CN112251706B - Preparation method of polycarbosilane/zirconia laser protection composite coating - Google Patents

Preparation method of polycarbosilane/zirconia laser protection composite coating Download PDF

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CN112251706B
CN112251706B CN202010991045.5A CN202010991045A CN112251706B CN 112251706 B CN112251706 B CN 112251706B CN 202010991045 A CN202010991045 A CN 202010991045A CN 112251706 B CN112251706 B CN 112251706B
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polycarbosilane
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zirconia
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王冬
赵玉真
梁永军
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Suzhou Na Chuangjia Environmental Protection Technology Engineering Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
    • C23C4/134—Plasma spraying
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/06—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation
    • B05D3/061—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation using U.V.
    • B05D3/062—Pretreatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/06—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation
    • B05D3/061—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation using U.V.
    • B05D3/065—After-treatment
    • B05D3/067—Curing or cross-linking the coating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/12—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by mechanical means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/50—Multilayers
    • B05D7/56—Three layers or more
    • B05D7/58—No clear coat specified
    • B05D7/582—No clear coat specified all layers being cured or baked together
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D2518/00—Other type of polymers
    • B05D2518/10—Silicon-containing polymers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
    • Y02T50/00—Aeronautics or air transport
    • Y02T50/60—Efficient propulsion technologies, e.g. for aircraft

Abstract

The invention belongs to the field of coating materials, and particularly relates to a preparation method of a polycarbosilane/zirconia laser protection composite coating. The method is characterized in that a bonding layer is sprayed on the surface of an aluminum substrate by using a plasma spraying method, then a zirconia coating doped with yttrium oxide, cerium oxide and ytterbium oxide is sprayed, and then polycarbosilane sol added with graphene powder is used for preparing the polycarbosilane coating on the zirconia coating by using a roll coating process, so that the composite coating with a good laser protection effect is obtained. In the laser protection process, after the polycarbosilane coating absorbs laser energy, the polycarbosilane coating is decomposed into silicon carbide SiC ceramic, the silicon carbide ceramic is high-temperature resistant and has good light reflectivity, and can generate strong scattering loss to laser beams, and graphene in the polycarbosilane coating has good heat conductivity, so that heat generated by laser is dissipated to the periphery, thermal stress is relieved to a certain extent, the heat resistance of a paint film is improved, and a better laser protection effect is achieved.

Description

Preparation method of polycarbosilane/zirconia laser protection composite coating
[ technical field ]: the invention belongs to the field of coating materials, and particularly relates to a preparation method of a polycarbosilane/zirconia laser protection composite coating.
[ background Art ] A method of: the laser weapon is a high-tech new-concept weapon which utilizes the huge energy carried by high-brightness strong laser beams to destroy or kill targets such as enemy airplanes, missiles, satellites and the like. The development of high-energy laser weapons has created a tremendous threat to aerial vehicles, and great importance has been attached to effective laser protection in military jurisdictions (Chen Guochao, Zhu Shizhen, Jiang ze. laser exposure protection of polymer matrix composites by additive coatings [ J ]. Journal of Materials science,2017,52(21): 12734-. The high-energy laser beam causes the irradiation target to generate a complex damage and destruction effect, and the damage mechanism is mainly embodied in thermal effect damage. When high-energy laser beams irradiate the material, the material is vaporized due to the large absorption of the irradiated material to the laser energy, and partial condensed particles or liquid drops are washed out together when the material steam is sprayed out at a high speed, so that the material is damaged by peeling, breakdown and the like. The shell materials of missiles, airplanes and satellites are generally metal materials with the melting point of about 1500 ℃, and strong laser with the power of 2-3 MW is easy to ablate, melt and vaporize as long as the strong laser irradiates a certain fixed part on the surface for 3-5 s, so that the internal fuel is combusted and exploded (Kaushal Hemani, Kaddoum Georges. applications of Lasers for practical Military Operations [ J ]. IEEE Access,2017,5: 0736-. Therefore, brushing and plating various functional coatings on the surface of the aircraft becomes the preferred method for laser protection.
Chinese patent 200810244070.6 discloses a protective coating resistant to laser ablation and a preparation method thereof, the method comprises the steps of firstly mixing polycarbosilane and divinylbenzene in proportion, heating and stirring to form a transparent mixed solution, then adding a proper amount of short carbon fiber and zirconia powder into the mixed solution, uniformly stirring to prepare a coating with a certain viscosity, coating the coating on the surface of a pretreated aluminum alloy substrate, putting the aluminum alloy substrate into an oven for heating and curing, and cooling to room temperature after curing to obtain a composite coating; the coating can weaken or eliminate the impact of laser on a substrate to a certain extent, so as to play a role in laser protection (patent number is 200810244070.6, the patent name is a protective coating resistant to laser ablation and a preparation method thereof, the inventor is Chenzhuangfeng, Sudun, Dojie, Wuwangping, Wanshuihong, Liuyong and Wangshiming, and the publication date is 2009, 6 months and 3 days). However, the thermal conductivity of the polymer material of the coating is generally low, the thermal conductivity and heat dissipation capacity are poor, and the local ablation condition is serious.
Based on the problems, the invention provides a preparation method of a polycarbosilane/zirconia laser protection composite coating, which comprises the steps of preparing a bonding layer and a zirconia layer on an aluminum-based material by using an ion spraying method, and preparing polycarbosilane at the outermost layer by using a roll coating process; the zirconium oxide is used for replacing high polymer materials, so that the high temperature resistance of the protective layer is effectively improved, and the effect of protecting high-intensity laser is better achieved; graphene in the polycarbosilane coating has good heat conducting capacity, so that heat generated by laser is dissipated to the periphery, thermal stress is relieved to a certain extent, and the heat resistance of a paint film is improved; has innovativeness, novelty and practicability.
[ summary of the invention ]: the invention provides a preparation method of a polycarbosilane/zirconia laser protection composite coating, and provides a composite coating consisting of a reflecting layer and a heat insulation layer double-layer structure, which comprehensively utilizes the high reflection and thermal barrier principles to realize better laser protection effect. Specifically, firstly, a bonding layer is sprayed on the surface of an aluminum substrate by using a plasma spraying method, then a zirconia coating doped with yttrium oxide, cerium oxide and ytterbium oxide is sprayed, then a polycarbosilane sol added with graphene powder is coated on the basis of the zirconia coating by using a roll coating process to prepare a polycarbosilane coating, and the polycarbosilane coating is dried to obtain the composite coating with good laser protection effect. The film has good laser resistance and can protect high-intensity laser.
[ technical solution of the present invention ]: the invention provides a preparation method of a polycarbosilane/zirconia laser protection composite coating, wherein the composite coating takes aluminum as a matrix, and a bonding layer, a zirconia coating and a polycarbosilane coating are sequentially arranged on the surface of the composite coating; the method is realized by the following steps:
first, giving a base material NiCrCoAlYHf a bonding layer
Firstly, grinding the surface of an aluminum alloy with the size of phi 25mm multiplied by 2mm and the model of 2A12 to be roughened by using sand paper; the 2A12 aluminum alloy is an aluminum alloy formed by smelting 0.00-0.50% of silicon, 0.30-0.90% of manganese, 0.00-0.30% of zinc, 1.2-1.8% of magnesium, 0.00-0.15% of titanium, 3.80-4.90% of copper, 0.00-0.50% of iron, 0.00-0.10% of nickel, 0.00-0.50% of iron and nickel and the balance of aluminum; cleaning the roughened aluminum alloy with acetone and deionized water for 3-5 times respectively, and drying in a vacuum blowing oven at 15-80 ℃ for 1-5 h to obtain the aluminum alloyA clean aluminum alloy base material; uniformly mixing 55.00-65.00 parts by weight of nickel, 16.00-22.00 parts by weight of chromium, 10.00-14.00 parts by weight of cobalt, 8.00-10.00 parts by weight of aluminum, 0.20-0.70 part by weight of yttrium and 0.05-0.30 part by weight of hafnium to obtain NiCrCoAlYHf powder with the particle size of 40-106 mu m, and applying the powder to the aluminum alloy base material in a plasma spraying manner; wherein the current in plasma spraying is 300-900A, the primary gas is high-purity Ar gas with the flow rate of 20-80L/min, and the secondary gas is H with the flow rate of 2-15L/min2The spraying distance is 50-200 mm, the powder transmission rate is 10-60 g/min, the thickness of the bonding layer is controlled to be 50-200 mu m, and the aluminum alloy material with the NiCrCoAlYHf bonding layer is prepared;
second, preparation of intermediate zirconia coating
Firstly, 65 to 75 parts by weight of zirconia ZrO having a particle size of 10 to 50 μm210 to 15 parts by weight of ytterbium oxide Yb having a particle diameter of 10 to 50 μm2O32 to 8 parts by weight of yttrium oxide Y having a particle size of 10 to 50 μm2O3And 8 to 12 parts by weight of cerium oxide CeO having a particle diameter of 10 to 50 μm2Uniformly mixing, and spraying the mixed powder onto the NiCrCoAlYHf bonding layer of the aluminum alloy material in the step one by adopting a plasma spraying mode, wherein the current in plasma spraying is 300-900A, the main gas is high-purity Ar gas with the flow rate of 20-80L/min, and the secondary gas is high-purity H with the flow rate of 2-15L/min2The gas spraying distance is 50-200 mm, the powder transmission rate is 10-60 g/min, and the thickness of the zirconia coating is controlled to be 80-300 mu m, so that the aluminum alloy material with the zirconia coating and the NiCrCoAlYHf bonding layer is prepared;
thirdly, preparing a top layer polycarbosilane coating
Firstly, mixing 35-45 parts by weight of polycarbosilane PCS, 25-35 parts by weight of divinylbenzene DVB and 5-10 parts by weight of dicumyl peroxide DCP at room temperature, magnetically stirring for 10-30 min at the rotating speed of 400-800 r/min, and then transferring the mixed solution into a water bath kettle at the temperature of 30-90 ℃ to continue to magnetically stir for 30-120 min at the rotating speed of 400-800 r/min; then adding 8-16 parts of thin layer with thickness of 0.5-2.0 n into the mixed solutionm, specific surface area 2630m2Taking graphene powder per gram and 1-2 parts of polyethylene glycol PEG with the molecular weight of 200-8000 as dispersing agents, and continuously stirring for 10-60 min to obtain polycarbosilane coating; and finally, performing roller coating on the zirconium oxide coating obtained in the second step by using a roller coating process to obtain polycarbosilane with the thickness of 50-300 microns, putting the polycarbosilane into a constant-temperature blast oven at 140-160 ℃ for heat treatment for 1-3 h, and cooling to room temperature to obtain the target polycarbosilane/zirconium oxide laser protection composite coating.
[ advantages and effects of the invention ]: the invention provides a preparation method of a polycarbosilane/zirconia laser protection composite coating, which has the following remarkable advantages: (1) hf element is added in the existing bonding layer material, so that the zirconia coating and the matrix can be well bonded together, and the important effect on improving the oxidation resistance of the coating is achieved; (2) the yttrium oxide, the cerium oxide and the ytterbium oxide are added into the zirconia coating, so that the stability of the zirconia coating can be improved, and the problem of coating falling off at high temperature is avoided, thereby effectively playing the role of a thermal barrier coating, preventing the temperature of a base material from rising, and avoiding the failure of the base material due to overhigh temperature; (3) after the polycarbosilane coating absorbs laser energy, the polycarbosilane coating is decomposed into silicon carbide ceramic, the silicon carbide ceramic is high-temperature resistant and has good light reflectivity, and strong scattering loss can be generated for laser beams, so that the striking of the laser to a matrix is weakened or eliminated, and the matrix material is effectively protected; (4) after the graphene is added into the polycarbosilane coating, the graphene has good thermal conductivity, so that heat generated by laser is dissipated to the periphery, thermal stress is relieved to a certain extent, the heat resistance of a paint film is improved, and meanwhile, the heat is uniformly transferred to the zirconia coating; (5) the polycarbosilane coating and the zirconia coating are combined, the high reflection and thermal barrier principles are comprehensively utilized, the better laser protection effect is realized, and the preparation process of the composite coating is simple and easy to implement.
Drawings
Fig. 1 is a schematic structural diagram of a laser protection composite coating of a target polycarbosilane/zirconia in the patent of the invention, wherein the numbers in the diagram are respectively as follows: 1 is an aluminum substrate, 2 is a bonding layer, 3 is a zirconia coating, and 4 is a polycarbosilane coating.
Detailed Description
In order to more clearly illustrate the advantages of the present patent, the following embodiments and effects of the present invention are further illustrated with reference to the following examples; it is to be understood that not all embodiments described herein are provided. All other embodiments that can be derived by one of ordinary skill in the art from the embodiments disclosed herein are intended to be within the scope of the present invention.
Example 1 preparation of a polycarbosilane/zirconia laser protective composite coating sample 1
The invention provides a preparation method of a polycarbosilane/zirconia laser protection composite coating, wherein the composite coating takes aluminum as a matrix, and a bonding layer, a zirconia coating and a polycarbosilane coating are sequentially arranged on the surface of the composite coating; as shown in fig. 1, the method specifically comprises the following steps:
first, giving a base material NiCrCoAlYHf a bonding layer
Firstly, grinding the surface of an aluminum alloy with the size of phi 25mm multiplied by 2mm and the model of 2A12 to be roughened by abrasive paper, then respectively washing for 3 times by acetone and deionized water, and placing the aluminum alloy in a vacuum air-blowing oven at the temperature of 30 ℃ for drying for 1h to obtain a clean aluminum alloy matrix material; then, 60.00 parts by weight of nickel, 20.00 parts by weight of chromium, 11.40 parts by weight of cobalt, 8.00 parts by weight of aluminum, 0.50 parts by weight of yttrium and 0.10 parts by weight of hafnium were uniformly mixed to obtain NiCrCoAlYHf powder, and the powder was applied to the above aluminum alloy base material by plasma spraying using a current of 600A, a main gas of high purity Ar gas at a flow rate of 50L/min and a sub gas of H at a flow rate of 6L/min2Gas spraying, spraying distance of 100mm, powder transmission rate of 30g/min and bonding layer thickness control of 100 mu m, so as to prepare the aluminum alloy material with the NiCrCoAlYHf bonding layer;
second, preparation of intermediate zirconia coating
First, 70 parts by weight of zirconia ZrO having a particle size of 50 μm212 parts by weight of ytterbium oxide Yb having a particle diameter of 50 μm2O38 parts by weight of yttrium oxide Y having a particle size of 50 μm2O3And 10 parts by weight of cerium oxide CeO having a particle size of 50 μm2The components are evenly mixed and then are mixed,and then spraying the mixed powder onto the NiCrCoAlYHf bonding layer of the aluminum alloy material in the step one by adopting a plasma spraying mode, wherein the current in the plasma spraying is 600A, the main gas is high-purity Ar gas with the flow rate of 60L/min, and the secondary gas is high-purity H with the flow rate of 6L/min2Gas spraying, spraying distance of 100mm, powder transmission rate of 30g/min and thickness control of zirconia coating of 200 mu m to prepare the aluminum alloy material with the zirconia coating and the NiCrCoAlYHf bonding layer;
thirdly, preparing a top layer polycarbosilane coating
Firstly, 43 parts by weight of polycarbosilane PCS, 32 parts by weight of divinylbenzene DVB and 16 parts by weight of dicumyl peroxide DCP are mixed at room temperature, magnetic stirring is carried out for 15min at the rotating speed of 600r/min, and then the mixed solution is moved into a water bath kettle at the temperature of 50 ℃ to continue magnetic stirring at the rotating speed of 600r/min for 60 min; then, 8 parts by weight of a thin layer having a thickness of 1.0nm and a specific surface area of 2630m was further added to the mixed solution2Taking graphene powder per gram and 1 part by weight of polyethylene glycol PEG with the molecular weight of 4000 as dispersing agents, and continuously stirring for 60min to obtain polycarbosilane coating; and finally, performing roll coating on the polycarbosilane with the thickness of 100 mu m on the basis of the zirconia coating obtained in the second step by using a roll coating process, putting the polycarbosilane into a constant-temperature blast oven at 150 ℃ for heat treatment for 3h, and cooling to room temperature to finally obtain the target polycarbosilane/zirconia laser protection composite coating sample 1.
The laser protection composite coating sample 1 of the target polycarbosilane/zirconia is irradiated by 1500W laser for 5s, the coating is ablated, but the coating does not fall off, the aluminum matrix is intact, and the temperature of the back rises slowly; after the laser irradiation of 2000W for 5s, the ablation black spots of the coating are enlarged, the center ablation is serious, but the coating still does not fall off, the aluminum matrix is intact, and the temperature of the back part rises slowly; the laser protection composite coating sample 1 of the target polycarbosilane/zirconia has good high temperature resistance and can protect high-intensity laser.
Example 2 preparation of a polycarbosilane/zirconia laser protective composite coating sample 2
The invention provides a preparation method of a polycarbosilane/zirconia laser protection composite coating, wherein the composite coating takes aluminum as a matrix, and a bonding layer, a zirconia coating and a polycarbosilane coating are sequentially arranged on the surface of the composite coating; the method is realized by the following steps:
first, giving a base material NiCrCoAlYHf a bonding layer
Firstly, grinding the surface of an aluminum alloy with the size of phi 25mm multiplied by 2mm and the model of 2A12 to be roughened by abrasive paper, then respectively washing for 3 times by acetone and deionized water, and placing the aluminum alloy in a vacuum air-blowing oven at the temperature of 30 ℃ for drying for 1h to obtain a clean aluminum alloy matrix material; then, 60.00 parts by weight of nickel, 20.00 parts by weight of chromium, 11.40 parts by weight of cobalt, 8.00 parts by weight of aluminum, 0.50 parts by weight of yttrium and 0.10 parts by weight of hafnium were uniformly mixed to obtain NiCrCoAlYHf powder, and the powder was applied to the above aluminum alloy base material by plasma spraying using a high purity Ar gas having a flow rate of 50L/min as a main gas and H having a flow rate of 5L/min as a sub gas2Gas spraying, spraying distance of 100mm, powder transmission rate of 30g/min and bonding layer thickness control of 100 mu m, so as to prepare the aluminum alloy material with the NiCrCoAlYHf bonding layer;
second, preparation of intermediate zirconia coating
First, 70 parts by weight of zirconia ZrO having a particle size of 50 μm212 parts by weight of ytterbium oxide Yb having a particle diameter of 50 μm2O38 parts by weight of yttrium oxide Y having a particle size of 50 μm2O3And 10 parts by weight of cerium oxide CeO having a particle size of 50 μm2Uniformly mixing, and then spraying the mixed powder onto the NiCrCoAlYHf bonding layer of the aluminum alloy material in the step one by adopting a plasma spraying mode, wherein the current in the plasma spraying is 600A, the main gas is high-purity Ar gas with the flow rate of 60L/min, and the secondary gas is high-purity H with the flow rate of 6L/min2Gas spraying, spraying distance of 100mm, powder transmission rate of 30g/min and thickness control of zirconia coating of 200 mu m to prepare the aluminum alloy material with the zirconia coating and the NiCrCoAlYHf bonding layer;
thirdly, preparing a top layer polycarbosilane coating
First, 45 parts by weight of polycarbosilane PCS, 35 parts by weight of divinylbenzene DVB and 10 parts by weight of dicumyl peroxide were mixed at room temperatureMixing DCP, magnetically stirring at 600r/min for 15min, transferring the mixture into 50 deg.C water bath, and magnetically stirring at 600r/min for 60 min; then, 9 parts by weight of a thin layer having a thickness of 1.0nm and a specific surface area of 2630m was added to the mixed solution2Taking graphene powder per gram and 1 part by weight of polyethylene glycol PEG with the molecular weight of 4000 as dispersing agents, and continuously stirring for 60min to obtain polycarbosilane coating; and finally, performing roll coating on the polycarbosilane with the thickness of 200 mu m on the basis of the zirconia coating obtained in the second step by using a roll coating process, putting the polycarbosilane into a constant-temperature blast oven at 150 ℃ for heat treatment for 3h, and cooling to room temperature to finally obtain a target polycarbosilane/zirconia laser protection composite coating sample 2.
The laser protection composite coating sample 2 of the target polycarbosilane/zirconia is irradiated by 1000W laser for 5s, the surface of the coating is coked, the aluminum matrix is intact, and the rise amplitude of the back temperature is very small; after the coating is irradiated by 2000W laser for 5s, the coating generates ablation black spots, but the coating is not obvious in the embodiment 1, the aluminum matrix is intact, and the back temperature is not high in the embodiment 1; the laser protection composite coating sample 2 of the target polycarbosilane/zirconia has good high temperature resistance and can protect high-intensity laser.
Example 3 preparation of a polycarbosilane/zirconia laser protective composite coating sample 3
The invention provides a preparation method of a polycarbosilane/zirconia laser protection composite coating, wherein the composite coating takes aluminum as a matrix, and a bonding layer, a zirconia coating and a polycarbosilane coating are sequentially arranged on the surface of the composite coating; the method is realized by the following steps:
first, giving a base material NiCrCoAlYHf a bonding layer
Firstly, grinding the surface of an aluminum alloy with the size of phi 25mm multiplied by 2mm and the model of 2A12 to be roughened by abrasive paper, then respectively washing for 3 times by acetone and deionized water, and placing the aluminum alloy in a vacuum air-blowing oven at the temperature of 30 ℃ for drying for 1h to obtain a clean aluminum alloy matrix material; then 60.00 weight parts of nickel, 20.00 weight parts of chromium, 11.40 weight parts of cobalt, 8.00 weight parts of aluminum, 0.50 weight parts of yttrium and 0.10 weight parts of hafnium are uniformly mixed to obtain NiCrCoAlYHf powder, and the powder is added to the NiCrCoAlYHf powder by adopting a plasma spraying modeThe aluminum alloy base material was coated with plasma at a current of 600A, a main gas of high purity Ar gas at a flow rate of 50L/min, and a sub gas of H gas at a flow rate of 6L/min2Gas spraying, spraying distance of 100mm, powder transmission rate of 30g/min and bonding layer thickness control of 100 mu m, so as to prepare the aluminum alloy material with the NiCrCoAlYHf bonding layer;
second, preparation of intermediate zirconia coating
First, 70 parts by weight of zirconia ZrO having a particle size of 50 μm212 parts by weight of ytterbium oxide Yb having a particle diameter of 50 μm2O38 parts by weight of yttrium oxide Y having a particle size of 50 μm2O3And 10 parts by weight of cerium oxide CeO having a particle size of 50 μm2Uniformly mixing, and then spraying the mixed powder onto the NiCrCoAlYHf bonding layer of the aluminum alloy material in the step one by adopting a plasma spraying mode, wherein the current in the plasma spraying is 600A, the main gas is high-purity Ar gas with the flow rate of 60L/min, and the secondary gas is high-purity H with the flow rate of 6L/min2Gas spraying, spraying distance of 100mm, powder transmission rate of 30g/min and thickness control of zirconia coating of 200 mu m to prepare the aluminum alloy material with the zirconia coating and the NiCrCoAlYHf bonding layer;
thirdly, preparing a top layer polycarbosilane coating
Firstly, 42 parts by weight of polycarbosilane PCS, 32 parts by weight of divinylbenzene DVB and 10 parts by weight of dicumyl peroxide DCP are mixed at room temperature, magnetic stirring is carried out for 15min at the rotating speed of 600r/min, and then the mixed solution is moved into a water bath kettle at the temperature of 50 ℃ to continue magnetic stirring at the rotating speed of 600r/min for 60 min; then, 15 parts by weight of a thin layer having a thickness of 1.0nm and a specific surface area of 2630m was further added to the mixed solution2Taking graphene powder per gram and 1 part by weight of polyethylene glycol PEG with the molecular weight of 4000 as dispersing agents, and continuously stirring for 60min to obtain polycarbosilane coating; and finally, performing roll coating on the polycarbosilane with the thickness of 300 mu m on the basis of the zirconia coating obtained in the second step by using a roll coating process, putting the polycarbosilane into a constant-temperature blast oven at 150 ℃ for heat treatment for 3h, and cooling to room temperature to finally obtain a target polycarbosilane/zirconia laser protection composite coating sample 3.
The laser protection composite coating sample 3 of the target polycarbosilane/zirconia is irradiated by 1000W laser for 5s, the surface of the coating is coked, the aluminum matrix is intact, and the rise amplitude of the back temperature is very small; after the coating is irradiated by 2000W laser for 5s, the coating generates ablation black spots, but the coating is not obvious in the embodiment 2, the aluminum matrix is intact, and the back temperature is not high in the embodiment 2; the laser protection composite coating sample 3 of the target polycarbosilane/zirconia has good high temperature resistance and can protect high-intensity laser.
Example 4 preparation of a polycarbosilane/zirconia laser protective composite coating sample 4
The invention provides a preparation method of a polycarbosilane/zirconia laser protection composite coating, wherein the composite coating takes aluminum as a matrix, and a bonding layer, a zirconia coating and a polycarbosilane coating are sequentially arranged on the surface of the composite coating; the method is realized by the following steps:
first, giving a base material NiCrCoAlYHf a bonding layer
Firstly, grinding the surface of an aluminum alloy with the size of phi 25mm multiplied by 2mm and the model of 2A12 to be roughened by abrasive paper, then respectively washing for 3 times by acetone and deionized water, and placing the aluminum alloy in a vacuum air-blowing oven at the temperature of 30 ℃ for drying for 1h to obtain a clean aluminum alloy matrix material; then, 60.00 parts by weight of nickel, 20.00 parts by weight of chromium, 11.40 parts by weight of cobalt, 8.00 parts by weight of aluminum, 0.50 parts by weight of yttrium and 0.10 parts by weight of hafnium were uniformly mixed to obtain NiCrCoAlYHf powder, and the powder was applied to the above aluminum alloy base material by plasma spraying using a current of 600A, a main gas of high purity Ar gas at a flow rate of 50L/min and a sub gas of H at a flow rate of 6L/min2Gas spraying, spraying distance of 100mm, powder transmission rate of 30g/min and bonding layer thickness control of 100 mu m, so as to prepare the aluminum alloy material with the NiCrCoAlYHf bonding layer;
second, preparation of intermediate zirconia coating
First, 70 parts by weight of zirconia ZrO having a particle size of 50 μm212 parts by weight of ytterbium oxide Yb having a particle diameter of 50 μm2O38 parts by weight of yttrium oxide Y having a particle size of 50 μm2O3And 10 parts by weight of cerium oxide CeO having a particle size of 50 μm2Uniformly mixing, and thenSpraying the mixed powder onto the NiCrCoAlYHf bonding layer of the aluminum alloy material in the step one by adopting a plasma spraying mode, wherein the current in the plasma spraying is 600A, the main gas is high-purity Ar gas with the flow rate of 60L/min, and the secondary gas is high-purity H with the flow rate of 6L/min2Gas spraying, spraying distance of 100mm, powder transmission rate of 30g/min and thickness control of zirconia coating of 200 mu m to prepare the aluminum alloy material with the zirconia coating and the NiCrCoAlYHf bonding layer;
thirdly, preparing a top layer polycarbosilane coating
Firstly, mixing 45 parts by weight of polycarbosilane PCS, 35 parts by weight of divinylbenzene DVB and 10 parts by weight of dicumyl peroxide DCP at room temperature, magnetically stirring for 15min at the rotating speed of 600r/min, and then moving the mixed solution into a water bath kettle at the temperature of 50 ℃ to continue to magnetically stir for 60min at the rotating speed of 600 r/min; then, 9 parts by weight of a thin layer having a thickness of 1.0nm and a specific surface area of 2630m was added to the mixed solution2Taking graphene powder per gram and 1 part by weight of polyethylene glycol PEG with the molecular weight of 4000 as dispersing agents, and continuously stirring for 60min to obtain polycarbosilane coating; and finally, performing roll coating on the polycarbosilane with the thickness of 200 mu m on the basis of the zirconia coating obtained in the second step by using a roll coating process, putting the polycarbosilane into a constant-temperature blast oven at 150 ℃ for heat treatment for 3h, and cooling to room temperature to finally obtain a target polycarbosilane/zirconia laser protection composite coating sample 4.
The laser protection composite coating sample 4 of the target polycarbosilane/zirconia is irradiated by 1000W laser for 5s, the surface of the coating is coked, the aluminum matrix is intact, the rise amplitude of the back temperature is small, the coking range of the coating is larger than that of the coating in the embodiment 2, but the color change is small; after 2000W laser irradiation for 5s, the coking range of the coating surface is further expanded, the deep color in the central area is gradually changed into light yellow from the periphery, the aluminum matrix is intact, and the back temperature is not high in the embodiment 2; the laser protection composite coating sample 4 of the target polycarbosilane/zirconia has good high temperature resistance and can protect high-intensity laser.
Example 5 preparation of a polycarbosilane/zirconia laser protective composite coating sample 5
The invention provides a preparation method of a polycarbosilane/zirconia laser protection composite coating, wherein the composite coating takes aluminum as a matrix, and a bonding layer, a zirconia coating and a polycarbosilane coating are sequentially arranged on the surface of the composite coating; the method is realized by the following steps:
first, giving a base material NiCrCoAlYHf a bonding layer
Firstly, grinding the surface of an aluminum alloy with the size of phi 25mm multiplied by 2mm and the model of 2A12 to be roughened by abrasive paper, then respectively washing the surface by acetone and deionized water for 3 times, and placing the surface in a vacuum blast oven at 30 ℃ for drying for 1h to obtain a clean aluminum alloy matrix material; then, 60.00 parts by weight of nickel, 20.00 parts by weight of chromium, 11.40 parts by weight of cobalt, 8.00 parts by weight of aluminum, 0.50 parts by weight of yttrium and 0.10 parts by weight of hafnium were uniformly mixed to obtain NiCrCoAlYHf powder, and the powder was applied to the above aluminum alloy base material by plasma spraying using a current of 600A, a main gas of high purity Ar gas at a flow rate of 50L/min and a sub gas of H at a flow rate of 6L/min2Gas spraying, spraying distance of 100mm, powder transmission rate of 30g/min and bonding layer thickness control of 100 mu m, so as to prepare the aluminum alloy material with the NiCrCoAlYHf bonding layer;
second, preparation of intermediate zirconia coating
First, 70 parts by weight of zirconia ZrO having a particle size of 50 μm212 parts by weight of ytterbium oxide Yb having a particle diameter of 50 μm2O38 parts by weight of yttrium oxide Y having a particle size of 50 μm2O3And 10 parts by weight of cerium oxide CeO having a particle size of 50 μm2Uniformly mixing, and then spraying the mixed powder onto the NiCrCoAlYHf bonding layer of the aluminum alloy material in the step one by adopting a plasma spraying mode, wherein the current in the plasma spraying is 600A, the main gas is high-purity Ar gas with the flow rate of 60L/min, and the secondary gas is high-purity H with the flow rate of 6L/min2Gas spraying, spraying distance of 100mm, powder transmission rate of 30g/min and thickness control of zirconia coating of 200 mu m to prepare the aluminum alloy material with the zirconia coating and the NiCrCoAlYHf bonding layer;
thirdly, preparing a top layer polycarbosilane coating
First, 45 parts by weight of polycarbosilane PCS and 30 parts by weight of polycarbosilane are mixed at room temperatureMixing divinylbenzene DVB in certain weight portion and dicumyl peroxide DCP in 10 weight portion, magnetically stirring at 600r/min for 15min, and magnetically stirring in a water bath at 50 deg.c for 60 min; then, 14 parts by weight of a thin layer having a thickness of 1.0nm and a specific surface area of 2630m was added to the mixture2Taking graphene powder per gram and 1 part by weight of polyethylene glycol PEG with the molecular weight of 4000 as dispersing agents, and continuously stirring for 60min to obtain polycarbosilane coating; and finally, performing roll coating on the polycarbosilane with the thickness of 200 mu m on the basis of the zirconia coating obtained in the second step by using a roll coating process, putting the polycarbosilane into a constant-temperature blast oven at 150 ℃ for heat treatment for 3h, and cooling to room temperature to finally obtain a target polycarbosilane/zirconia laser protection composite coating sample 5.
The laser protection composite coating sample 5 of the target polycarbosilane/zirconia is irradiated by 1000W laser for 5s, the surface of the coating is coked, the aluminum matrix is intact, the rise amplitude of the back temperature is small, the coking range of the coating is larger than that of the coating in the embodiment 2, the color change is small, and a few micro cracks appear on the coating; after the laser irradiation of 2000W for 5s, the coking range of the coating surface is further expanded, the deep color in the central area is gradually changed into light yellow from the periphery, the aluminum matrix is intact, the back temperature is not higher than that of the embodiment 2, but the microcracks are increased compared with that of the embodiment 4; the laser protection composite coating sample 5 of the target polycarbosilane/zirconia has good high temperature resistance and can protect high-intensity laser.

Claims (1)

1. A method for preparing a polycarbosilane/zirconia laser protection composite coating, wherein the composite coating takes aluminum as a substrate, and a bonding layer, a zirconia coating and a polycarbosilane coating are sequentially arranged on the surface of the composite coating; the method is realized by the following steps:
first, giving a base material NiCrCoAlYHf a bonding layer
Firstly, grinding the surface of an aluminum alloy with the size of phi 25mm multiplied by 2mm and the model of 2A12 to be roughened by using sand paper; wherein the 2A12 aluminum alloy is composed of 0.00-0.50% of silicon, 0.30-0.90% of manganese, 0.00-0.30% of zinc, 1.2-1.8% of magnesium, 0.00-0.15% of titanium, 3.80-4.90% of copper, 0.00-0.50% of iron, 0.00-0.10% of nickel,0.00-0.50% of iron and nickel and the balance of aluminum; cleaning the roughened aluminum alloy with acetone and deionized water for 3-5 times respectively, and drying in a vacuum blowing oven at 15-80 ℃ for 1-5 h to obtain a clean aluminum alloy matrix material; then, 55.00 to 65.00 weight parts of nickel, 16.00 to 22.00 weight parts of chromium, 10.00 to 14.00 weight parts of cobalt, 8.00 to 10.00 weight parts of aluminum, 0.20 to 0.70 weight part of yttrium and 0.05 to 0.30 weight part of hafnium are uniformly mixed to obtain NiCrCoAlYHf powder with the particle size of 40 to 106 mu m, and the powder is applied to the aluminum alloy base material by adopting a plasma spraying mode, wherein the current in plasma spraying is 300 to 900A, the main gas is high-purity Ar gas with the flow rate of 20 to 80L/min, and the secondary gas is H with the flow rate of 2 to 15L/min2The spraying distance is 50-200 mm, the powder transmission rate is 10-60 g/min, the thickness of the bonding layer is controlled to be 50-200 mu m, and the aluminum alloy material with the NiCrCoAlYHf bonding layer is prepared;
second, preparation of intermediate zirconia coating
Firstly, 65 to 75 parts by weight of zirconia ZrO having a particle size of 10 to 50 μm210 to 15 parts by weight of ytterbium oxide Yb having a particle diameter of 10 to 50 μm2O32 to 8 parts by weight of yttrium oxide Y having a particle size of 10 to 50 μm2O3And 8 to 12 parts by weight of cerium oxide CeO having a particle diameter of 10 to 50 μm2Uniformly mixing, and spraying the mixed powder onto the NiCrCoAlYHf bonding layer of the aluminum alloy material in the step one by adopting a plasma spraying mode, wherein the current in plasma spraying is 300-900A, the main gas is high-purity Ar gas with the flow rate of 20-80L/min, and the secondary gas is high-purity H with the flow rate of 2-15L/min2The gas spraying distance is 50-200 mm, the powder transmission rate is 10-60 g/min, and the thickness of the zirconia coating is controlled to be 80-300 mu m, so that the aluminum alloy material with the zirconia coating and the NiCrCoAlYHf bonding layer is prepared;
thirdly, preparing a top layer polycarbosilane coating
Firstly, 35-45 parts by weight of polycarbosilane PCS, 25-35 parts by weight of divinylbenzene DVB and 5-10 parts by weight of dicumyl peroxide DCP are mixed at room temperature, and magnetic stirring is carried out at the rotating speed of 400-800 r/minStirring for 10-30 min, then transferring the mixed solution into a water bath kettle at 30-90 ℃ and continuing to magnetically stir for 30-120 min at the rotating speed of 400-800 r/min; then 8-16 parts by weight of thin layer with the thickness of 0.5-2.0 nm and the specific surface area of 2630m is added into the mixed solution2Taking graphene powder per gram and 1-2 parts by weight of polyethylene glycol PEG with the molecular weight of 200-8000 as dispersing agents, and continuously stirring for 10-60 min to obtain polycarbosilane coating; and finally, performing roller coating on the zirconium oxide coating obtained in the second step by using a roller coating process to obtain polycarbosilane with the thickness of 50-300 microns, putting the polycarbosilane into a constant-temperature blast oven at 140-160 ℃ for heat treatment for 1-3 h, and cooling to room temperature to obtain the target polycarbosilane/zirconium oxide laser protection composite coating.
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