CN108455978B - Surface-toughened alumina fiber rigid heat-insulating tile multilayer composite material, coating composition, preparation method and application thereof - Google Patents
Surface-toughened alumina fiber rigid heat-insulating tile multilayer composite material, coating composition, preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a surface-toughened alumina fiber rigid heat-insulating tile multilayer composite material, a coating composition, a preparation method and application thereof. The composite material comprises a porous alumina fiber matrix, a surface toughened alumina compact ceramic layer, a high-emissivity oxide thermal barrier coating and a low-chemical-catalytic-coefficient glass coating. The coating composition includes a surface toughened alumina dense ceramic layer composition, a high emissivity oxide thermal barrier coating composition, and a low chemical catalytic coefficient glass coating composition. The preparation method of the composite material comprises the steps of sequentially preparing the substrate, the compact ceramic layer, the thermal barrier coating and the glass coating. The invention also provides the use of the composite material in a thermal protection material for the outer surface of an aircraft. The invention adopts a novel process technology and utilizes a unique substrate and a coating composition to prepare the composite material which can be repeatedly used for a long time in an environment of 1600 ℃ and has excellent temperature resistance.
Description
The application is a divisional application of 2016, 14, 201610825929.7 entitled "multilayer composite material of aluminum oxide fiber rigid heat insulation tile with toughened surface, coating composition, preparation method and application thereof".
Technical Field
The invention relates to a surface-toughened alumina fiber rigid heat-insulating tile multilayer composite material and a preparation method thereof, belonging to the technical field of functional composite materials.
Background
The oxide ceramic fiber rigid heat insulation tile multilayer composite material is used as a heat protection material on the outer surface of an aircraft, and has the advantages of high temperature resistance, light weight, reusability and the like. Therefore, the American space shuttle adopts the multilayer composite material of the rigid heat insulation tile as the heat protection material in a large area. Typical Rigid insulating tile multilayer composite substrates include LI-900 and LI-2200 (U.S. Pat. No. 3952083), FRCI (U.S. Pat. No. 4148962), HTP (R.P. Banas. et. al., thermal and Mechanical Properties of the HTP Family of Hot Ceramic Insulation Materials, AIAA-85-1055), AETB (Daniel B.Leiser et. al., operations for Improving thermal Ceramic Insulation Materials, 6, No.7-8, pp.757-768, 1985), and BRI (U.S. Pat. No. 6716782B 2). The five rigid heat-insulating tile multilayer composite materials all take quartz fiber as a main component. However, the reusable temperature limit of the multilayer composite material of the rigid heat insulation tile taking quartz fiber as the main component is 1500 ℃, and when the temperature is higher than the reusable temperature limit, the quartz fiber can be rapidly crystallized, so that the heat insulation tile is shrunk and deformed, and further the heat insulation tile is failed. Therefore, the multilayer composite material of the rigid heat insulation tile taking quartz fiber as the main component has low reliability when used as the heat insulation material of the outer surface of the aircraft at the temperature higher than 1500 ℃.
The American GE company developed Mullite rigid insulating tile multilayer composite material (REusable External Insulation, REI-Mullite, NASA TMX-2719, pages 17-60) for the thermal protection of the outer surface of the space plane, and the temperature resistance of the composite material is superior to that of LI-900 all-quartz rigid insulating tile multilayer composite material.
The development work of the fiber matrix of the rigid ceramic heat insulation tile is developed from the 80 th century in China. The Shandong Industrial ceramics research design institute of China at CN 101691138A discloses a preparation method of a space shuttle heat insulation tile. The heat insulation tile for the space shuttle is composed of 50-95% of quartz fiber, 5-50% of alumina fiber and 0-5% of boron nitride powder sintering agent. The formulation of the insulating tile coating disclosed in this patent contains a large amount of alkali metal and alkaline earth metal ions, which causes a significant decrease in the viscosity of the coating at high temperatures, limiting the service temperature of the insulating tile, and thus such a coating can only be used below 1200 ℃.
CN102199042A discloses a composition of a lightweight rigid ceramic heat insulation tile and a preparation method thereof. The rigid ceramic heat insulation tile consists of 50 to 100 percent of quartz fiber and 0 to 50 percent of mullite fiber, wherein a boron nitride powder sintering agent accounting for 0.01 to 15 percent of the mass of the ceramic fiber is added, and silicon carbide powder accounting for 0 to 20 percent of the mass of the ceramic fiber is added as a high-temperature radiation resistant agent. CN 104529369a and CN201510632711.5 disclose a method for preparing a rigid heat insulation tile multilayer composite material composed of quartz fibers, alumina fibers and/or zirconia fibers.
The flight speed of the new generation of high-speed aircraft reaches several Mach or even more than ten Mach, the temperature of the large-area position of the windward side of the aircraft can reach 1500 ℃ to 1650 ℃, so that a rigid heat insulation tile multilayer composite material with higher temperature resistance has to be developed to meet the heat protection requirement of the new generation of high-speed aircraft.
The alumina fiber has excellent temperature resistance, and can be repeatedly used for a long time at a temperature of 1600 ℃. An alumina fiberboard produced by Zircar company in America can be used as a civil product for high-temperature furnace linings, chemical reactor thermal protection and the like. The Zircar company has strict secrecy of the production process of the fiberboard and has no disclosure of the publication. The Zircar company also sells a ceramic precursor suitable for surface densification of its alumina plate, and its specific formulation is not disclosed in the literature. However, there has been no report of using Zircar alumina fiber boards with surface compounded high emissivity coatings as aircraft exterior surface insulation. Therefore, the multilayer composite material of the surface toughened alumina fiber rigid heat insulation tile capable of resisting 1600 ℃ for a long time is independently developed, is applied to the field of ultrahigh temperature heat insulation in the aerospace field, and has important strategic significance.
The frozen gel injection molding method is widely applied to preparing porous ceramic materials. The Shanghai silicate research institute of Chinese academy of sciences proposed the preparation of alumina porous ceramics (CN200610119248.5, CN200610119233.9, CN200710037605.8) by ceramic freeze injection molding with alumina sol. Preparing a porous ceramic material (CN200810150654.7) suitable for a solid oxide fuel cell by using a freeze drying technology at the university of SiAn Richardson; wanlongan et al, university of qinghua, proposed a "freeze-gel forming" process for preparing porous ceramic materials (CN 200710099624.3). The ceramic raw materials used in the above patents are all powders, and the pore-forming agent is water or tert-butyl alcohol, etc. In the actual ceramic preparation process, the ice crystals formed by freezing are converted into large-size defects after the solvent is volatilized, so that the strength of a blank body is low, and the service performance of the material is seriously influenced. The porosity of the porous ceramic material prepared by taking a powder ceramic precursor as a raw material and adopting a freezing gel injection molding process is generally not higher than 50%, and the thermal conductivity of the product is higher; and the pores in the porous ceramic are arranged in an orientation mode, so that the anisotropy of the material is caused.
When the multilayer composite material of the high-temperature-resistant rigid heat insulation tile is used as a large-area heat insulation material on the outer surface of an aircraft, a high-emissivity coating needs to be compounded on the windward side of the heat insulation tile. The high emissivity coating re-radiates a substantial portion of the aerodynamic heat generated during flight of the aircraft back into the low temperature background space. On the other hand, the surface of the heat insulation tile densified by the coating can prevent plasma hot air on the surface of an aircraft from entering the interior of the heat insulation tile body through the pores of the tile during flight, and the mass and heat transfer can be generated. Finally, the high emissivity coating also serves a water-resistant function.
Because the alumina fiber heat insulation tile is a porous material, the porosity is more than 80%, the compressive strength in the thickness direction is only 1.5MPa, and when the high-emissivity coating is directly sprayed on the surface of the material by plasma sputtering, the surface of the heat insulation tile with the sprayed layer is easy to pulverize and break. The surface of the insulating tile to be sprayed with the high emissivity coating must be densified and toughened.
US4093771 discloses a reactive Cured Glass powder (RCG) with high reactivity and a method for preparing a Glass coating using the RCG as a raw material. Such glass frits are suitable for use as surface coatings for lightweight ceramic tile rockschid Insulation (LI, US 3952083). A typical RCG coating formula consists of 97.5 percent of high-activity reaction curing glass powder and 2.5 percent of molybdenum disilicide high-emissivity substances by mass fraction, wherein the sintering temperature is 1150 ℃, and the sintering time is 1.5 hours. However, RCG glass coatings have poor impact resistance and long-term service temperatures of no more than 1260 ℃.
US 5079082 discloses a method of making a Toughened monolithic Fibrous Insulation material (TUFI). The patent adds silicon tetraboride powder as a coating sintering aid on the basis of an RCG glass coating. By reducing the particle size of the particles in the coating slurry, the coating substance penetrates more into the fiber matrix when the coating slurry is sprayed, thereby forming a gradient fiber-reinforced composite. A typical TUFI coating formulation is 77.5% RCG glass powder, 2.5% silicon tetraboride sintering aid and 20% molybdenum disilicide high emissivity substance. The sintering temperature was 1220 ℃ and the sintering time was 1.5 hours. The shock resistance of the TUFI coating is greatly improved compared with that of an RCG glass coating, and the TUFI coating is widely used as a main scheme of a surface coating of a heat insulation tile of a space plane and a heat insulation tile of an aircraft such as X-37, X-43, X-51 and the like. The long-term service temperature of the TUFI coating does not exceed 2600 deg.F (1427 deg.C). The TUFI coating matched well with various grades of rigid insulating tile multi-layer composite substrates (LI, FRCI, AETB, BRI) developed in the United states.
US 7767305B1 discloses a method for preparing a High Efficiency Tantalum-based coating Composite (HETC). TaSi in HETC coating formulation2、 MoSi2And of RCG glass fritThe relative proportion can be optimally designed according to the linear expansion coefficient, the emissivity index requirement and the temperature resistance index requirement of the rigid heat insulation tile multilayer composite material matrix. The HETC coating is not only suitable for the oxide ceramic fiber rigid heat insulation tile multilayer composite material, but also suitable for the carbon fiber light rigid heat insulation tile multilayer composite material. TaSi in HETC coatings2The function of reducing the chemical catalytic coefficient of the coating surface is achieved.
The American GE company develops a REI-Mullite fiber rigid heat-insulating tile multilayer composite material and simultaneously develops a high-emissivity Thermal barrier coating suitable for a heat-insulating tile System, and the main components of the high-emissivity Thermal barrier coating are high-emissivity substances such as nickel oxide, chromium oxide and cobalt oxide, and high-temperature-resistant ceramic fillers such as titanium dioxide, zirconic acid dam and strontium titanate (NASA CR-4227, Thermal Protection System of the Space Shuttle, Appendix III-16).
In China, CN103467074A and CN201510632090.0 respectively disclose a high-temperature resistant coating, a preparation method thereof and an improvement method thereof, the full spectrum emissivity of the prepared high-emissivity coating hemisphere is more than or equal to 0.85, and the thermal expansion property of the high-temperature resistant coating hemisphere can realize good matching with the rigid heat insulation tile multilayer composite material described in CN 201510632711.5.
Disclosure of Invention
The invention aims to overcome the defect that the existing quartz fiber-based reusable light rigid heat insulation tile multilayer composite material is insufficient in temperature resistance, and different technical schemes are adopted to finally provide an alumina fiber rigid heat insulation tile multilayer composite material with higher temperature resistance, reusability, light weight and toughened surface and a preparation method thereof, so as to provide material scheme support for designing a large-area heat protection system on the outer surface of a new-generation high-speed aircraft.
Therefore, the invention achieves the purpose through the following technical scheme:
1. a surface-toughened alumina dense ceramic layer composition, comprising two sol continuous phases including a first sol continuous phase that is an alkaline sol continuous phase and a second sol continuous phase that is an alumina sol and/or a zirconia sol, and at least one refractory ceramic powder dispersed phase; the at least one high temperature resistant ceramic powder dispersed phase is selected from the group consisting of quartz glass powder, alumina powder, boron nitride powder, aluminum nitride powder, zirconia powder and titanium dioxide; preferably, the at least one high-temperature-resistant ceramic powder dispersed phase is aluminum nitride powder and/or quartz glass powder.
2. The surface-toughened alumina dense ceramic layer composition according to claim 1, wherein the surface-toughened alumina dense ceramic layer composition is composed of the two sol continuous phases and the at least one high temperature resistant ceramic powder dispersed phase.
3. The surface-toughened alumina dense ceramic layer composition according to claim 1 or 2, characterized in that:
the amount of the first sol continuous phase is 1 part by mass of a 25 mass% first sol continuous phase;
the second sol continuous phase is 0.7 to 0.8 parts by mass of a 40 mass% second sol continuous phase; and/or
The at least one refractory ceramic dispersed phase is 0.2 to 0.3 parts by mass of a refractory ceramic dispersed phase having a particle size of 1 to 2 microns.
4. The surface-toughened alumina dense ceramic layer composition of claim 3, wherein the surface-toughened alumina dense ceramic layer composition is a composition comprising:
(1)1 part of 25 mass percent alkaline silica sol, 0.7 to 0.8 part of 40 mass percent alumina sol and 0.2 to 0.3 part of 1 to 2 micron aluminum nitride powder;
(2)1 part of 25 mass percent alkaline silica sol, 0.7 to 0.8 part of 30 to 35 mass percent zirconia sol and 0.2 to 0.3 part of aluminum nitride powder with the particle size of 1 to 2 microns;
(3)1 part of 25 percent of alkaline silica sol, 0.7 to 0.8 part of 30 percent to 35 percent of zirconia sol and 0.2 to 0.3 part of quartz glass powder with the grain diameter of 1 to 2 microns.
5. A high emissivity coating composition comprising at least one member selected from the group consisting of yttria stabilized zirconia powder, quartz glass powder, barium zirconate powder, nickel oxide powder, alumina powder, zirconia powder, borosilicate glass powder; more preferably, the high emissivity coating composition comprises:
(1) yttria stabilized zirconia powder;
(2) nickel oxide powder; and
(3) and (3) quartz glass powder.
6. The high emissivity coating composition of claim 1, wherein the high emissivity coating composition comprises:
(1) yttria stabilized zirconia powder;
(2) nickel oxide powder; and
(3) and (3) quartz glass powder.
7. The high emissivity coating composition of claim 5 or 6, wherein:
the particle size of the yttrium oxide stabilized nickel oxide powder is 1 micron to 3 microns;
the particle size of the nickel oxide powder is 1-3 microns; and/or
The particle size of the quartz glass powder is 1 to 3 micrometers.
8. The high emissivity coating composition of any one of claims 5 through 7, wherein:
the high emissivity coating composition comprises 1 part by weight of yttria-stabilized zirconia powder;
the nickel oxide powder in the high-emissivity coating composition is 1.8 to 2.2 parts by weight; and/or
The high emissivity coating composition comprises 2.8 to 3.2 parts by weight of quartz glass powder.
9. A low chemical catalytic coefficient glass coating composition comprising a continuous phase, a high emissivity phase and a high temperature low chemical catalytic coefficient dispersed phase.
10. The low chemical catalytic coefficient glass coating composition according to claim 9, characterized in that the low chemical catalytic coefficient glass coating composition is composed of a continuous phase, a high emissivity phase and a high temperature low chemical catalytic coefficient dispersed phase.
11. The low chemical catalytic coefficient glass coating composition according to claim 9 or 10, characterized in that:
the continuous phase is a reaction cured glass sintering continuous phase;
the high emissivity phase is a molybdenum disilicide high emissivity phase; and/or
The high-temperature low-chemical-catalytic-coefficient dispersed phase is at least one selected from the group consisting of tantalum disilicide, mercury silicide, and tungsten silicide.
12. The low chemical catalytic coefficient glass coating composition according to claim 11, characterized in that:
the continuous phase is 1 part by weight of reaction cured glass sintering continuous phase;
the high emissivity phase is molybdenum disilicide high emissivity phase of 0.4 to 0.6 weight part; and/or
The high-temperature low-chemical catalytic coefficient disperse phase is 0.4 to 0.6 weight part.
13. The low-stoichiometry glass coating composition of any of claims 9-12, wherein the high-temperature, low-stoichiometry diffusive phase comprises at least tungsten silicide and/or mercury silicide.
14. The utility model provides a rigidity heat insulating tile multilayer combined material which characterized in that, rigidity heat insulating tile multilayer combined material includes by inside to outside in proper order:
(1) a porous alumina fiber matrix;
(2) surface toughening alumina compact ceramic layer;
(3) a high emissivity oxide thermal barrier coating; and
(4) low chemical catalytic coefficient glass coating.
15. The multilayer composite material for rigid insulating tiles according to claim 14, characterized in that:
the matrix is prepared from alumina fiber and acidic silica sol;
the surface toughened alumina compact ceramic layer is coated by the surface toughened alumina compact ceramic layer composition in any one of technical schemes 1 to 4;
the high-emissivity oxide thermal barrier coating is coated by the surface toughened alumina compact ceramic layer composition in any one of technical schemes 5 to 8; and/or
The low chemical catalytic coefficient glass coating is prepared by the low chemical catalytic coefficient glass coating composition of any one of the technical schemes 9 to 13.
16. The multilayer composite material for the rigid heat insulation tile according to claim 15 is characterized in that the mass ratio of the alumina fibers to the acidic silica sol is 1:195 to 205, and the concentration of the acidic silica sol is 8 to 10 mass%.
17. The rigid insulating tile multilayer composite according to any of claims 14 to 16, characterized in that:
the thickness of the surface toughened alumina compact ceramic layer is 3mm to 5 mm;
the high emissivity oxide thermal barrier coating has a thickness of 100 to 200 microns; and/or
The low chemical catalytic coefficient glass coating has a thickness of 100 to 200 microns.
18. A method of making the rigid insulating tile multilayer composite of any of claims 14 to 17, comprising the steps of:
(1) mixing the alumina fiber and the acidic silica sol, uniformly stirring, filtering, preparing a wet blank from a filter cake in a wet blank mold, freezing the wet blank in a freezing mold to prepare a frozen blank, drying the frozen blank, and sintering to prepare the porous alumina fiber matrix;
(2) applying the make surface toughened alumina dense ceramic layer composition onto a surface of the porous alumina fiber matrix, drying and curing to form the surface toughened alumina dense ceramic layer;
(3) forming the high emissivity oxide thermal barrier coating by using a plasma sputtering process to deposit the high emissivity oxide thermal barrier coating on the surface toughened alumina dense ceramic layer; and
(4) and coating the low chemical catalytic coefficient glass coating composition on the high-emissivity oxide thermal barrier coating and sintering to form the low chemical catalytic coefficient glass coating.
19. The method according to claim 18, wherein in the step (1):
dispersing alumina fiber by using a blade type shearing stirrer, wherein the stirring speed is 2000-3000 r/min, and the stirring time is 10-30 min;
the filtration is carried out by using a 50-mesh filter screen;
the freezing is performed by using liquid nitrogen, the liquid nitrogen submerges the surface of the freezing mould for 15-20 cm during freezing, and the freezing time is 1-2 hours;
drying the frozen blank at 120 ℃; and/or
The sintering temperature of the sintering is 1250-1500 ℃, and the heat preservation time of the sintering is 1-4 hours.
20. The method according to claim 18 or 19, characterized in that in step (2):
the drying is carried out at room temperature and the curing is carried out at 200 ℃ to 400 ℃.
21. The method according to any one of claims 18 to 20, wherein in the step (3), the process parameters of the plasma sputtering method are as follows: the sputtering carrier gas is oxygen/propane flame, the flow rate of propane is 1150-1250L/h, the flow rate of oxygen is 2200-2300L/h, and the heat flow density of the jet gas flow is 1.15-1.20 MW/m2。
22. The method according to any one of claims 18 to 21, wherein in the step (4), the low chemical catalytic coefficient glass coating is coated by spraying, and the carrier gas pressure is 0.2 to 0.5 MPa; and/or the temperature for sintering the glass coating with the low chemical catalytic coefficient is 1200-1250 ℃, and the heat preservation time for sintering is 0.5-1.5 hours.
23. Use of the rigid insulating tile multilayer composite according to any of claims 14 to 17 or the rigid insulating tile multilayer composite produced by the method of any of claims 18 to 22 in thermal protection of aircraft exterior surfaces, ultra high temperature chemical reactor thermal protection materials, nuclear reactor ultra high temperature thermal protection materials, ultra high temperature kiln insulation liners or metal melt filters.
The present invention, through trial and error, identifies desirable surface toughened alumina dense ceramic layer compositions, and low chemical catalytic coefficient glass coating compositions suitable for forming coatings on the alumina fiber rigid insulating tile multilayer composites made by the present invention such that the rigid insulating tile multilayer composites have desired properties. The method of the invention adopts a frozen gel injection molding process to prepare the fiber substrate, and selects the proper surface toughened alumina compact ceramic layer composition, the surface toughened alumina compact ceramic layer composition and the low chemical catalytic coefficient glass coating composition to form a surface toughened alumina compact ceramic layer, a surface toughened alumina compact ceramic layer and a low chemical catalytic coefficient glass coating in turn. The prepared multilayer composite material of the rigid heat insulation tile is a multilayer composite material of an aluminum oxide fiber rigid heat insulation tile with toughened surface, and comprises an aluminum oxide fiber heat insulation tile substrate A, a surface toughened compact aluminum oxide ceramic layer B, a high-emissivity coating C and a low-chemical-catalysis-coefficient compact glass coating D. The process flow for preparing the rigid heat insulation tile multilayer composite material comprises the following steps:
firstly, preparing a fiber matrix A by using a frozen gel casting process. The invention discloses a method for preparing a porous ceramic by using a frozen gel casting method, which is mainly used for preparing porous ceramics taking ceramic powder as a raw material and used for civil occasions such as a metal melt filter.
Secondly, coating and surface toughening compact alumina ceramic layer, especially compact composition containing alumina sol and aluminum nitride powder, on the outer surface of the substrate A, and sintering at high temperature after the reagent is solidified, thereby preparing surface toughening compact alumina ceramic layer B;
thirdly, preparing a high-emissivity coating C outside the ceramic layer B by using a plasma sputtering spraying method;
and fourthly, the inventor finds out through multiple experiments that the high-emissivity oxide thermal barrier coating cannot obtain a smooth coating on the surface of the surface toughened alumina compact ceramic layer, so that the high-temperature-resistant low-catalytic-coefficient compact glass coating D is prepared on the outer layer of the high-emissivity oxide thermal barrier coating.
The innovation points of the invention are at least as follows:
(1) the aluminum oxide fiber rigid heat insulation tile multilayer composite material with the toughened surface, which is prepared by the invention, can be repeatedly used for a long time in an environment of 1600 ℃, and the temperature resistance is superior to that of the existing rigid heat insulation tile multilayer composite material, such as the rigid heat insulation tile multilayer composite material taking quartz fiber and the like as main components;
(2) the invention creatively uses the freezing gel injection molding method to prepare the aluminum oxide fiber rigid heat insulation tile multilayer composite material matrix with high performance;
(3) the inventor develops a surface toughening and densifying method for a multilayer composite material of an alumina fiber rigid heat insulation tile;
(4) the inventor develops a formula and a process for a high-emissivity coating on the surface of a multi-layer composite material of an alumina fiber rigid heat-insulating tile;
(5) the present inventors developed high emissivity coating formulations and innovatively produced high emissivity coatings using a plasma sputter coating process.
The aluminum oxide fiber rigid heat-insulating tile multilayer composite material with the toughened surface can be used for various purposes such as a heat protection material on the outer surface of an aircraft, a heat protection material of an ultrahigh-temperature chemical reactor, a nuclear reactor ultrahigh-temperature heat protection material, a heat-insulating lining of an ultrahigh-temperature kiln, a metal melt filter and the like.
Drawings
FIG. 1 is a schematic structural view of a multi-layer composite material of an alumina fiber rigid heat insulation tile of the present invention. Wherein 1 is the main structure of the alumina fiber heat insulation tile; 2 is a surface toughened compact alumina ceramic layer; 3 is a non-smooth high-emissivity coating prepared by using a plasma sputtering spraying process; 4 is a low chemical catalytic coefficient smooth glass coating prepared by using a spraying-sintering process; 5 is designed to reserve a breathing zone, and when the multi-layer composite material of the alumina fiber rigid heat insulation tile is heated in the using process, air in the matrix can be dissipated to the background space through the channel.
FIG. 2 is a flow chart of the preparation process of the multilayer composite material of the alumina fiber rigid heat insulation tile, which comprises four steps of substrate preparation, surface densification, high emissivity coating preparation and low catalytic coefficient coating preparation.
FIG. 3 is a scanning electron micrograph of a multi-layer composite matrix of the alumina fiber rigid heat-insulating tile of the present invention.
Detailed Description
As described above, the present invention provides in a first aspect a surface-toughened alumina dense ceramic layer composition comprising two sol continuous phases including a first sol continuous phase which is an alkaline sol continuous phase and a second sol continuous phase which is an alumina sol and/or a zirconia sol, and at least one refractory ceramic powder dispersoid phase; the at least one high temperature resistant ceramic powder dispersed phase is selected from the group consisting of quartz glass powder, alumina powder, boron nitride powder, aluminum nitride powder, zirconia powder and titanium dioxide, preferably aluminum nitride powder and/or quartz glass powder.
In some preferred embodiments, the surface toughened alumina dense ceramic layer composition consists of the two sol continuous phases and the at least one high temperature resistant ceramic powder dispersed phase.
In some more preferred embodiments, the first sol continuous phase is used in an amount of 1 part by mass of 25% by mass of the first sol continuous phase.
It is also preferable that the second sol continuous phase is 0.7 to 0.8 parts by mass of 40% by mass of the second sol continuous phase.
It is also preferred that the at least one refractory ceramic dispersed phase is 0.2 to 0.3 parts by mass of a refractory ceramic dispersed phase having a particle size of 1 to 2 microns.
In some further preferred embodiments, the surface-toughened alumina dense ceramic layer composition may comprise 1 part by mass of 25% basic silica sol, 0.7 to 0.8 part by mass of 40% alumina sol, 0.2 to 0.3 part of aluminum nitride powder having a particle size of 1 to 2 microns. In other preferred embodiments, the surface-toughened alumina dense ceramic layer composition may include 1 part by mass of 25% alkaline silica sol, 0.7 to 0.8 part by mass of 30% to 35% zirconia sol, and 0.2 to 0.3 part by mass of 1 to 2 μm aluminum nitride powder. In other preferred embodiments, the surface-toughened alumina dense ceramic layer composition may include 1 part by mass of 25% alkaline silica sol, 0.7 to 0.8 part by mass of 30% to 35% zirconia sol, and 0.2 to 0.3 part by mass of 1 to 2 μm silica glass frit.
In a second aspect, the present invention provides a high emissivity coating composition comprising at least one selected from the group consisting of yttria stabilized zirconia powder, quartz glass powder, zirconic acid dam powder, nickel oxide powder, alumina powder, zirconia powder, borosilicate glass powder. More preferably, the high emissivity coating composition comprises: (1) yttria stabilized zirconia powder; (2) nickel oxide powder; and (3) quartz glass frit.
In some more preferred embodiments, the high emissivity coating composition is comprised of: (1) yttria-stabilized zirconia powder; (2) nickel oxide powder; and (3) quartz glass frit.
In some preferred embodiments, the yttria-stabilized zirconia powder has a particle size of from 1 micron to 3 microns (e.g., 1, 2, or 3 microns). The nickel oxide powder has a particle size of 1 micron to 3 microns (e.g., 1, 2, or 3 microns). In addition, the particle size of the silica glass frit is 1 to 3 micrometers (e.g., 1, 2, or 3 micrometers).
In some more preferred embodiments, the high emissivity coating composition comprises 1 part by weight yttria-stabilized zirconia powder, 1.8 to 2.2 parts by weight nickel oxide powder, and 2.8 to 3.2 parts by weight silica glass powder.
In a third aspect, the present invention provides a low chemical catalytic coefficient glass coating composition comprising a continuous phase, a high emissivity phase and a high temperature low chemical catalytic coefficient dispersed phase.
More preferably, the low chemical catalytic coefficient glass coating composition consists of a continuous phase, a high emissivity phase and a high temperature low chemical catalytic coefficient dispersed phase.
In some preferred embodiments, the continuous phase may be a reaction-cured glass-sintered continuous phase. It is also preferred that the high emissivity phase may be a molybdenum disilicide high emissivity phase. It is also preferable that the high-temperature low-chemical-catalytic-coefficient dispersed phase is at least one selected from the group consisting of tantalum disilicide, mercury silicide, and tungsten silicide.
In some more preferred embodiments, the continuous phase is a reaction-cured glass-sintered continuous phase of 1 part by weight and the high emissivity phase is a molybdenum disilicide high emissivity phase of 0.4 to 0.6 parts by weight; the high-temperature low-chemical catalytic coefficient disperse phase is 0.4 to 0.6 weight part.
In some particularly preferred embodiments, the high temperature low chemical catalytic coefficient dispersed phase comprises at least tungsten silicide and/or mercury silicide. The inventor surprisingly found that the tantalum disilicide powder contained in the high-temperature low-chemical-catalytic-coefficient dispersed phase can be replaced by tungsten silicide, mercury silicide and the like, and the effect of reducing the catalytic coefficient of the coating can be achieved.
The present invention provides in a third aspect a rigid insulating tile multilayer composite comprising: (1) a porous alumina fiber matrix; (2) surface toughening alumina compact ceramic layer; (3) a high emissivity oxide thermal barrier coating; and (4) a low chemical catalytic coefficient glass coating.
In some preferred embodiments, the matrix is made from alumina fibers and an acidic silica sol; the surface toughened alumina dense ceramic layer is coated by the surface toughened alumina dense ceramic layer composition of the first aspect of the invention; the high-emissivity oxide thermal barrier coating is coated by the surface toughened alumina compact ceramic layer composition of the second aspect of the invention; and/or the low chemical catalytic coefficient glass coating is made from the low chemical catalytic coefficient glass coating composition of the third aspect of the invention.
In some preferred embodiments, the mass ratio of the alumina fibers to the acidic silica sol is from 1:195 to 205, more preferably 1: 200. The concentration of the acidic silica sol is 8 to 10 mass%, for example 8, 9 or 10 mass%.
The present invention does not specifically limit the thickness of each layer as long as the desired properties can be achieved. However, in some preferred embodiments, the surface toughened alumina dense ceramic layer has a thickness of 3mm to 5 mm. The high emissivity oxide thermal barrier coating may have a thickness of 100 microns to 200 microns, such as 100, 110, 120, 130, 140, 150, 160, 170, 180, 190, or 200 microns. Additionally, the low chemical catalytic coefficient glass coating may have a thickness of 100 microns to 200 microns, such as 100, 110, 120, 130, 140, 150, 160, 170, 180, 190, or 200 microns.
The present invention provides in a fifth aspect a method of manufacturing a rigid insulating tile multilayer composite according to the fourth aspect of the invention, the method comprising the steps of:
(1) mixing the alumina fiber and the acidic silica sol, uniformly stirring, filtering, preparing a wet blank from a filter cake in a wet blank mold, freezing the wet blank in a freezing mold to prepare a frozen blank, drying the frozen blank, and sintering to prepare the porous alumina fiber matrix;
(2) applying the make surface toughened alumina dense ceramic layer composition onto a surface of the porous alumina fiber matrix, drying and curing to form the surface toughened alumina dense ceramic layer;
(3) forming the high emissivity oxide thermal barrier coating by using a plasma sputtering process to deposit the high emissivity oxide thermal barrier coating on the surface toughened alumina dense ceramic layer; and
(4) and coating the low chemical catalytic coefficient glass coating composition on the high-emissivity oxide thermal barrier coating and sintering to form the low chemical catalytic coefficient glass coating.
In some preferred embodiments, in step (1), the alumina fibers are dispersed using a paddle shear mixer at a mixing speed of 2000 to 3000 revolutions per minute (e.g., 2000, 2500, or 3000 revolutions per minute) for a mixing time controlled to be 10 to 30 minutes, e.g., 10, 15, 20, 25, or 30 minutes. Too high a stirring speed or too long a stirring time may result in too short an alumina fiber being beaten and too high a bulk density of the filtered green body, e.g. > 0.6g/cm3The low density requirements of spacecraft insulation may not be met. The filtering device used for the filtration is not particularly limited in the present invention, but it is preferable that the mesh number of the filtering device is 50. The filtration can be carried out by gravity sedimentation.
In some preferred embodiments, the freezing is performed using liquid nitrogen which is submerged 15cm to 20cm above the surface of the freezing mold for 1 hour to 2 hours. The freezing medium is water contained in silica sol.
When the frozen blank is dried, the frozen blank may be dried at 120 ℃.
The sintering temperature of the sintering is 1250 ℃ to 1500 ℃ (for example 1250, 1300, 1350, 1400, 1450 or 1500 ℃), and the holding time of the sintering is 1 hour to 4 hours (for example 1, 2, 3 or 4 hours).
In the step (2), it is preferable that the drying is performed at room temperature and the curing is performed at 200 to 400 ℃ (e.g., 200, 300, or 400 ℃).
In the step (3), it is preferable that the process parameters of the plasma sputtering method are as follows: the sputtering carrier gas is oxygen/propane flame, the flow rate of propane is 1150-1250L/h, the flow rate of oxygen is 2200-2300L/h, and the heat flow density of the jet gas flow is 1.15-1.20 MW/m2。
The high-emissivity coating prepared in step (3) cannot be smooth enough, so a glass coating D with a low catalytic coefficient needs to be further compounded on the surface of the coating, so that the catalytic coefficient of the surface of the coating is reduced, and the temperature resistance of the coating is improved. In the step (4), preferably, the low chemical catalytic coefficient glass coating is applied by spraying, and the carrier gas pressure is 0.2 to 0.5 MPa. Additionally, the high emissivity coating may be sintered at a temperature of 1200 to 1250 ℃ for a soak time of 0.5 to 1.5 hours, such as 0.5, 1, or 1.5 hours.
The present invention also provides in a sixth aspect a rigid insulating tile multilayer composite obtainable by the process of the fifth aspect of the invention.
In some more specific embodiments, the method according to the fifth aspect of the present invention may comprise the steps of:
(1) the multi-layer composite material matrix A of the alumina fiber rigid heat insulation tile is prepared by a freezing gel injection molding method.
Specifically, alumina cellucotton and acidic silica sol can be mixed according to the mass ratio of 1: 195-205, and placed in a dispersing barrel, and the concentration of the silica sol is controlled to be 8-10% by mass fraction. The alumina fiber cotton was dispersed using a paddle shear mixer. The stirring speed is controlled to be 2000 to 3000 r/min, and the stirring time is controlled to be 10 to 30 min. And transferring the ceramic slurry to a tool with a filter screen for filtering after stirring, and removing most of silica sol. The alumina fiber is trapped, and the filter cake forms the wet blank of the alumina fiber heat insulation tile. The used filter screen is a 50-mesh wire mesh. Depending on the density of the insulation tiles required by the design, the wet green may be pressed to a thickness by applying a pressure to achieve a desired density. Transferring the pressed wet blank into a freezing mold, locking the freezing mold by using a screw, placing the freezing mold into a freezing box, and pouring liquid nitrogen into the freezing box to enable the liquid nitrogen level to be 15-20 cm higher than the upper surface of the freezing mold. The frozen mold should have sufficient low temperature mechanical strength to prevent the alumina ceramic tile green body from expanding and cracking due to the volume expansion tendency generated by the crystallization of water during the freezing process. After waiting for 1 to 2 hours, completely volatilizing liquid nitrogen in the freezing box, disassembling the freezing mould, taking out the heat-insulating tile frozen blank, placing the frozen blank on a stainless steel clamp, controlling the height of a clamp positioning column according to the required density, and locking the positioning clamp by using a screw. And (3) rapidly drying the frozen blank in a microwave drying oven at 120 ℃, and sintering the frozen blank in a silicon carbide sintering sagger after the frozen blank is completely dried. The sintering temperature is 1250 ℃ to 1500 ℃, and the heat preservation time is 1 to 4 hours, so as to obtain the multilayer composite material fiber matrix of the alumina fiber rigid heat insulation tile. The sintering method can also be seen in, for example, CN201510632711.5, the manner of sintering disclosed by the present applicant. In addition, after the sintering is finished, the product obtained by sintering can be processed to the required profile size through a numerical control machine tool, and the matrix A is prepared.
(2) Preparation of dense ceramic layers using a brush coating process
The two sol continuous phases and at least one refractory ceramic powder dispersed phase can be mixed and ball milled to prepare a brushable ceramic sol suspension precursor, and if desired, the viscosity of the suspension can be adjusted using viscosity modifiers such as acrylamide to make it more suitable for brushing. After the suspension is brushed to the surface of the substrate A required to prepare the compact ceramic layer B, the substrate A is dried at room temperature and then is further cured in an oven at 200-400 ℃ to form the compact ceramic layer B.
(3) Preparation of high-emissivity thermal barrier coating C by using plasma sputtering method
A high emissivity coating composition is applied to the surface toughened alumina dense ceramic layer using a plasma sputtering process. The sputtering carrier gas uses oxygen/propane flame, the propane flow rate is controlled to 1150-1250L/h, the oxygen flow rate is controlled to 2200-2300L/h, and the heat flow density of the jet gas flow is 1.15-1.20 MW/m2. The thickness of the high emissivity oxide thermal barrier coating is controlled to be 100 to 200 microns, and the amount of glaze is 0.02 to 0.03g/cm2。
(4) Preparation of Low chemical catalytic coefficient glass coating D Using spray-Rapid sintering Process
The high-emissivity coating prepared in the step (3) cannot be smooth, so that a low-catalytic-coefficient glass coating D is further compounded on the surface of the coating, the catalytic coefficient of the surface of the coating is reduced, and the temperature resistance of the coating is improved. The amount of the glaze sprayed on the glass coating D with low catalytic coefficient canIs 0.04 to 0.06g/cm2. The carrier gas pressure is controlled to be 0.2 to 0.5MPa and the final thickness of the coating is 100 to 200 microns. The sintering temperature of the coating is 1200 to 1250 ℃, and the heat preservation time is 0.5 to 1.5 hours.
The invention will be further illustrated by means of the following examples, without however restricting its scope to these examples.
Example 1A preparation of alumina fiber rigid insulating tile multilayer composite matrix a using a cryogel casting process
Mixing alumina cellucotton and acid silica sol according to the mass ratio of 1:200, placing the mixture in a dispersing barrel, and controlling the concentration of the silica sol to be 9 mass percent. The alumina cellucotton was dispersed using a paddle shear mixer, the mixing speed was controlled to 2500 rpm, and the mixing time was controlled to 20 minutes. And after stirring, transferring the ceramic slurry to a tool with a filter screen for filtering, wherein the filter screen is a 50-mesh wire gauze, the alumina fiber impregnated with the acidic silica sol is intercepted, and a filter cake forms an alumina fiber heat-insulation tile wet blank. Depending on the design, a desired target density of 0.40g/cm3 for the rigid insulating tile multilayer composite is achieved by applying pressure to the wet green to a thickness of 35mm in order to achieve the desired density requirements. And transferring the pressed wet blank into a freezing mold, locking the freezing mold by using a screw, placing the freezing mold into a freezing box, and pouring liquid nitrogen into the freezing box to enable the liquid nitrogen level to be 15cm higher than the upper surface of the freezing mold. After waiting for 1.5 hours, completely volatilizing liquid nitrogen in the freezing box, disassembling the freezing mould, taking out the heat-insulating tile frozen blank, placing the frozen blank on a stainless steel clamp, limiting the height of a positioning column of the clamp to be 35cm according to the required density, and locking the positioning clamp by using a screw. And (3) drying the frozen blank in a microwave drying box at 120 ℃, after the frozen blank is completely dried, putting the frozen blank in a silicon carbide sintering sagger to sinter in a muffle furnace, wherein the sintering temperature is 1250 ℃, and the heat preservation time is 2.5 hours, so as to obtain the multilayer composite material fiber matrix of the alumina fiber rigid heat insulation tile. After the sintering was completed, the sintered product was processed to a desired profile size (length 300 mm. times. width 300 mm. times. thickness 30mm), thereby producing the substrate A, and the compressive strength of the produced substrate A was tested, and the results are shown in Table 1 below.
Examples 2A to 5A
Examples 2 to 5 were carried out in the same manner as in example 1 except for the contents shown in table 1 below.
Example 6A
Examples 2 to 5 were carried out in substantially the same manner as in the examples except that, after filtration, the wet green mold was transferred to a pressure molding machine, a pressure of 2.5MPa was applied to obtain a wet green ceramic fiber heat insulating tile, the wet green was dried in a microwave oven at 120 c, after the freeze-dried green was completely dried, a dry green was obtained, and then the sintering and processing were carried out.
TABLE 1 preparation of matrix A
Note: the mass ratio is the mass ratio of the alumina fiber and the acidic silica sol.
Example 1B coating of dense ceramic layer B
Preparing a compact ceramic layer composition which comprises 1 part of 25 mass percent alkaline silica sol, 0.7 part of 40 mass percent alumina sol and 0.3 part of 1 micron aluminum nitride powder, and adjusting the viscosity by using acrylamide to prepare a ceramic sol suspension precursor. After this suspension precursor was brushed on the surface of the substrate a obtained in example 1, where the dense ceramic layer B was to be prepared (coating thickness 4mm), it was dried at room temperature and then further cured in an oven at 300 ℃ to form a dense ceramic layer B, and the density of the coating B was measured, and the results are shown in table 2 below.
Example 2B
Example 2B was carried out in substantially the same manner as example 1B, except that a zirconia sol having a mass fraction of 30% was used instead of the alumina sol.
Example 3B
Example 3B was carried out in substantially the same manner as example 2B, except that quartz glass powder was used instead of the aluminum nitride powder.
Example 4B
Example 4B was performed in substantially the same manner as example 1B, except that yttrium oxide was used instead of the aluminum nitride powder.
Example 5B
Example 5B was carried out in substantially the same manner as example 1B, except that the base 6A was used instead of the base 1A.
TABLE 2 formulation of ceramic layer B
EXAMPLE 1C coating of high emissivity coating
A high emissivity coating composition consisting of 1 part by weight of yttria-stabilized zirconia powder, 2 parts by weight of nickel oxide powder and 3 parts by weight of quartz glass powder was applied to the coating B coated in example 2 using a plasma sputtering method. The sputtering carrier gas uses oxygen/propane flame, the propane flow rate is controlled to 1150-1250L/h, the oxygen flow rate is controlled to 2200-2300L/h, and the heat flow density of the jet gas flow is 1.15-1.20 MW/m2. The thickness of the high emissivity oxide thermal barrier coating is controlled to be 100 to 200 microns. Then, the temperature resistance was measured, and the results are shown in the following Table 3.
Examples 2C to 4C
Examples 2C to 4C were carried out in the same manner as example 1C except for the contents shown in table 3 below.
Table 3 preparation of thermal barrier coating C
Example lD coating of Low chemical catalytic coefficient glass coating D
Prepared in the composition of 1 part by weightCuring the low-catalytic-coefficient glass coating composition of a glass sintering continuous phase, 0.5 weight part of a molybdenum disilicide high-emissivity phase and 0.5 weight part of a high-temperature low-chemical-catalytic-coefficient dispersion phase, and forming a low-chemical-catalytic-coefficient glass coating D by a spraying-sintering method, wherein the amount of spraying glaze can be 0.05g/cm2. The carrier gas pressure was controlled at 0.4MPa and the final coating thickness was 150 microns. The sintering temperature of the coating is 1220, and the heat preservation time is 1.5 hours. And the emissivity was measured, the results of which are shown in table 4 below.
Examples 2D, 3D, 5D to 8D
The same procedure as in example 1 was conducted, except that the contents shown in Table 4 below were used.
Example 4D
Example 4D is conducted in substantially the same manner as example l D, except that the composition of the low catalytic coefficient glass coating composition: 77.5 parts by weight of a reaction-cured glass-sintered continuous phase, 20 parts by weight of a molybdenum disilicide high emissivity phase and 2.5 parts by weight of silicon tetraboride.
TABLE 4 preparation of Low chemical catalytic coefficient glass coating D
Claims (19)
1. The utility model provides a rigidity heat insulating tile multilayer combined material which characterized in that, rigidity heat insulating tile multilayer combined material includes by inside to outside in proper order: (1) a porous alumina fiber matrix; (2) surface toughening alumina compact ceramic layer; (3) a high emissivity oxide thermal barrier coating; and (4) a low chemical catalytic coefficient glass coating;
the matrix is prepared from alumina fiber and acidic silica sol; the surface toughened alumina compact ceramic layer is coated by the surface toughened alumina compact ceramic layer composition; the high emissivity oxide thermal barrier coating is coated with a high emissivity coating composition; and/or the low chemical catalytic coefficient glass coating is made of a low chemical catalytic coefficient glass coating composition;
the surface toughened alumina dense ceramic layer composition is one of the following compositions: (1)1 part by mass of 25% alkaline silica sol, 0.7 to 0.8 part by mass of 40% alumina sol and 0.2 to 0.3 part by mass of 1 to 2 micron aluminum nitride powder; (2)1 part by mass of 25% alkaline silica sol, 0.7 to 0.8 part by mass of 30% to 35% zirconia sol and 0.2 to 0.3 part by mass of 1 to 2 micron aluminum nitride powder; (3)1 part by mass of 25% alkaline silica sol, 0.7 to 0.8 part by mass of 30% to 35% zirconia sol, and 0.2 to 0.3 part by mass of quartz glass powder with a particle size of 1 to 2 μm;
the high emissivity coating composition comprises at least one selected from the group consisting of yttria-stabilized zirconia powder, quartz glass powder, barium zirconate powder, nickel oxide powder, alumina powder, zirconia powder and borosilicate glass powder;
the low chemical catalytic coefficient glass coating composition includes a continuous phase, a high emissivity phase, and a high temperature low chemical catalytic coefficient dispersed phase.
2. The rigid insulating tile multilayer composite as set forth in claim 1,
the mass ratio of the alumina fiber to the acidic silica sol is 1:195 to 205, and the concentration of the acidic silica sol is 8 to 10 mass%.
3. The rigid insulating tile multilayer composite as set forth in claim 1,
the thickness of the surface toughened alumina compact ceramic layer is 3mm to 5 mm.
4. The rigid insulating tile multilayer composite as set forth in claim 1,
the high emissivity oxide thermal barrier coating has a thickness of 100 microns to 200 microns.
5. The rigid insulating tile multilayer composite as set forth in claim 1,
the low chemical catalytic coefficient glass coating has a thickness of 100 to 200 microns.
6. The rigid insulating tile multilayer composite as set forth in claim 1,
the high emissivity coating composition comprises: (1) yttria stabilized zirconia powder; (2) nickel oxide powder; and (3) quartz glass frit.
7. The rigid insulating tile multilayer composite as set forth in claim 1,
the high emissivity coating composition is composed of: (1) yttria stabilized zirconia powder; (2) nickel oxide powder; and (3) quartz glass frit.
8. The rigid insulating tile multilayer composite of claim 1, 6 or 7,
the particle size of the yttria-stabilized zirconia powder is 1-3 microns; the particle size of the nickel oxide powder is 1-3 microns; and/or the particle size of the quartz glass frit is 1 to 3 microns.
9. The rigid insulating tile multilayer composite as set forth in claim 6 or 7,
the high emissivity coating composition comprises 1 part by weight of yttria-stabilized zirconia powder; the nickel oxide powder in the high-emissivity coating composition is 1.8 to 2.2 parts by weight; and/or the quartz glass powder in the high emissivity coating composition is in a weight part of 2.8 to 3.2 parts.
10. The rigid insulating tile multilayer composite as set forth in claim 1,
the low chemical catalytic coefficient glass coating composition consists of a continuous phase, a high emissivity phase and a high temperature low chemical catalytic coefficient dispersoid phase.
11. The rigid insulating tile multilayer composite as set forth in claim 1 or 10,
the continuous phase is a reaction cured glass sintering continuous phase; the high emissivity phase is a molybdenum disilicide high emissivity phase; and/or the high temperature low chemical catalytic coefficient dispersed phase is at least one selected from the group consisting of tantalum disilicide, mercury silicide, and tungsten silicide.
12. The rigid insulating tile multilayer composite as set forth in claim 1 or 10,
the continuous phase is 1 part by weight of reaction cured glass sintering continuous phase; the high emissivity phase is molybdenum disilicide high emissivity phase of 0.4 to 0.6 weight part; and/or the high-temperature low-chemical-catalytic-coefficient dispersed phase is 0.4 to 0.6 part by weight.
13. The rigid insulating tile multilayer composite as set forth in claim 1 or 10,
the high-temperature low-chemical catalytic coefficient dispersed phase at least comprises tungsten silicide and/or mercury silicide.
14. A method of manufacturing a rigid insulating tile multilayer composite as claimed in any of claims 1 to 13, said method comprising the steps of:
(1) mixing alumina fiber and acidic silica sol, stirring uniformly, filtering, preparing a wet blank from a filter cake in a wet blank mold, freezing the wet blank in a freezing mold to prepare a frozen blank, drying the frozen blank, and sintering to prepare the porous alumina fiber matrix;
(2) applying the surface toughened alumina dense ceramic layer composition onto the surface of the porous alumina fiber matrix, drying and curing to form the surface toughened alumina dense ceramic layer;
(3) forming the high emissivity oxide thermal barrier coating by using a plasma sputtering process to deposit the high emissivity oxide thermal barrier coating on the surface toughened alumina dense ceramic layer; and
(4) and coating the low chemical catalytic coefficient glass coating composition on the high-emissivity oxide thermal barrier coating and sintering to form the low chemical catalytic coefficient glass coating.
15. The method of claim 14, wherein in step (1):
dispersing alumina fiber by using a blade type shearing stirrer, wherein the stirring speed is 2000-3000 r/min, and the stirring time is 10-30 min;
the filtration is carried out by using a 50-mesh filter screen;
the freezing is performed by using liquid nitrogen, the liquid nitrogen submerges the surface of the freezing mould for 15-20 cm during freezing, and the freezing time is 1-2 hours;
drying the frozen blank at 1200 ℃; and/or
The sintering temperature of the sintering is 1250-1500 ℃, and the heat preservation time of the sintering is 1-4 hours.
16. The method of claim 15, wherein in step (2):
the drying is carried out at room temperature and the curing is carried out at 200 ℃ to 400 ℃.
17. The method according to claim 14, wherein in the step (3), the process parameters of the plasma sputtering method are as follows: the sputtering carrier gas is oxygen/propane flame, the flow rate of propane is 1150-1250L/h, the flow rate of oxygen is 2200-2300L/h, and the heat flow density of the jet gas flow is 1.15-1.20 MW/m2。
18. The method according to claim 14, wherein in the step (4), the low chemical catalytic coefficient glass coating is applied by spraying, and the carrier gas pressure is 0.2 to 0.5 MPa; and/or the temperature for sintering the glass coating with the low chemical catalytic coefficient is 1200-1250 ℃, and the heat preservation time for sintering is 0.5-1.5 hours.
19. Use of a rigid insulating tile multilayer composite according to any of claims 1 to 13 in thermal protection materials for aircraft exterior surfaces, ultra high temperature chemical reactor thermal protection materials, nuclear reactor ultra high temperature thermal protection materials, ultra high temperature kiln insulation liners or metal melt filters.
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| CN107434421B (en) * | 2017-08-10 | 2019-12-10 | 航天特种材料及工艺技术研究所 | antenna window component with wave-transmitting, heat-insulating and bearing performances and preparation method thereof |
| CN107892569B (en) * | 2017-11-21 | 2020-08-28 | 淄博双马新材料科技股份有限公司 | Composite submerged nozzle lining material for continuous casting |
| CN108929049A (en) * | 2018-08-21 | 2018-12-04 | 徐培培 | A method of Basalt fiber high-temperature resisting performance is promoted by surface modification |
| CN109320273A (en) * | 2018-09-13 | 2019-02-12 | 南京鑫达晶体材料科技有限公司 | A kind of improved alumina fibre plate and preparation method thereof |
| CN109626994B (en) * | 2018-11-23 | 2021-12-28 | 昆明理工大学 | Thermal barrier coating material with low infrared transmittance and preparation method thereof |
| CN111217620B (en) * | 2018-11-26 | 2022-08-09 | 航天特种材料及工艺技术研究所 | High-temperature-resistant coating on surface of nano porous heat-insulating material substrate, preparation method and substrate |
| CN111099909B (en) * | 2019-12-30 | 2020-12-29 | 浙江大学 | High-performance ceramic with surface modified polycrystalline mullite fiber compounded with rare earth lanthanum zirconate and preparation method thereof |
| CN112250450B (en) * | 2020-09-15 | 2022-05-03 | 航天特种材料及工艺技术研究所 | Preparation method of heat insulation tile blank capable of resisting high temperature of 2000 DEG C |
| CN113979769B (en) * | 2021-11-29 | 2022-09-23 | 航天特种材料及工艺技术研究所 | Rigid ultrathin heat insulation material and preparation method thereof |
| CN114540740B (en) * | 2022-03-14 | 2023-07-11 | 西安热工研究院有限公司 | Borosilicate glass modified yttrium oxide stabilized zirconia thermal barrier coating and preparation method thereof |
| CN114622153B (en) * | 2022-03-14 | 2023-07-11 | 西安热工研究院有限公司 | Glass modified cerium oxide stabilized zirconia thermal barrier coating and preparation method thereof |
| CN116161952B (en) * | 2023-04-26 | 2023-08-18 | 淄博职业学院 | High fracture toughness composite ceramic material and preparation method thereof |
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| CN108455978A (en) | 2018-08-28 |
| CN108467260A (en) | 2018-08-31 |
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| CN108383391B (en) | 2021-04-30 |
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