；
Fig. 2 is the metallograph in the titanium alloy surface composite coating section.
Specific embodiment
The present invention provides a kind of titanium alloy surface composite coating, the fire-retardant painting including being arranged on titanium alloy substrate surface Layer is arranged on the heat insulating coat of the flame retardant coating upper surface and is arranged on the infrared stealth painting of the heat insulating coat upper surface Layer；
Wherein, the flame retardant coating is by Ti40Zr25Ni3Cu12Be20It is formed；
The heat insulating coat is by ZrO2-Y2O3It is formed；
The infrared stealth coating is diamond-like DLC coatings.
In the present invention, if without specified otherwise, all raw material components are well known to the skilled person commercially available Product.
Titanium alloy surface composite coating provided by the invention includes the flame retardant coating for being arranged on titanium alloy substrate surface, described Flame retardant coating is by Ti40Zr25Ni3Cu12Be20It is formed；In the present invention, the thickness of the flame retardant coating be preferably 0.1~ 0.15mm, more preferably 0.12~0.14mm.In the specific embodiment of the invention, the thickness of the flame retardant coating can be specially 0.1mm、0.12mm、0.15mm。
The titanium alloy surface composite coating provided by the invention includes being arranged on the heat-insulated of the flame retardant coating upper surface Coating, the heat insulating coat is by ZrO2-Y2O3It is formed；In the present invention, the thickness of the heat insulating coat be preferably 0.20~ 0.25mm, more preferably 0.22~0.23mm.In the specific embodiment of the invention, the thickness of the heat insulating coat can be specially 0.20mm、0.22mm、0.25mm.In the present invention, the Y in the heat insulating coat2O3Mass percent be preferably 7%~ 8%, more preferably 7.2~7.8%.
The titanium alloy surface composite coating provided by the invention includes being arranged on the infrared of the heat insulating coat upper surface Camouflage coating, the infrared stealth coating are diamond-like DLC coatings；In the present invention, the thickness of the infrared stealth coating Preferably 0.004~0.008mm, more preferably 0.005~0.0007mm.It is described infrared hidden in the specific embodiment of the invention The thickness of body coating can be specially 0.004mm, 0.005mm, 0.008mm.
In the present invention, NiCrAlY tie coats are further included between the flame retardant coating and heat insulating coat；In the present invention In, the mass content of Al is preferably 4.5~7.5% in the NiCrAlY tie coats, and more preferably 5~7%；The quality of Y contains Amount preferably 0.5~2.5%, more preferably 1.0~2.0%；The mass content of Cr is preferably 21~23%, and more preferably 21.5 ~22.5%, surplus Ni.
In the present invention, the thickness of the NiCrAlY tie coats is preferably 0.08~0.10mm.Of the invention specific real It applies in example, the thickness of the NiCrAlY tie coats can be specially 0.08mm, 0.09mm, 0.10mm.
The present invention also provides the preparation methods of the titanium alloy surface composite coating, include the following steps：
Using electric spark deposition method titanium alloy substrate surface depositing Ti40Zr25Ni3Cu12Be20, form flame retardant coating；
Using plasma spraying method the flame retardant coating surface spraying ZrO2-Y2O3, form heat insulating coat；
Diamond-like DLC coatings are prepared on the surface of the heat insulating coat using plasma reinforced chemical vapour deposition method, As infrared stealth coating, titanium alloy surface composite coating is obtained.
The present invention uses electric spark deposition method in the surface depositing Ti of titanium alloy substrate40Zr25Ni3Cu12Be20, formed fire-retardant Coating.The present invention preferably cleans titanium alloy with alcohol before using electric spark deposition method deposition flame retardant coating in pond is cleaned by ultrasonic Matrix surface, and dry up；In the present invention, the scavenging period is preferably 3~7 minutes, more preferably 4~6 minutes.In this hair In bright, the electric spark deposition method preferably carries out in an inert atmosphere, is carried out more preferably in argon gas atmosphere；In the present invention In, the flow of the inert atmosphere gases is preferably 10~20L/min, more preferably 12~18L/min, most preferably 14~ 16L/min。
In the present invention, the discharge capacity of the deposition process is preferably 40~120 μ F.In the present invention, the electric discharge Capacitance is preferably the process of a gradual change, and more preferably discharge capacity reduces step by step after first increasing step by step in the range； In the present invention, the increased process of discharge capacity preferably increases to 120 μ F with the speed of F/ grades of 20~40 μ by 40 μ F, at this Preferably increased in invention specific embodiment with the speed of F/ grades of 40 μ；In the present invention, discharge capacity often increaseds or decreases level-one, Just one layer of flame retardant coating of preferred deposition.
In the present invention, the flame retardant coating of deposition step by step can increase the thickness and compactness of flame retardant coating.
In the present invention, the discharge voltage of the deposition process is preferably 60~100V, more preferably 70~90V, optimal It is selected as 75~85V.
In the present invention, the sedimentation time of the deposition process is preferably 1~5min/cm2, more preferably 2~4min/ cm2。
After obtaining flame retardant coating, the invention also includes use surface system of the supersonic flame spraying method in the flame retardant coating Standby NiCrAlY transition zones.The present invention preferably carries out sandblasting before spraying NiCrAlY transition zones are carried out to obtained flame retardant coating Processing.In the present invention, blasting method well-known to those skilled in the art is selected in the blasting treatment, and obtains rough surface Spend the flame retardant coating for 3~8 μm.
In the present invention, the NiCrAlY transition zones can improve the bond strength of heat insulating coat and bottom, and compensation is heat-insulated The larger gap of coating and flame retardant coating coefficient of thermal expansion improves the thermal shock performance of heat insulating coat.
In the present invention, the fuel employed in the supersonic flame spraying method is preferably kerosene；In the present invention, institute The pressure for stating fuel is preferably 1.73~1.76MPa, more preferably 1.74~1.75MPa.In the present invention, the stream of the fuel Amount is preferably 17~21L/h, more preferably 18~20L/h.In the present invention, employed in the supersonic flame spraying method Combustion-supporting gas is preferably oxygen；In the present invention, the pressure of the combustion-supporting gas is preferably 1.5~1.8MPa, and more preferably 1.6 ~1.7MPa.In the present invention, the flow of the combustion-supporting gas is preferably 36~40m3/ h, more preferably 37~39m3/h.At this In invention, the distance sprayed in the supersonic flame spraying method is preferably 298~302mm, more preferably 299~301mm.
In the present invention, the length of the spray gun gun barrel employed in the supersonic flame spraying method is preferably 100mm.
In the present invention, the pressure of cooling water is preferably 0.5~0.9MPa used in the supersonic flame spraying method, More preferably 0.6~0.8MPa.
After obtaining NiCrAlY tie coats, the present invention uses plasma spraying method in the surface spraying of the flame retardant coating ZrO2-Y2O3, form heat insulating coat.In the present invention, the main gas of plasma employed in the spraying process is preferably argon gas； In the present invention, the pressure of the argon gas is preferably 0.5~0.9MPa, more preferably 0.6~0.9MPa.In the present invention, institute It is preferably 26~28L/min to state argon flow amount, more preferably 26.5~27.5L/min.
In the present invention, the plasma secondary gas employed in the spraying process is preferably hydrogen；In the present invention, institute The pressure for stating hydrogen is preferably 0.2~0.6MPa, more preferably 0.3~0.5MPa.In the present invention, the flow of the hydrogen is excellent It is selected as 85~105L/min, more preferably 90~100L/min.In the present invention, the hydrogen can be improved in spraying process Voltage and spray efficiency.
In the present invention, the cooling gas employed in the spraying process is preferably compressed air, in the present invention, described The pressure for cooling down gas is preferably 0.1~0.5MPa, more preferably 0.2~0.4MPa.
In the present invention, the spray distance in the spraying process is preferably 83~87mm, more preferably 84~86mm. In the present invention, the voltage in the spraying process is preferably 73~77V, more preferably 74~76V；Electric current is preferably 595~ 605A, more preferably 598~602A.
After obtaining heat insulating coat, the present invention is using plasma reinforced chemical vapour deposition method on the surface of the heat insulating coat Diamond-like DLC coatings are prepared, as infrared stealth coating, obtain titanium alloy surface composite coating.In the present invention, it is described etc. Plasma enhanced chemical vapor sedimentation is preferably gradient transition method.
In the present invention, the gradient transition method preferably includes following steps：In ZrO2-Y2O3Heat insulating coat surface is successively Deposit Cr2N transition zones, Cr3C2Transition zone and diamond-like DLC coatings.
In the present invention, the Cr2N transition zones, Cr3C2Transition zone can eliminate the internal stress of diamond-like DLC coatings, Improve the bond strength and corrosion resistance between heat insulating coat and diamond-like DLC coatings.
The present invention is before the plasma reinforced chemical vapour deposition is carried out, preferably ZrO2-Y2O3Heat insulating coat is clear to carrying out It washes.Present invention preferably employs ion beam to the ZrO2-Y2O3Heat insulating coat is cleaned.In the present invention, the cleaning process It is preferred that it carries out in an inert atmosphere；In the present invention, the flow for providing the inert gas of the inert atmosphere is preferably 168~ 172sccm, more preferably 169~171sccm.In the present invention, the inert gas is preferably argon gas.
In the present invention, pressure is preferably 0.8~1.2Pa in the stove of the vacuum drying oven in the cleaning process, more preferably 0.9~1.1Pa.In the present invention, the ion source power during the ion beam cleaning is 1.0~2.0KW, more preferably 1.2~1.8KW, most preferably 1.4~1.6KW.In the present invention, the back bias voltage during the ion beam cleaning is preferably 300~800V, more preferably 400~700V, most preferably 500~600V.In the present invention, the ion beam cleaning process Time is preferably 50~65min, more preferably 53~62min, most preferably 55~58min.
In the present invention, the Cr2In the stove of vacuum drying oven in N transition layer deposition processes pressure be preferably 0.3~ 1.0Pa, more preferably 0.5~0.8Pa, most preferably 0.6~0.7Pa.In the present invention, the Cr2N transition layer deposition processes Employed in protection gas be preferably argon gas；In the present invention, the flow of the protection gas is preferably 168~172sccm, more excellent It is selected as 169~171sccm.In the present invention, the Cr2Reaction gas employed in N transition layer deposition processes is selected as nitrogen； In the present invention, the flow of the reaction gas is preferably 10~60sccm, more preferably 20~50sccm, most preferably 30~ 40sccm。
In the present invention, the Cr2N transition layer deposition processes are preferably unbalanced magnetron sputtering C r.Described non-equilibrium Target power output during magnetron sputtering C r is preferably 12~15kW, more preferably 13~14kW.In the present invention, it is described non-equilibrium The ion source power of magnetron sputtering C r processes is preferably 1.2~1.5kW, more preferably 1.3~1.4kW.In the present invention, it is described The back bias voltage of unbalanced magnetron sputtering C r processes is preferably 0.4~1.0Pa, more preferably 0.5~0.9Pa, most preferably 0.6~ 0.8Pa.In the present invention, the time of the unbalanced magnetron sputtering C r processes is preferably 45~55min, more preferably 48~ 52min。
In the present invention, the Cr3C2In the stove of vacuum drying oven in transition layer deposition process pressure be preferably 0.4~ 1.0Pa, more preferably 0.5~0.8Pa, most preferably 0.6~0.7Pa.In the present invention, the Cr3C2Transition layer deposition process Employed in protection gas be preferably argon gas, it is described protection gas flow be preferably 168~172sccm, more preferably 169~ 171sccm.In the present invention, the Cr3C2Reaction gas employed in transition layer deposition process is preferably CH4, the reaction gas Flow be preferably 70~110sccm, more preferably 80~100sccm, most preferably 85~95sccm.
In the present invention, the Cr3C2Transition layer deposition process is preferably non-balance magnetically controlled sputter transition metal.Described Target power output during unbalanced magnetron sputtering C r is preferably 4~15kW, more preferably 5~13kW, most preferably 8~10kW. In the present invention, the ion source power of the unbalanced magnetron sputtering C r processes is preferably 1.5~1.9kW, more preferably 1.6~ 1.8kW.In the present invention, the back bias voltage of the unbalanced magnetron sputtering C r processes is preferably 98~102Pa, more preferably 99~ 101Pa.In the present invention, the time of the unbalanced magnetron sputtering C r processes is preferably 25~35min, more preferably 28~ 32min。
In the present invention, in the stove of the vacuum drying oven in the diamond-like DLC coating deposition process pressure be preferably 0.2~ 0.6Pa, preferably 0.3~0.5Pa.In the present invention, the protection gas employed in the diamond-like DLC coating deposition process Preferably argon gas, the flow of the protection gas is preferably 168~172sccm, more preferably 169~171sccm.In the present invention In, the reaction gas employed in the diamond-like DLC coating deposition process is preferably CH4, the flow of the reaction gas is preferred For 120~125sccm, more preferably 122~124sccm.In the present invention, in the diamond-like DLC coating deposition process Ion source power be preferably 2.0~2.4kW, more preferably 2.1~2.3kW.In the present invention, the diamond-like DLC is applied Back bias voltage in layer deposition process is preferably 60~90V, more preferably 65~85V, most preferably 70~80V.In the present invention, The sedimentation time of the diamond-like DLC coating deposition process is preferably 75~85min, more preferably 78~82min, most preferably For 79~81min.
It is closed the present invention also provides the titanium alloy surface composite coating or using the titanium that above-mentioned preparation method is prepared Application of the golden watch surface composite coating in aerospace parts.
Titanium alloy surface composite coating provided by the invention is described in detail with reference to embodiment, but cannot be incited somebody to action They are interpreted as limiting the scope of the present invention.
Embodiment 1
Titanium alloy surface is cleaned in pond is cleaned by ultrasonic with alcohol, is dried up after cleaning 5min；
Using electric spark deposition method in titanium alloy surface depositing Ti40Zr25Ni3Cu12Be20, form the resistance that thickness is 0.15mm Coating is fired, the process of the deposition carries out in argon gas atmosphere, and the flow of argon gas is 20L/min, and sets voltage as 60V, frequency Rate is 2KHz, and discharge capacity increases, then reduce step by step step by step from 40 μ F, 80 μ F, 120 μ F, sedimentation time 5min/cm2；
It obtains flame retardant coating and sandblasting is carried out to the flame retardant coating, after obtaining the coating that surface roughness is 6-8 μm, adopt The Ni-22wt%Cr-6wt%Al-2wt%Y tie coats for being 0.08mm with supersonic flame spraying method coating thickness；In Supersonic In fast flame spraying process, basis material Ni-22wt%Cr-6wt%Al-2wt%Y；Fuel is kerosene, controls the stream of kerosene It measures as 19L/h, pressure 1.75MPa；Combustion-supporting gas is oxygen, and the flow for controlling oxygen is 38m3/ h, pressure 1.7MPa；Spray It is 330mm to apply distance；Barrel length is 100mm；Cooling water pressure is 0.7MPa；
After obtaining Ni-22wt%Cr-6wt%Al-2wt%Y tie coats, use plasma spraying method coating thickness for The ZrO of 0.25mm2- 7wt%Y2O3Heat insulating coat；In Plasma Spraying Process Using, the main gas of plasma is argon gas, and pressure is 0.7MPa, flow 27L/min；Plasma secondary gas is hydrogen, and pressure 0.4MPa, flow 95L/min, cooling gas is pressure Contracting air, pressure 0.3MPa, flow 3m3/h；Spray distance is 85mm；Voltage is 75V；Electric current is 600A；
Obtain ZrO2- 7wt%Y2O3After heat insulating coat, using the plasma reinforced chemical vapour deposition legal system of gradient transition The diamond-like DLC infrared stealth coatings that standby thickness is 0.005mm, the excessive method of gradient include the following steps：
First with ion beam cleaning base material, it is 1.0Pa that pressure is controlled in stove in cleaning process, Ar throughputs：170sccm, Ion source power：1.0kW, back bias voltage：300V, time：50min；
Cr2N transition zones deposit：Pressure in stove：0.3Pa, Ar throughput：170sccm, N2Throughput：10sccm, it is non-equilibrium Magnetron sputtering C r, target power output：12kW, ion source power：1.2kW, back bias voltage：120V, time：45min；
Cr3C2Transition zone deposits：Pressure in stove：0.4Pa, Ar throughput：170sccm, CH4Flow：70sccm, it is non-equilibrium Magnetron sputtering C r, target power output：4kW, ion source power：1.5kW, back bias voltage：100V, time：25min；
Diamond-like rock layers deposit：Pressure in stove：0.4Pa, Ar throughput：170sccm, CH4Flow：120sccm, ion source Power：2.0kW, back bias voltage：60V, time：75min；
After the completion of the above process, titanium alloy surface composite coating is obtained.
The concrete structure of the titanium alloy surface composite coating is as shown in Figure 1, complex function coating is divided using three-decker Fire-retardant, heat-insulated and infrared stealth function is not played.Bottom is Ti40Zr25Ni3Cu12Be20Non-crystaline amorphous metal effectively prevent titanium fire to send out It is raw, and form metallurgical binding in titanium alloy substrate；Middle layer is ZrO2(7wt%) Y2O3Coating, heat-insulating capability rise more than 70 DEG C To heat insulating function；It is topmost DLC infrared stealth coatings, there is infrared stealth.
By the titanium alloy surface composite coating carry out Metallographic Analysis, test result as shown in Fig. 2, the metallograph from Left-to-right is followed successively by the Ti of titanium alloy substrate, Bai Liang40Zr25Ni3Cu12Be20Non-crystaline amorphous metal flame retardant coating, porous ZrO2- (7wt%) Y2O3The DLC infrared stealth coatings of heat insulating coat and black.It can be seen that electric spark deposition Ti40Zr25Ni3Cu12Be20 Amorphous alloy layer and matrix and ZrO2(7wt%) Y2O3The interface of sprayed coating is clear；The close plating of DLC coatings is on YSZ coatings Face forms good combination between composite coating and matrix and composite coating.
The titanium alloy composite coating is carried out continuously 75 thermal shock tests according to HB7296-96 standards just to occur slightly shelling Fall, coating surface peel off less than 10%, continuous 6 secondary coating of thermal shock test specified in the standard without peel off crack the defects of As qualified standard improves significantly, considerably beyond qualified number as defined in standard.
It is respectively by infrared emittance of the titanium alloy composite coating in room temperature, 200 DEG C, 400 DEG C 8~14 μm of wave bands： 0.42、0.585、0.577。
Embodiment 2
Titanium alloy surface is cleaned in pond is cleaned by ultrasonic with alcohol, is dried up after cleaning 5min；
Using electric spark deposition method in titanium alloy surface depositing Ti40Zr25Ni3Cu12Be20, form the resistance that thickness is 0.1mm Fire coating, what the process of the deposition carried out in argon gas atmosphere, the flow of argon gas is 20L/min, and set voltage for 60V, Frequency is 2KHz, and discharge capacity increases step by step from 40 μ F, 80 μ F, 120 μ F, then is reduced to 40 μ F step by step, is than sedimentation time 5min/cm2；
It obtains flame retardant coating and sandblasting is carried out to the flame retardant coating, after obtaining the coating that surface roughness is 6~8 μm, Use Ni-22wt%Cr-6wt%Al-2wt%Y tie coat of the supersonic flame spraying method coating thickness for 0.10mm；Super In velocity of sound flame spraying process, basis material Ni-22wt%Cr-6wt%Al-2wt%Y；Fuel is kerosene, controls kerosene Flow is 21L/h, pressure 1.75MPa；Combustion-supporting gas is oxygen, and the flow for controlling oxygen is 40m3/ h, pressure 1.7MPa； Spray distance is 330mm；Barrel length is 100mm；Cooling water pressure is 0.7MPa；.
After obtaining Ni-22wt%Cr-6wt%Al-2wt%Y tie coats, use plasma spraying method coating thickness for The ZrO of 0.20mm2(8wt%) Y2O3Heat insulating coat；In Plasma Spraying Process Using, the main gas of plasma is controlled as argon gas, pressure For 0.7MPa, flow 27L/min；Plasma secondary gas is hydrogen, and pressure 0.4MPa, flow 100L/min cool down gas For compressed air, pressure 0.3MPa, flow 3m3/h；Spray distance is 85mm；Voltage is 77V；Electric current is 605A；
Obtain ZrO2(8wt%) Y2O3After heat insulating coat, using the plasma reinforced chemical vapour deposition method of gradient transition The diamond-like DLC infrared stealth coatings that thickness is 0.008mm are prepared, the excessive method of gradient includes the following steps：
First with ion beam cleaning base material, it is 1.0Pa that pressure is controlled in stove in cleaning process, Ar throughputs：170sccm, Ion source power：2.0kW, back bias voltage：500V, time：50min；
Cr2N transition zones deposit：Pressure in stove：0.6Pa, Ar throughput：170sccm, N2Throughput：30sccm, it is non-equilibrium Magnetron sputtering C r, target power output：15kW, ion source power：1.5kW, back bias voltage：120V, time：50min；
Cr3C2Transition zone deposits：Pressure in stove：0.4Pa, Ar throughput：170sccm, CH4Flow：100sccm, it is non-equilibrium Magnetron sputtering C r, target power output：10kW, ion source power：1.9kW, back bias voltage：100V, time：30min；
Diamond-like rock layers deposit：Pressure in stove：0.4Pa, Ar throughput：170sccm, CH4Flow：123sccm, ion source Power：2.4kW, back bias voltage：70V, time：80min；
After the completion of the above process, titanium alloy surface composite coating is obtained.
The titanium alloy surface composite coating is subjected to Metallographic Analysis, thermal shock resistance test and the test of infrared emittance, Its test result and embodiment 1 are basically identical.
Embodiment 3
Titanium alloy surface is cleaned in pond is cleaned by ultrasonic with alcohol, is dried up after cleaning 5min；
Using electric spark deposition method in titanium alloy surface depositing Ti40Zr25Ni3Cu12Be20, form the resistance that thickness is 0.12mm Coating is fired, what the deposition process carried out in argon gas atmosphere, the flow of argon gas is 20L/min, and sets voltage as 60V, frequency Rate is 2KHz, and discharge capacity increases step by step from 40 μ F, 80 μ F, 120 μ F, then reduces 40 μ F step by step, is 5min/ than sedimentation time cm2；
It obtains flame retardant coating and sandblasting is carried out to the flame retardant coating, after obtaining the coating that surface roughness is 6-8 μm, adopt The tie coat of Ni-22wt%Cr-6wt%Al-2wt%Y for being 0.09mm with supersonic flame spraying method coating thickness；Super In velocity of sound flame spraying process, basis material Ni-22wt%Cr-6wt%Al-2wt%Y；Fuel is kerosene, controls kerosene Flow is 21L/h, pressure 1.75MPa；Combustion-supporting gas is oxygen, and the flow for controlling oxygen is 40m3/ h, pressure 1.7MPa； Spray distance is 330mm；Barrel length is 100mm；Cooling water pressure is 0.7MPa；.
After obtaining Ni-22wt%Cr-6wt%Al-2wt%Y tie coats, use plasma spraying method coating thickness for The ZrO of 0.22mm2(7.5wt%) Y2O3Heat insulating coat；In Plasma Spraying Process Using, the main gas of control plasma is argon gas, is pressed Power is 0.7MPa, flow 27L/min；Plasma secondary gas is hydrogen, and pressure 0.4MPa, flow 105L/min are cooled down Gas is compressed air, pressure 0.3MPa, flow 3m3/h；Spray distance is 85mm；Voltage is 76V；Electric current is 605A；
Obtain ZrO2(7.5wt%) Y2O3After heat insulating coat, using the plasma reinforced chemical vapour deposition of gradient transition Method prepares the diamond-like DLC infrared stealth coatings that thickness is 0.004mm, and the excessive method of gradient includes the following steps：
First with ion beam cleaning base material, it is 1.0Pa that pressure is controlled in stove in cleaning process, Ar throughputs：170sccm, Ion source power：2.0kW, back bias voltage：800V, time：50min；
Cr2N transition zones deposit：Pressure in stove：1.0Pa, Ar throughput：170sccm, N2Throughput：60sccm, it is non-equilibrium Magnetron sputtering C r, target power output：15kW, ion source power：1.5kW, back bias voltage：120V, time：55min；
Cr3C2Transition zone deposits：Pressure in stove：1.0Pa, Ar throughput：170sccm, CH4Flow：110sccm, it is non-equilibrium Magnetron sputtering C r, target power output：15kW, ion source power：1.9kW, back bias voltage：100V, time：35min；
Diamond-like rock layers deposit：Pressure in stove：0.4Pa, Ar throughput：170sccm, CH4Flow：125sccm, ion source Power：2.2kW, back bias voltage：90V, time：85min；
After the completion of the above process, titanium alloy surface composite coating is obtained.
The titanium alloy surface composite coating is subjected to Metallographic Analysis, thermal shock resistance test and the test of infrared emittance, Its test result and embodiment 1 are basically identical.
As can be seen from the above embodiments, composite coating of the present invention is in addition to excellent fire-retardant, heat-insulated and red Other than outer Stealth Fighter, excellent thermal shock resistance is also shown, is subjected to 75 thermal shocks cycle, complex function disbonding is not To 10%, meanwhile, it is respectively in the infrared emittance of room temperature, 200 DEG C, 400 DEG C 8~14 μm of wave bands：0.42、0.585、 0.577, less than the infrared emittance of existing infrared stealth coating.
The above is only the preferred embodiment of the present invention, not makees limitation in any form to the present invention.It should It points out, for those skilled in the art, without departing from the principle of the present invention, if can also make Dry improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.

Claims (10)

1. a kind of titanium alloy surface composite coating, including being arranged on the flame retardant coating on titanium alloy substrate surface, being arranged on the resistance The heat insulating coat of combustion coating upper surface and the infrared stealth coating for being arranged on the heat insulating coat upper surface；
Wherein, the flame retardant coating is by Ti40Zr25Ni3Cu12Be20It is formed；
The heat insulating coat is by ZrO2-Y2O3It is formed；
The infrared stealth coating is diamond-like DLC coatings.
2. titanium alloy surface composite coating as described in claim 1, which is characterized in that the thickness of the flame retardant coating is 0.1 ~0.15mm.
3. titanium alloy surface composite coating as described in claim 1, which is characterized in that the thickness of the heat insulating coat is 0.20 ~0.25mm.
4. titanium alloy surface composite coating as described in claim 1, which is characterized in that the thickness of the infrared stealth coating is 0.004~0.008mm.
5. titanium alloy surface composite coating as described in claim 1, which is characterized in that the flame retardant coating and heat insulating coat it Between further include NiCrAlY tie coats, the thickness of the NiCrAlY tie coats is 0.08~0.10mm.
6. such as the preparation method of Claims 1 to 5 any one of them titanium alloy surface composite coating, include the following steps：
Using electric spark deposition method titanium alloy substrate surface depositing Ti40Zr25Ni3Cu12Be20, form flame retardant coating；
Using plasma spraying method the flame retardant coating surface spraying ZrO2-Y2O3, form heat insulating coat；
Diamond-like DLC coatings are prepared on the surface of the heat insulating coat using plasma reinforced chemical vapour deposition method, as Infrared stealth coating obtains titanium alloy surface composite coating.
7. preparation method as claimed in claim 6, which is characterized in that voltage during the electric spark deposition method for 60~ 100V, discharge frequency are 1000~2000Hz, discharge capacity is 40~120 μ F.
8. preparation method as claimed in claim 6, which is characterized in that deposited on the surface of titanium alloy substrate Ti40Zr25Ni3Cu12Be20It is further included after forming flame retardant coating：Using supersonic flame spraying method on the surface of the flame retardant coating Prepare NiCrAlY tie coats.
9. preparation method as claimed in claim 6, which is characterized in that the plasma reinforced chemical vapour deposition method is gradient Transition method.
10. any one of any one of Claims 1 to 5 titanium alloy surface composite coating or claim 6~9 the preparation side Application of the titanium alloy surface composite coating that method is prepared in aerospace parts.
CN201810172242.7A 2018-03-01 2018-03-01 A kind of titanium alloy surface composite coating and its preparation method and application Pending CN108265292A (en)

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