CN114085098B - Corrosion-resistant, sintering-resistant and high-temperature creep-resistant alumina composite ceramic and preparation method thereof - Google Patents

Corrosion-resistant, sintering-resistant and high-temperature creep-resistant alumina composite ceramic and preparation method thereof Download PDF

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CN114085098B
CN114085098B CN202111420993.4A CN202111420993A CN114085098B CN 114085098 B CN114085098 B CN 114085098B CN 202111420993 A CN202111420993 A CN 202111420993A CN 114085098 B CN114085098 B CN 114085098B
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CN114085098A (en
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刘杰
张义平
江济
胡刚毅
毛福春
陈琳
冯晶
王建坤
张陆洋
苏涛
利建雨
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YUNNAN POLICE OFFICER ACADEMY
Kunming University of Science and Technology
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    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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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    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
    • C23C4/134—Plasma spraying

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Abstract

The invention relates to the technical field of public safety and fire fighting equipment, and discloses an aluminum oxide composite ceramic with corrosion resistance, sintering resistance and high-temperature creep resistance and a preparation method thereof. The preparation method comprises the following steps: preparing an adhesive layer on the surface of the alumina composite ceramic in an atmospheric plasma spraying manner; step II: preparing (RE) on the surface of the bonding layer by means of atmospheric plasma spraying 3 TaO 7 ) 1‑x (RETaO 4 ) x A porous structure heat insulation and cooling layer consisting of two-phase ceramics; step III: preparing compact AlTaO on the surface of the heat insulation and cooling layer by means of atmospheric plasma spraying 4 And (4) an anti-corrosion layer. The invention solves the problems of growth of crystal grains, performance degradation, insufficient sintering resistance and corrosion resistance of the alumina ceramic matrix composite material at high temperature in the prior art.

Description

Corrosion-resistant, sintering-resistant and high-temperature creep-resistant aluminum oxide composite ceramic and preparation method thereof
Technical Field
The invention relates to the technical field of public safety and fire-fighting equipment, in particular to an aluminum oxide composite ceramic with corrosion resistance, sintering resistance and high-temperature creep resistance and a preparation method thereof.
Background
With the increasing maturity of unmanned aerial vehicle technology and the further expansion of aerial photography technology, domestic unmanned aerial vehicle application field is increasingly extensive, include: photogrammetry, emergency disaster relief, public safety, resource exploration, environment monitoring, natural disaster monitoring and assessment, forest fire protection monitoring and the like. At present, the fire department in China faces increasingly complex fire fighting and rescue and social rescue modes, the limitation of the traditional on-site detection means is increasingly prominent on the conditions of various earthquake rescues, high-rise fires and the like, and the unmanned aerial vehicle has the characteristics of flexible operation, comprehensive visual field, simplicity in operation, high safety and the like, and the function of the unmanned aerial vehicle in the field of fire fighting is also increasingly prominent.
At present, the unmanned aerial vehicle surface material is resin matrix combined material and carbon fiber braid etc. mostly, though has better intensity, but its high temperature resistant, corrosion-resistant and anti sintering performance is not enough, is applied to the fire control field and then has certain limitation. The fiber reinforced alumina ceramic matrix composite material such as alumina, zirconia or silica fiber and the like is widely applied to the aerospace field due to the characteristics of high melting point, oxidation resistance, small specific gravity, high strength and the like, and can reach the working temperature of more than 1300 ℃ as a structural member of a high-temperature area or a heat-insulating protective coating material. However, the alumina ceramic matrix composite material has the problems of performance degradation caused by grain growth and insufficient high-temperature creep resistance in the use process of the alumina ceramic matrix composite material as a high-temperature structural material, and meanwhile, water vapor in the air can react with alumina to cause matrix failure; however, because of volcanic eruption, sand storm and the like, the air contains a large amount of low-melting-point oxides such as magnesium oxide, aluminum oxide, calcium oxide, iron oxide and the like, and the oxides react with aluminum oxide ceramics after being melted at high temperature to cause material failure, thereby limiting the application of the material.
Disclosure of Invention
The invention aims to provide an alumina composite ceramic with corrosion resistance, sintering resistance and high-temperature creep resistance and a preparation method thereof, and aims to solve the problems of growth of crystal grains, performance degradation, insufficient sintering resistance and corrosion resistance of an alumina ceramic matrix composite material at high temperature in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme: the aluminum oxide composite ceramic is composed of an aluminum oxide composite ceramic substrate, a bonding layer, a heat insulation and cooling layer and an anti-corrosion layer.
In another aspect of the present disclosure, a method for preparing an aluminum oxide composite ceramic with corrosion resistance, sintering resistance and high temperature creep resistance is provided, which includes the following steps:
step I: preparing an adhesive layer on the surface of the alumina composite ceramic in an atmosphere plasma spraying manner;
step II: preparing (RE) on the surface of the bonding layer by means of atmospheric plasma spraying 3 TaO 7 ) 1-x (RETaO 4 ) x A porous structure heat insulation and cooling layer consisting of two-phase ceramics;
step III: preparing compact AlTaO on the surface of the heat insulation and cooling layer by means of atmospheric plasma spraying 4 And (4) an anti-corrosion layer.
The principle and the advantages of the scheme are as follows: in the technical scheme, the used matrix material is an alumina ceramic matrix composite, and the prepared coating provides the matrix material with the properties of sintering resistance, corrosion resistance, high-temperature creep resistance and the like. The heat insulation and temperature reduction layer with the porous structure is prepared on the surface of the alumina-based composite ceramic matrix, so that the heat insulation and temperature reduction effects can be achieved, the surface problems of performance degradation and the like of alumina caused by grain growth at high temperature are reduced, and the sintering resistance and the high-temperature creep resistance of the alumina are improved. Meanwhile, a compact anti-corrosion layer is prepared on the surface of the heat insulation and cooling layer, so that the low-melting-point oxide corrosion resistance and the steam corrosion resistance of the material are improved. In addition, in the present scheme, use is made of(RE 3 TaO 7 )/(RETaO 4 ) The two-phase ceramic is used as a heat insulation and cooling layer, both the two layers have extremely low heat conductivity, and meanwhile, the coating is of a porous structure, so that the heat conductivity is further reduced, and therefore, an excellent heat insulation and cooling effect can be provided, and the characteristics of the two-phase composition can inhibit the growth of crystal grains, improve the anti-sintering performance of the material and ensure that the porosity in the coating is basically unchanged; and the existence of interfacial thermal resistance between two phases of ceramics can further reduce the heat transfer performance of the material. Aluminum tantalate (AlTaO) 4 ) As an anti-corrosion layer, the surface of the material is compact, the contact angle with water is more than 90 degrees, and the material has the characteristic of hydrophobicity, and can have super-hydrophobicity by regulating and controlling the phase morphology, so that the water vapor corrosion resistance of the material is improved; meanwhile, the aluminum tantalate and the low-melting-point oxide have good chemical compatibility and are not easy to react with each other, and the low-melting-point oxide solution directly slides off the surface of the coating due to the existence of the compact coating, so that the low-melting-point oxide solution is prevented from entering the coating and reacting with the alumina and the composite ceramic. In addition, the rare earth tantalate coating and the aluminum tantalate coating have good chemical compatibility, the rare earth tantalate coating and the aluminum tantalate coating do not react when being used and contacted for a long time at high temperature, and excellent heat insulation protection and corrosion resistance can be always kept in the using process. Through research, the heat-insulating anti-corrosion coating in the prior art adopts rare earth zirconate to be compounded with calcium oxide, magnesium oxide, aluminum oxide and silicon oxide for use, but because the melting point of the oxide is low, the oxide can react with the rare earth zirconate violently in the use process under a high-temperature condition, the corrosion resistance effect cannot be provided, and the heat-insulating protection effect cannot be provided after the coating fails.
Preferably, as a modification, the alumina composite ceramic matrix is a fiber-reinforced alumina ceramic of one or more of alumina, zirconia or silica fibers.
In the technical scheme, the alumina composite ceramic matrix is made of the materials, so that the strength and performance requirements of the matrix can be met, and the materials are commercially available finished products, so that the material source is wide, and the application technology is mature.
Preferably, as an improvement, the bonding layer is NiCoCrAlY modified by noble metal, and the noble metal is one or more of platinum, palladium, rhodium, ruthenium, iridium and osmium.
In the technical scheme, niCoCrAlY is used as the bonding layer, the NiCoCrAlY has the characteristics of high melting point and strong oxidation resistance, and meanwhile, a certain amount of noble metal (platinum, palladium, rhodium, ruthenium, iridium and osmium) with strong oxidation resistance is added, so that the oxidation resistance of the bonding layer material can be further improved in a synergistic manner, the generation of thermally generated oxides on the surface of the bonding layer is inhibited, and the thermal stress between layers in a coating system is reduced.
Preferably, as a modification, the noble metal is added to NiCoCrAlY in an amount of 1-10% by mass of the NiCoCrAlY.
In the technical scheme, when NiCoCrAlY is modified, too high addition of the noble metal can cause too high material cost and reduction of mechanical properties such as hardness, fracture toughness and tensile strength, and too low addition of the noble metal can not provide enough oxidation resistance.
Preferably, as a modification, the thickness of the adhesive layer is 100 to 200um.
In the technical scheme, the thickness of the bonding layer is a relatively good thickness range verified by tests, the material cost and the preparation time can be increased due to the fact that the thickness of the bonding layer is too high, the bonding force of the coating is reduced, the bonding capability is poor due to the fact that the thickness of the bonding layer is too low, and the bonding layer is easy to oxidize and peel off.
Preferably, as an improvement, the heat insulating and cooling layer is (RE) 3 TaO 7 ) 1-x (RETaO 4 ) x The value range of x is 0.2-0.8, and the thickness of the cooling and heat-insulating layer is 200-1000um.
In this solution, (RE) 3 TaO 7 )/(RETaO 4 ) The two-phase ceramic is used as the heat insulation and temperature reduction layer because both the two layers have extremely low heat conductivity, and the coating is of a porous structure to further reduce the heat conductivity so as to provide excellent heat insulation and temperature reduction effects, and the characteristics of the two-phase composition can inhibit the growth of crystal grains, improve the anti-sintering performance of the material and ensure that the porosity in the coating is basically unchanged; and the existence of interfacial thermal resistance between two phases of ceramics can further reduce the heat transfer performance of the material. x is selected from the group consisting ofThe coating in this range has extremely low thermal conductivity and excellent mechanical properties, including high fracture toughness and high hardness; while other contents result in too high a material thermal conductivity or insufficient fracture toughness and hardness, reducing the life and protective properties of the coating. Foretell cooling insulating layer thickness is for the better thickness range through experimental verification, and cooling insulating layer thickness is too high can increase material weight, reduces the cohesion between layer to lead to the coating to become invalid, and cooling insulating layer thickness crosses lowly can thermal-insulated barrier propterty not enough, is difficult to provide effective protection for the substrate material, and the impact of high-speed particle makes too thin coating drop simultaneously in the use.
Preferably, as an improvement, the corrosion resistant layer is AlTaO 4 The thickness of the anti-corrosion layer of the ceramic is 30-100um.
In the technical scheme, alTaO 4 The ceramic surface is compact, the contact angle of the ceramic surface and water is more than 90 degrees, and the ceramic surface has the characteristic of hydrophobicity, and can have super-hydrophobicity by regulating and controlling phase morphology, so that the water vapor corrosion resistance of the material is improved; meanwhile, the aluminum tantalate and the low-melting-point oxide have good chemical compatibility and are not easy to react with each other, and the existence of the compact coating enables the low-melting-point oxide solution to directly slide off the surface of the coating, so that the low-melting-point oxide solution is prevented from entering the inside of the coating and reacting with alumina and composite ceramic. The thickness of the corrosion-resistant layer is a better thickness range verified by tests, the weight of the material is increased when the thickness of the corrosion-resistant layer is too high, so that the bonding strength between the layers is reduced, and the corrosion resistance of the coating is reduced when the thickness of the corrosion-resistant layer is too low, so that the coating is corroded, sintered and densified.
Preferably, as an improvement, in the step I, the power of the spray gun is 35-45kW, the distance of the spray gun is 50-100mm, the flow rates of argon and hydrogen are 45-50/8-10 and 30-45/6-15slpm respectively, the feeding speed is 30-40g/min, the speed of the spray gun is 300-600mm/s, and the spraying time is 2-10min.
In the technical scheme, when the adhesive layer is sprayed, an atmospheric plasma spraying mode is adopted, and the coating prepared by adopting the mode is compact, low in porosity and high in bonding strength. In the spraying process, the power of the spray gun, the speed of the spray gun, the air flow, the feeding speed and the spraying time have certain influence on the spraying effect and strength, the parameters are determined through experiments, the appearance, the phase-free structure and the performance of the coating can be changed under the condition of changing conditions, and the excellent performance generated in the experiment cannot be provided. The spray gun cannot melt powder to spray the powder in a liquid form when the power of the spray gun is too low, and the sprayed coating is seriously amorphized when the power of the spray gun is too high, so that the original crystal structure of the coating is changed; the distance of the spray gun is determined to ensure the spraying power and the coating thickness, and the distance is matched with the air flow, the feeding speed and the spraying speed, so that the coating with a specific crystal structure, a microstructure, a porosity and a thickness can be obtained in corresponding time, and the service use requirement can be met.
Preferably, as an improvement, in the step II, the process parameters of the atmospheric plasma spraying are that the power of a spray gun is 30-40kW, the distance of the spray gun is 80-120mm, the gas flows of argon and hydrogen are respectively 30-40/10-15 and 30-45/10-15slpm, the feeding speed is 30-50g/min, the speed of the spray gun is 100-300mm/s, and the spraying time is 5-10min; in the step III, the technological parameters of the atmospheric plasma spraying are that the power of a spray gun is 35-42kW, the distance of the spray gun is 100-150mm, the flow rates of argon and hydrogen are 32-42/10-15 and 40-43/10-12slpm respectively, the feeding speed is 35-60g/min, the speed of the spray gun is 200-500mm/s, and the spraying time is 2-10min.
In the technical scheme, when the anti-corrosion layer is sprayed, an atmospheric plasma spraying mode is adopted, and the coating prepared by adopting the mode is compact, low in porosity and high in bonding strength. In the spraying process, the power of the spray gun, the speed of the spray gun, the air flow, the feeding speed and the spraying time have certain influence on the spraying effect and strength, the parameters are determined through experiments, the appearance, the phase-free structure and the performance of the coating can be changed under the condition of changing conditions, and the excellent performance generated in the experiment cannot be provided. The spray gun cannot melt powder to spray the powder in a liquid form when the power of the spray gun is too low, and the sprayed coating is seriously amorphized when the power of the spray gun is too high, so that the original crystal structure of the coating is changed; the distance of the spray gun is determined in order to ensure the spraying power and the coating thickness, and the distance is matched with the air flow, the feeding speed and the spraying speed, so that the coating with a specific crystal structure, a microstructure, a porosity and a thickness is obtained in corresponding time, and the service use requirement is met.
Drawings
FIG. 1 is a schematic structural diagram of a corrosion-resistant, sintering-resistant, and high-temperature creep-resistant alumina composite ceramic material.
FIG. 2 shows the result of the contact angle test of aluminum tantalate ceramics with water (bottom aluminum tantalate, spherical shape as water drop).
FIG. 3 is a microstructure diagram of a corrosion-resistant, sintering-resistant, high temperature creep-resistant alumina composite ceramic material.
Detailed Description
The following is further detailed by way of specific embodiments:
reference numerals in the drawings of the specification include: the aluminum oxide composite ceramic base body 1, the bonding layer 2, the heat insulation and cooling layer 3 and the anti-corrosion layer 4.
The scheme is summarized as follows:
as shown in figures 1 and 3, the aluminum oxide composite ceramic with corrosion resistance, sintering resistance and high temperature creep resistance consists of an aluminum oxide composite ceramic substrate 1, an adhesive layer 2, a heat insulation and cooling layer 3 and an anti-corrosion layer 4 which are sequentially arranged.
Wherein, the alumina composite ceramic matrix is one or more fiber reinforced alumina ceramics in alumina, zirconia or silica fiber.
The bonding layer is NiCoCrAlY modified by noble metal, the noble metal is one or more of platinum, palladium, rhodium, ruthenium, iridium and osmium, and the addition amount of the noble metal is 1-10% of the mass of the NiCoCrAlY; the thickness of the adhesive layer is 100-200um.
The heat insulation and temperature reduction layer is (RE) 3 TaO 7 ) 1-x (RETaO 4 ) x The value range of x is 0.2-0.8, and the thickness of the heat insulation and cooling layer is 200-1000um.
The anti-corrosion layer is AlTaO 4 The thickness of the anti-corrosion layer of the ceramic is 30-100um, and is shown in figure 2, which is the result of the contact angle test of the aluminum tantalate ceramic and water, wherein the bottom is aluminum tantalate and the ball is roundThe aluminum tantalate ceramic is shaped into a water drop, and the water contact angle of the aluminum tantalate ceramic at room temperature is 103 degrees (far more than 90 degrees), which proves that the aluminum tantalate ceramic has the characteristic of hydrophobicity.
A preparation method of the aluminum oxide composite ceramic with corrosion resistance, sintering resistance and high temperature creep resistance comprises the following steps:
step I: preparing a bonding layer with the thickness of 100-200um on the surface of the alumina composite ceramic by an atmospheric plasma spraying mode, wherein the process parameters of the atmospheric plasma spraying are that the power of a spray gun is 35-45kW, the distance of the spray gun is 50-100mm, the gas flow of argon and hydrogen is 45-50/8-10 and 30-45/6-15slpm respectively, the feeding speed is 30-40g/min, the speed of the spray gun is 300-600mm/s, and the spraying time is 2-10min;
step II: preparing (RE) on the surface of the bonding layer by means of atmospheric plasma spraying 3 TaO 7 ) 1-x (RETaO 4 ) x The thickness of the coating is 200-1000um according to the requirements of temperature reduction and heat insulation; first using Y 2 O 3 And Ta 2 O 5 Prepared into spherical (RE) by a high-temperature solid-phase method 3 TaO 7 ) 1-x (RETaO 4 ) x Two-phase powder, wherein the process parameters of the spray gun power is 30-40kW, the spray gun distance is 80-120mm, the gas flow rates of argon and hydrogen are respectively 30-40/10-15 and 30-45/10-15slpm, the feeding speed is 30-50g/min, the spray gun speed is 100-300mm/s, and the spraying time is 5-10min;
step III: preparing compact AlTaO on the surface of the heat insulation and cooling layer by means of atmospheric plasma spraying 4 An anti-corrosion layer, the thickness of the coating is 30-100um; first of all, al is used 2 O 3 And Ta 2 O 5 Preparing spherical AlTaO by high-temperature solid-phase method 4 The technological parameters of the spherical powder during atmospheric plasma spraying are that the power of a spray gun is 35-42kW, the distance of the spray gun is 100-150mm, the flow rates of argon and hydrogen are 32-42/10-15 and 40-43/10-12slpm respectively, the feeding speed is 35-60g/min, the speed of the spray gun is 200-500mm/s, and the spraying time is 2-10min.
Examples 1 and 6 are examples of the present invention,comparative examples 1 to 10 are comparative examples of the present invention, and each example and comparative example are different only in the selection of specific raw materials and some parameters in the preparation process, and are described in table 1. Wherein the base fiber is an alumina composite ceramic matrix; the adhesive layer additive refers to the selection and addition of noble metal in the noble metal modified NiCoCrAlY, and the thickness refers to the thickness of the adhesive layer; material/thickness of heat insulating and cooling layer refers to heat insulating and cooling layer (RE) 3 TaO 7 ) 1-x (RETaO 4 ) x Specific choice of two-phase ceramic/thickness of insulating cooling layer.
TABLE 1
Figure BDA0003377354220000061
Figure BDA0003377354220000071
Figure BDA0003377354220000081
The performance tests were conducted on the corrosion-resistant, sintering-resistant, and high-temperature creep-resistant alumina composite ceramics prepared in the above examples and comparative examples, respectively.
The first experimental example: corrosion resistance test
The test method comprises the following steps: after the coating is prepared according to the method, alO with the molar ratio of 33CaO-9MgO-13 is placed on the surface of the coating 1.5 -45SiO 2 The placement amount of the mixed powder of the low-melting-point oxides is 30mg/cm 2 And then the material is placed in a high-temperature furnace and is kept at 1300 ℃ for 20 hours, and then the material is taken out and cut into a section for SEM observation of the reaction permeation condition of the CMAS component in the coating. If the corrosion resistance of the coating material is poor, the coating material reacts with CMAS components to react and penetrate intensely and continuously, so that the deeper the penetration depth is, the poorer the CMAS corrosion resistance is.
And (3) detection results: examples 1-6 and comparative example 3 were aluminum tantalate coatings with strong corrosion resistance on the surface, wherein the tantalum element was saturated with aluminum and was difficult to react with the CMAS component, thus the reaction penetration depth was less than 10 microns at 1300 ℃ for 20 hours, whereas the bond coat material reacted with CMAS in comparative example 1, leaving no bond coat on the surface, whereas the rare earth element in the rare earth tantalate in comparative example 2 reacted strongly with the CMAS component to a penetration depth of over 100 microns, severely damaging the coating structure and coating properties, which had lost the effect of protecting the substrate. Comparative example 4 is not modified by noble metal, the bonding layer material is easy to be oxidized to generate oxide by heat, and huge thermal stress is generated between the ceramic layer and the bonding layer, so that the bonding force between layers is reduced, and the service life of the coating is shortened; comparative example 5 the adhesive layer was too low in thickness, with a certain adhesion layer that allowed good bonding of the coating to the substrate, but the adhesion layer was oxidized after a period of time, while the too thin adhesive layer failed prematurely due to diffusion of its components to the substrate and ceramic layer; comparative example 6 the coefficient of the two-phase ceramic in the heat insulation and temperature reduction layer is changed, and the ceramic layer has too high thermal conductivity to provide effective heat insulation protection effect, so that the bonding layer is rapidly oxidized and loses efficacy; comparative example 7 the corrosion resistant layer was too low in thickness to fail prematurely when subjected to corrosion by the outer low melting point oxide or the low melting point oxide penetrated directly through the corrosion resistant layer to destroy the inner insulating and cooling layer; comparative example 8 uses a single-phase ceramic, resulting in too high thermal conductivity of the ceramic layer to provide effective thermal insulation protection, causing rapid oxidation failure of the bonding layer; the anti-corrosion layer of the comparative example 9 is too thick, so that the centrifugal force generated by the excessive self weight of the coating is too large and the coating fails in advance, the addition amount of the noble metal of the bonding layer of the comparative example 10 is too high, so that the cost is increased, and meanwhile, the bonding layer is difficult to melt for spraying, so that the bonding layer coating which meets the bonding strength and the appearance cannot be prepared. It can be seen that the materials prepared in examples 1-6 have strong corrosion resistance.
Experimental example II: test for resistance to sintering
The test method comprises the following steps: the porosity of the alumina ceramic composite matrix used in the examples and comparative examples was 10%, and the sintering resistance of the material was tested by heating the surface of the coating layer with a flame gun after the coating layer was prepared, by heating the coating layer to 1400 ℃ for 5 minutes in 20 seconds by flame, then cooling the coating layer in air for 5 minutes, and performing the same heating and cooling again, after repeating the above cycle for 100 times, the porosity of the matrix alumina ceramic composite matrix was measured, and the larger the porosity, the better the sintering resistance.
And (3) detection results: the alumina ceramic composite substrates of examples 1-6 had porosities of 8.1%, 9.5%, 8.8%, 8.7%, 9.0%, and 8.3%, respectively, while comparative examples 1-3 had porosities of 3.9%, 5.2%, and 1.1%. In the comparative example 3, the coating completely falls off in the cycle 3 without the adhesive layer, and the substrate is not protected at all, so the shrinkage of pores is the most serious, the adhesive layer on the surface in the comparative example 1 has a certain antioxidation effect, but the protective effect on the substrate material is lost due to the complete oxidation and peeling of the adhesive layer in the 62 experiments, so the pores are serious. Comparative example 4 is not modified by noble metal, the bonding layer material is easy to be oxidized to generate oxide by heat, and huge thermal stress is generated between the ceramic layer and the bonding layer, so that the bonding force between layers is reduced, and the service life of the coating is shortened; comparative example 5 the adhesive layer is too low in thickness, having a certain adhesion layer to allow good bonding of the coating to the substrate, but the adhesion layer will be oxidized after a certain period of time, while an excessively thin adhesion layer will fail prematurely due to diffusion of its components to the substrate and the ceramic layer; comparative example 6 the coefficient of the two-phase ceramic in the heat insulation and temperature reduction layer is changed, and the ceramic layer has too high thermal conductivity to provide effective heat insulation protection effect, so that the bonding layer is rapidly oxidized and loses efficacy; comparative example 7 the corrosion resistant layer was too low in thickness to fail prematurely when subjected to corrosion by the outer low melting point oxide or the low melting point oxide penetrated directly through the corrosion resistant layer to destroy the inner heat insulating and cooling layer; comparative example 8 uses a single-phase ceramic, resulting in too high thermal conductivity of the ceramic layer to provide effective thermal insulation protection, causing rapid oxidation failure of the bonding layer; the anti-corrosion layer of the comparative example 9 is too thick, so that the centrifugal force generated by the excessive self weight of the coating is too large and the coating fails in advance, the addition amount of the noble metal of the bonding layer of the comparative example 10 is too high, so that the cost is increased, and meanwhile, the bonding layer is difficult to melt for spraying, so that the bonding layer coating which meets the bonding strength and the appearance cannot be prepared.
Experiment example three: high temperature creep resistance test
The test method comprises the following steps: the high creep of the material is tested by a three-point bending method, the specific process is that after a corresponding coating material is prepared on the surface of a long strip-shaped substrate with the size of 3 x 4 x 36mm, the material is kept at 1300 ℃, the three-point bending test is carried out, the load in the test process is continuously increased until the material is broken, and the higher the load when the material is broken, the better the high-temperature creep resistance is.
And (3) detection results: the fracture pressure of the samples in examples 1-6 is 150-200MPa, while the fracture pressure of the samples in comparative examples 1-10 is 120-135MPa, so that the prepared coating material can obviously improve the high-temperature creep resistance of the alumina ceramic composite material.
The foregoing is merely an example of the present invention and common general knowledge in the art of designing and/or characterizing particular aspects and/or features is not described in any greater detail herein. It should be noted that, for those skilled in the art, without departing from the technical solution of the present invention, several variations and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.

Claims (8)

1. The aluminum oxide composite ceramic with corrosion resistance, sintering resistance and high temperature creep resistance is characterized in that: the heat-insulating and temperature-reducing aluminum oxide composite ceramic substrate consists of an aluminum oxide composite ceramic substrate, an adhesive layer, a heat-insulating and temperature-reducing layer and an anti-corrosion layer; the bonding layer is NiCoCrAlY modified by noble metal, and in the NiCoCrAlY modified by noble metal, the addition amount of the noble metal is 1-10% of the mass of the NiCoCrAlY; the heat insulation and temperature reduction layer is (RE) 3 TaO 7 ) 1-x (RETaO 4 ) x The value range of x is 0.2-0.8, and the thickness of the cooling and heat-insulating layer is 200-1000um.
2. The corrosion-resistant sintering-resistant high-temperature creep-resistant alumina composite ceramic according to claim 1, wherein: the alumina composite ceramic matrix is one or more fiber reinforced alumina ceramics in alumina, zirconia or silica fibers.
3. The alumina composite ceramic of claim 2, which is resistant to corrosion, sintering and high temperature creep, and is characterized in that: the noble metal is one or more of platinum, palladium, rhodium, ruthenium, iridium and osmium.
4. The corrosion-resistant sintering-resistant high temperature creep-resistant alumina composite ceramic according to claim 3, wherein: the thickness of the bonding layer is 100-200um.
5. The corrosion-resistant sintering-resistant high temperature creep-resistant alumina composite ceramic according to claim 4, wherein: the anti-corrosion layer is AlTaO 4 The thickness of the anti-corrosion layer of the ceramic is 30-100um.
6. The preparation method of the corrosion-resistant, sintering-resistant and high-temperature creep-resistant alumina composite ceramic is characterized by comprising the following steps of:
step I: preparing an adhesive layer on the surface of the alumina composite ceramic in an atmospheric plasma spraying manner;
step II: preparing (RE) on the surface of the bonding layer by means of atmospheric plasma spraying 3 TaO 7 ) 1-x (RETaO 4 ) x A porous structure heat insulation and cooling layer consisting of two-phase ceramics;
step III: preparing compact AlTaO on the surface of the heat insulation and cooling layer by means of atmospheric plasma spraying 4 And (4) an anti-corrosion layer.
7. The method for preparing the corrosion-resistant sintering-resistant high-temperature creep-resistant alumina composite ceramic according to claim 6, wherein the method comprises the following steps: in the step I, the technological parameters of the atmospheric plasma spraying are that the power of a spray gun is 35-45kW, the distance of the spray gun is 50-100mm, the gas flow rates of argon and hydrogen are 45-50/8-10 and 30-45/6-15slpm respectively, the feeding speed is 30-40g/min, the speed of the spray gun is 300-600mm/s, and the spraying time is 2-10min.
8. The method for preparing the corrosion-resistant sintering-resistant high-temperature creep-resistant alumina composite ceramic according to claim 7, wherein the method comprises the following steps: in the step II, the technological parameters of the atmospheric plasma spraying are that the power of a spray gun is 30-40kW, the distance of the spray gun is 80-120mm, the flow rates of argon and hydrogen are respectively 30-40/10-15 and 30-45/10-15slpm, the feeding speed is 30-50g/min, the speed of the spray gun is 100-300mm/s, and the spraying time is 5-10min; in the step III, the technological parameters of the atmospheric plasma spraying are that the power of a spray gun is 35-42kW, the distance of the spray gun is 100-150mm, the gas flow rates of argon and hydrogen are respectively 32-42/10-15 and 40-43/10-12slpm, the feeding speed is 35-60g/min, the speed of the spray gun is 200-500mm/s, and the spraying time is 2-10min.
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