CN117325547A - High-strength high-temperature-resistant heat insulation material and preparation method thereof - Google Patents
High-strength high-temperature-resistant heat insulation material and preparation method thereof Download PDFInfo
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- CN117325547A CN117325547A CN202311392973.XA CN202311392973A CN117325547A CN 117325547 A CN117325547 A CN 117325547A CN 202311392973 A CN202311392973 A CN 202311392973A CN 117325547 A CN117325547 A CN 117325547A
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- 239000012774 insulation material Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000835 fiber Substances 0.000 claims abstract description 260
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 206
- 239000010452 phosphate Substances 0.000 claims abstract description 206
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 205
- 239000000853 adhesive Substances 0.000 claims abstract description 147
- 230000001070 adhesive effect Effects 0.000 claims abstract description 147
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 98
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 93
- 229910026551 ZrC Inorganic materials 0.000 claims abstract description 54
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 52
- 239000007787 solid Substances 0.000 claims abstract description 52
- 239000000945 filler Substances 0.000 claims abstract description 46
- 239000011248 coating agent Substances 0.000 claims abstract description 40
- 238000000576 coating method Methods 0.000 claims abstract description 40
- 238000000498 ball milling Methods 0.000 claims abstract description 37
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910000423 chromium oxide Inorganic materials 0.000 claims abstract description 33
- 238000003756 stirring Methods 0.000 claims abstract description 27
- 238000002156 mixing Methods 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 238000003825 pressing Methods 0.000 claims abstract description 9
- 239000002002 slurry Substances 0.000 claims description 51
- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical compound [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 19
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 18
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 claims description 17
- 229910052596 spinel Inorganic materials 0.000 claims description 17
- 239000011029 spinel Substances 0.000 claims description 17
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 claims description 12
- 229910000166 zirconium phosphate Inorganic materials 0.000 claims description 12
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 claims description 12
- 239000000463 material Substances 0.000 abstract description 13
- 239000013078 crystal Substances 0.000 abstract description 10
- 238000006388 chemical passivation reaction Methods 0.000 abstract description 6
- 238000007711 solidification Methods 0.000 abstract 1
- 230000008023 solidification Effects 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 18
- 239000002245 particle Substances 0.000 description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 15
- 239000010439 graphite Substances 0.000 description 15
- 229910002804 graphite Inorganic materials 0.000 description 15
- 238000004132 cross linking Methods 0.000 description 12
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 10
- 230000004048 modification Effects 0.000 description 9
- 238000012986 modification Methods 0.000 description 9
- 239000002694 phosphate binding agent Substances 0.000 description 9
- 239000011810 insulating material Substances 0.000 description 8
- 238000013329 compounding Methods 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000005496 eutectics Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical class [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 239000012790 adhesive layer Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000007723 die pressing method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229940001007 aluminium phosphate Drugs 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000011499 joint compound Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 235000014380 magnesium carbonate Nutrition 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012783 reinforcing fiber Substances 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
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- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
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- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
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- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
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- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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- B64G—COSMONAUTICS; VEHICLES OR EQUIPMENT THEREFOR
- B64G1/00—Cosmonautic vehicles
- B64G1/22—Parts of, or equipment specially adapted for fitting in or to, cosmonautic vehicles
- B64G1/52—Protection, safety or emergency devices; Survival aids
- B64G1/58—Thermal protection, e.g. heat shields
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- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- B32B2307/00—Properties of the layers or laminate
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- B32B2307/306—Resistant to heat
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
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- C04B2235/52—Constituents or additives characterised by their shapes
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Abstract
The invention relates to a high-strength high-temperature-resistant heat insulation material and a preparation method thereof. The method comprises the following steps: uniformly dispersing zirconia fibers and zirconium carbide fibers by using water, and manufacturing a fiber wet sheet by using the water; mixing and ball milling solid phosphate, magnesia and chromium oxide to obtain a filler, adding a phosphate solution, mixing and stirring to obtain a high-temperature-resistant phosphate adhesive; coating a high-temperature-resistant phosphate adhesive on the surface of the reflecting screen, and curing to obtain a modified reflecting screen; a plurality of modified reflecting screens and a plurality of fiber wet sheets are alternately arranged, and the high-strength high-temperature-resistant heat insulation material is prepared through mould pressing and solidification; in the alternate arrangement, a fiber wet sheet is arranged between every two modified reflecting screens, and the surface of the fiber wet sheet is coated with a high-temperature-resistant phosphate adhesive. The invention realizes the control of the high-temperature crystal form of the phosphate, and simultaneously uses the phosphate adhesive to carry out oxidation inhibition treatment on the reflecting screen, thereby improving the interface stability of the multilayer material and achieving the purpose of durable application of the material under the ultra-high temperature condition.
Description
Technical Field
The invention belongs to the technical field of heat insulation materials, and particularly relates to a high-strength high-temperature-resistant heat insulation material and a preparation method thereof.
Background
As various aerospace vehicles develop towards high Mach numbers and long endurance, the power systems of the aircrafts face increasingly severe thermal environments; to prevent the power system high temperature heat flow from affecting the flight stability of the aircraft, it must be thermally protected. The high-temperature-resistant multilayer heat insulation material has excellent high-temperature radiation resistance, has great advantages in a heat protection structure of a power system, and has been widely applied to various aerospace vehicles.
The prior multi-layer heat insulating material uses a high-temperature-resistant zirconia fiber heat insulating material as a spacer layer and uses phosphate as a binder, so that the problem of huge high Wen Weixing capability is solved, and particularly the durability application stability of the material in an ultra-high temperature environment is poor. The main reasons are as follows: firstly, common high-temperature adhesives such as aluminum phosphate, zirconium phosphate, aluminum dihydrogen phosphate and the like are easy to expand when heated at high temperature, so that strength failure and the like occur to the high-temperature long-term application of the materials, and the structural stability of the materials is difficult to maintain; and secondly, the used reflecting screen is rapidly oxidized in a high-temperature environment, so that the interface structure is suddenly changed, and the material structure is invalid.
Therefore, the problems of insufficient temperature resistance and strength to the high Wen Jiaogao temperature of the phosphate must be improved, and in addition, the oxidation inhibition screen technology must be adopted to prevent, so as to realize the durable application of the high temperature resistant multilayer material under the ultra-high temperature condition and avoid structural failure.
In summary, it is highly necessary to provide a high-strength high-temperature-resistant heat insulating material and a preparation method thereof.
Disclosure of Invention
In order to solve one or more technical problems in the prior art, the invention provides a high-strength high-temperature-resistant heat insulation material and a preparation method thereof. The invention prepares the high-strength and maintainable ultrahigh-temperature heat-insulating material by taking the high-temperature-resistant phosphate as the adhesive, and the adopted adhesive is a multi-component compound high-performance high-temperature-resistant adhesive taking the phosphate as the main component, so that the prepared heat-insulating material has the characteristics of ultrahigh temperature resistance and high strength, and can realize the durable application of the heat-insulating material under the ultrahigh temperature condition.
The invention provides a preparation method of a high-strength high-temperature-resistant heat insulation material in a first aspect, which comprises the following steps:
(1) Uniformly dispersing zirconia fibers and zirconium carbide fibers by using water to obtain fiber slurry, and manufacturing a fiber wet sheet from the fiber slurry;
(2) Mixing solid phosphate, magnesia and chromium oxide, performing ball milling to obtain a filler, and then mixing and stirring a phosphate solution and the filler to obtain a high-temperature-resistant phosphate adhesive;
(3) Coating the high-temperature-resistant phosphate adhesive on the surface of the reflecting screen, and curing to obtain a modified reflecting screen;
(4) Alternately arranging a plurality of modified reflecting screens and a plurality of fiber wet sheets, and then performing mould pressing and curing to obtain a high-strength high-temperature-resistant heat insulation material; in the alternate arrangement, a wet fiber sheet is arranged between every two modified reflecting screens, and the surface of the wet fiber sheet is coated with the high-temperature-resistant phosphate adhesive.
Preferably, the diameter of the zirconia fiber is 3-10 mu m, and the diameter of the zirconium carbide fiber is 2-5 mu m; the fiber slurry contains 0.2 to 3 percent of the sum of the mass percentages of zirconia fiber and zirconium carbide fiber; and/or the mass ratio of the zirconia fiber to the zirconium carbide fiber is (4-10): 1.
preferably, the thickness of the wet fiber sheet is 0.5 to 3mm.
Preferably, the mass ratio of the solid phosphate to the magnesia to the chromium oxide is (6-13): (2-7): (1-3); the solid phosphate is solid aluminum phosphate and/or solid zirconium phosphate; the grain diameter of the magnesia is 10-200 mu m; and/or the ball milling time is 6-12 h.
Preferably, the stirring is stirring at room temperature for 3-6 hours.
Preferably, the phosphate solution has a solids content of 20 to 60wt%; the mass ratio of the phosphate solution to the filler is (2-9): 1, a step of; and/or the phosphate solution is one or more of aluminum dihydrogen phosphate solution, aluminum phosphate solution and zirconium phosphate solution.
Preferably, the thickness of the high temperature resistant phosphate adhesive coated on the surface of the reflecting screen is 30-90 mu m; and/or the surface of the fiber wet sheet is coated with the high-temperature-resistant phosphate adhesive, wherein the thickness of the high-temperature-resistant phosphate adhesive is 30-90 mu m.
Preferably, in step (3) and/or step (4), the curing is: curing for 4-8 h at 80-100 ℃ and then curing for 10-15 h at 120-180 ℃.
Preferably, in step (2): the filler also comprises aluminum magnesium spinel, and preferably, in the filler, the mass ratio of the solid phosphate to the magnesia to the chromium oxide to the aluminum magnesium spinel is (6-13): (2-7): (1-3): (1-5); and/or after stirring, adding zirconium carbide whisker and aluminum nitride fiber, dispersing uniformly, and then adding magnesia powder, dispersing uniformly to obtain the high-temperature-resistant phosphate adhesive.
The present invention provides in a second aspect a high strength, high temperature resistant insulation material made by the method of the invention described in the first aspect.
Compared with the prior art, the invention has at least the following beneficial effects:
the high-temperature-resistant phosphate adhesive is prepared by performing interfacial modification on ball-milled magnesia, phosphate and chromium oxide to control a high-temperature crystal form of the phosphate and improve the temperature resistance of the phosphate adhesive, and the high-performance high-temperature-resistant adhesive is prepared by multi-component compounding with the phosphate as a main component; meanwhile, the reflecting screen is coated in advance by the high-temperature-resistant phosphate adhesive and cured at a high temperature, so that oxidation inhibition treatment of the reflecting screen is realized, interface stability of the multilayer material is improved, finally, the preparation of the high-strength ultrahigh-temperature-resistant multilayer heat insulation material is realized, the purpose of durable application of the material is achieved, and the failure of the structure of the heat insulation material under the ultrahigh-temperature condition can be effectively avoided.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below in connection with the embodiments of the present invention. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a preparation method of a high-strength high-temperature-resistant heat insulation material in a first aspect, which comprises the following steps:
(1) Uniformly dispersing zirconia fibers and zirconium carbide fibers by using water to obtain fiber slurry, and manufacturing a fiber wet sheet from the fiber slurry; in the invention, specifically, a certain amount of zirconia fiber and zirconium carbide fiber are weighed and put in water, and after being uniformly dispersed by a pulping machine, fiber slurry is obtained, and the fiber slurry is manufactured into fiber wet sheets by a sheet making machine, for example, the fiber slurry is put in a charging basket of the sheet making machine, and after being manually or automatically homogenized, the sheet making machine is started, and the fiber wet sheets with certain thickness are manufactured by the sheet making machine;
(2) Mixing and ball milling solid phosphate, magnesia and chromium oxide (chromium oxide) to obtain a filler (also called as high-temperature filler), and then mixing and stirring a phosphate solution with the filler to obtain a high-temperature-resistant phosphate adhesive; the stirring speed is not particularly limited, and can be 200-800 r/min;
(3) Coating the high-temperature-resistant phosphate adhesive on the surface of the reflecting screen, and curing to obtain a modified reflecting screen; in the invention, at least the surface of the reflecting screen, which is contacted with the wet fiber sheet, is coated with the high-temperature-resistant phosphate adhesive obtained in the step (2); the invention has no special requirement on the reflecting screen, the reflecting screen can be one or more of graphite paper, graphite cloth and carbon fiber cloth, and the thickness of the reflecting screen is 0.025-0.1 mm;
(4) Alternately arranging a plurality of modified reflecting screens and a plurality of fiber wet sheets, and then performing mould pressing and curing to obtain a high-strength high-temperature-resistant heat insulation material; in the alternative arrangement, a fiber wet sheet is arranged between every two modified reflecting screens, and the surface of the fiber wet sheet is coated with the high-temperature-resistant phosphate adhesive; in the invention, the surface of the wet fiber sheet contacted with the modified reflecting screen is coated with the high-temperature-resistant phosphate adhesive obtained in the step (2); in the invention, for example, a compaction tool can be used for carrying out the mould pressing, the parameter for carrying out the mould pressing is not particularly required, and the mould pressing is carried out by adopting the existing conventional mould pressing parameter; for example, the pressure of the die pressing is 0.5-3 MPa, and the die pressing time is 10-90 min; the number of the modified reflecting screens and the fiber wet sheets is not particularly required, and the modified reflecting screens and the fiber wet sheets are optimally designed according to actual application conditions (such as the total thickness requirement of a high-strength high-temperature-resistant heat insulation material in actual application); preferably, the thickness of the high-strength high-temperature-resistant heat insulation material is 5-60 mm; the high-strength high-temperature-resistant heat insulation material prepared by the invention can realize durable application under the ultra-high temperature condition, so that the high-strength high-temperature-resistant heat insulation material is also called as a high-strength ultra-high-temperature-resistant multilayer heat insulation material; in the present invention, the ultra-high temperature condition refers to a high temperature condition of 1500 ℃ or higher.
Firstly, preparing a fiber wet sheet by compounding zirconium carbide fibers and zirconium oxide fibers with excellent high-temperature stability, then preparing a high-strength and high-temperature-resistant phosphate adhesive, firstly mixing solid phosphate, magnesia and chromium oxide, and ball-milling in a ball-milling tank to finish modification; magnesia may be used to boost the high Wen Weixing capacity of phosphate binders; meanwhile, the mixed matrix of phosphate and chromium oxide realizes microscopic-scale blending modification on magnesia through ball milling, realizes control on a phosphate high-temperature crystal form, avoids high-temperature failure of a phosphate adhesive, then stirs a phosphate solution and a high-temperature filler to form the high-temperature-resistant phosphate adhesive, coats the surface of a reflecting screen with the high-temperature-resistant phosphate adhesive, carries out high-temperature curing, carries out oxidation inhibition modification, and finally alternately arranges a plurality of modified reflecting screens and fiber wet sheets, coats the high-temperature-resistant phosphate adhesive on the interface of the fiber wet sheets, and prepares the high-strength ultrahigh-temperature-resistant multilayer heat insulation material through mould pressing and curing.
The high-temperature-resistant phosphate adhesive is prepared by performing interfacial modification on ball-milled magnesia, phosphate and chromium oxide to realize control on a high-temperature crystal form of the phosphate and improve the temperature resistance of the phosphate adhesive, and the high-performance high-temperature-resistant adhesive is prepared by multi-component compounding with the phosphate as a main component, and in addition, the solid phosphate is added into the filler, so that the content of the phosphate of the high-temperature-resistant crystal form can be increased, the dispersibility between a phosphate solution and other filler components can be improved, the pre-crosslinking can be promoted, the performance of the phosphate adhesive can be improved, and the composition of the phosphate adhesive can be optimized; meanwhile, the reflecting screen is coated in advance by the high-temperature-resistant phosphate adhesive and cured at a high temperature, so that oxidation inhibition treatment of the reflecting screen is realized, interface stability of the multilayer material is improved, finally, the preparation of the high-strength ultrahigh-temperature-resistant multilayer heat insulation material is realized, the purpose of durable application of the material is achieved, and the failure of the structure of the heat insulation material under the ultrahigh-temperature condition can be effectively avoided.
According to some preferred embodiments, the zirconia fibers have a diameter (average diameter) of 3 to 10 μm and the zirconia fibers have a diameter (average diameter) of 2 to 5 μm; in the present invention, it is preferable that the diameter of the zirconia fiber is 3 to 10 μm, the diameter of the zirconia fiber is 2 to 5 μm, and more preferable that the diameter of the zirconia fiber is larger than the diameter of the zirconia fiber, the fiber size difference degree compounding can improve the strength of the wet fiber sheet, the subsequent operation is convenient, and the diameter of the zirconia fiber is preferably finer because the zirconia fiber has good temperature resistance but high thermal conductivity; the fiber slurry contains 0.2-3 percent (for example, 0.2 percent, 0.5 percent, 0.8 percent, 1 percent, 1.2 percent, 1.5 percent, 1.8 percent, 2 percent, 2.2 percent, 2.5 percent, 2.8 percent or 3 percent) of the sum of the mass percentages (mass fractions) of the zirconia fiber and the zirconia fiber, and the mass fractions can ensure the effective dispersion and lap joint of the fiber and effectively avoid the condition of uneven dispersion or low lap joint compound degree; and/or the mass ratio of the zirconia fiber to the zirconium carbide fiber is (4-10): 1 (e.g., 4:1, 5:1, 6:1, 7:1, 8:1, 9:1, or 10:1).
According to some preferred embodiments, the wet sheet of fibers has a thickness of 0.5 to 3mm; in the present invention, in order to ensure uniformity of the heat insulating material and stable coating of the high temperature resistant phosphate adhesive while ensuring excellent high temperature infrared radiation inhibiting performance of the multi-layered material, it is preferable that the thickness of the fibrous wet sheet is 0.5 to 3mm and the thickness of the reflecting screen is 0.025 to 0.1mm.
According to some preferred embodiments, the mass ratio of the solid phosphate, the magnesia and the chromia is (6-13): (2-7): (1-3); the invention obtains the preferable proportion through a large number of creative experiments, and discovers that the proportion can realize the high-temperature resistant modification design of a phosphate adhesive system by realizing the effective control of crystal forms, thereby ensuring that the phosphate adhesive with ultrahigh temperature resistance and high strength is obtained; in the present invention, if the ratio of each component is not within this preferable range, the control of the crystal form may be disabled, and the unsuitable mass ratio may result in the composition of the material being uneven and the crystal structure being unstable, thereby reducing the overall performance of the phosphate adhesive under high temperature conditions.
According to some preferred embodiments, the solid phosphate is an aluminium-based phosphate and/or a zirconium-based phosphate, preferably the solid phosphate is a solid aluminium phosphate and/or a solid zirconium phosphate; the particle size (average particle size) of the magnesia is 10-200 μm (for example, 10, 20, 30, 40, 50, 60, 70, 80, 90, 100, 110, 120, 130, 140, 150, 160, 170, 180, 190 or 200 μm), and in the invention, it is preferable that the particle size of the magnesia is 10-200 μm, if the particle size of the magnesia is too small, agglomeration is easy to occur, the high temperature stability of the prepared phosphate binder is poor, and if the particle size of the magnesia is too large, the ball milling process is difficult to form a modified eutectic system with phosphate and chromium oxide, and the improvement of the high temperature stability of the phosphate binder is also unfavorable; and/or the ball milling time is 6 to 12 hours (e.g., 6, 7, 8, 9, 10, 11, or 12 hours).
According to some preferred embodiments, the stirring is at room temperature for 3-6 hours (e.g., 3, 4, 5, or 6 hours); in the present invention, the room temperature may be, for example, 20 to 30 ℃.
According to some preferred embodiments, the phosphate solution has a solids content of 20-60 wt% (e.g. 20wt%, 25wt%, 30wt%, 35wt%, 40wt%, 45wt%, 50wt%, 55wt% or 60 wt%), i.e. the phosphate solution contains 20-60 wt% of phosphate; and/or the mass ratio of the phosphate solution to the filler is (2-9): 1 (e.g., 2:1, 3:1, 4:1, 5:1, 6:1, 7:1, 8:1, or 9:1).
In the present invention, it is preferable that the mass ratio of the phosphate solution to the filler is (2 to 9): 1, the phosphate adhesive with ultrahigh temperature resistance and high strength is ensured to be obtained, and in the preferable proportioning range, the phosphate adhesive can be prepared according to different viscosity requirements of a phosphate adhesive system, so that the high temperature resistant adhesive with different viscosities is obtained, and the actual application situation can be better adapted; in the present invention, it is preferable that the solid content of the phosphate solution is controlled to 20 to 60wt%, and if the solid content in the phosphate solution is too large, it results in a small amount of high temperature resistant component in the phosphate adhesive according to the present invention, and if the high temperature resistant component is too much, it results in a limited increase in the high temperature strength of the phosphate adhesive.
According to some preferred embodiments, the phosphate solution is one or more of an aluminum dihydrogen phosphate solution, an aluminum phosphate solution, a zirconium phosphate solution; in the present invention, the phosphate is an aluminum-based phosphate and/or a zirconium-based phosphate; in the present invention, the phosphate solution refers to an aqueous phosphate solution.
According to some preferred embodiments, the thickness of the refractory phosphate binder applied to the surface of the reflective screen is 30-90 μm (e.g. 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85 or 90 μm), and in the present invention, it is preferred that the thickness of the refractory phosphate binder applied to the surface of the reflective screen is 30-90 μm, and it has been found that if the adhesive layer on the reflective screen is too thin, oxidation inhibition effect is poor, and if the adhesive layer is too thick, the reflective screen is easily fragile; and/or the surface of the fibrous wet sheet is coated with the high temperature resistant phosphate binder to a thickness of 30 to 90 μm (e.g., 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85, or 90 μm).
According to some preferred embodiments, in step (3) and/or step (4), the curing is: the gradient temperature-rising curing is preferably performed in the present invention by curing at 80 to 100 c (e.g., 80 c, 90 c or 100 c) for 4 to 8 hours (e.g., 4, 5, 6, 7 or 8 hours) and then at 120 to 180 c (e.g., 120 c, 130 c, 140 c, 150 c, 160 c, 170 c or 180 c) for 10 to 15 hours (e.g., 10, 11, 12, 13, 14 or 15 hours), so that bubbling of the phosphate binder and the like can be effectively prevented, thereby advantageously ensuring the overall performance of the phosphate binder and the high-strength high-temperature-resistant heat insulating material.
According to some preferred embodiments, in step (2): the filler also comprises aluminum magnesium spinel, and preferably, in the filler, the mass ratio of the solid phosphate to the magnesia to the chromium oxide to the aluminum magnesium spinel is (6-13): (2-7): (1-3): (1-5), the invention obtains the preferable proportion through a large number of creative experiments, and the invention discovers that the proportion can effectively realize the high-temperature resistant modification design of a phosphate adhesive system by realizing the effective control of crystal forms; and/or after stirring, adding zirconium carbide whisker and aluminum nitride fiber, dispersing uniformly, and then adding magnesia powder, dispersing uniformly to obtain the high-temperature-resistant phosphate adhesive.
The high-temperature-resistant phosphate adhesive is preferably adopted, magnesia and aluminum magnesium spinel are taken as ultra-high temperature components, the mixed matrix of phosphate and chromium oxide realizes microscopic-scale blending modification on the magnesia and aluminum magnesium spinel through ball milling, the control on the high-temperature crystal form of the phosphate can be better realized, and the ball milling process can enable the magnesia and aluminum magnesium spinel, the phosphate and the chromium oxide to form a modified eutectic system, so that the high-temperature failure of high-temperature glue (phosphate adhesive) is avoided; avoid the failure of phosphate at high temperature and even at ultra-high temperature (above 1500 ℃); meanwhile, the high-temperature-resistant reinforcing fiber (aluminum nitride fiber) and the nano whisker (zirconium carbide whisker) are introduced to toughen a high-temperature glue system (a pre-crosslinking system), and the liquid phosphate adhesive (phosphate solution) is used for densifying the reinforcing body, so that the reinforcing body can be more tightly combined with the main components, the high-temperature strength of the phosphate adhesive is obviously improved, and the high-temperature-resistant performance and the high-temperature strength of the prepared high-strength high-temperature-resistant heat insulation material are further improved.
According to the invention, a basic network structure is built in the adhesive by forming the pre-crosslinking system, and then the zirconium carbide whisker, the aluminum nitride fiber and the magnesium oxide powder are added, so that uniform dispersion of the compound components can be realized more easily, the components can be fully distributed in the whole phosphate adhesive, interaction among the components can be better ensured, and the toughening performance and high-temperature stability performance of the zirconium carbide whisker, the aluminum nitride fiber and the magnesium oxide powder can be utilized to the greatest extent, so that the overall performance of the phosphate adhesive can be obviously enhanced; in addition, the magnesium oxide powder is added into the pre-crosslinking system, the addition of the magnesium oxide powder is beneficial to improving the high-temperature stability of the phosphate adhesive, the thermal expansion performance of the phosphate adhesive can be better controlled, and the problem of fracture or damage caused by mismatch of thermal expansion can be more effectively avoided; the multi-component compound high-performance high-temperature-resistant adhesive taking phosphate as a main component is also obtained in the preferable technical scheme, has the characteristics of high temperature resistance, no expansion and high strength, and is beneficial to further improving the high temperature resistance and the high temperature strength of the prepared high-strength high-temperature-resistant heat insulation material.
According to some specific embodiments, step (2) is: mixing and ball milling solid phosphate, magnesia, chromium oxide (chromium oxide) and aluminum magnesium spinel to obtain a filler (also called as high-temperature filler), mixing and stirring a phosphate solution and the filler to obtain a pre-crosslinked system, adding zirconium carbide whiskers and aluminum nitride fibers into the pre-crosslinked system and uniformly dispersing, and adding magnesia powder and uniformly dispersing to obtain the high-temperature-resistant phosphate adhesive; in the present invention, for example, the stirring may be uniformly dispersed, and the rotation speed of the stirring is not particularly limited, and may be, for example, 200 to 800r/min.
The invention does not limit the sources of the raw materials specifically, and products which can be directly purchased in the market or synthesized by the existing method can be adopted.
According to some preferred embodiments, the particle size (average particle size) of the aluminum magnesium spinel is 20 to 500 μm (e.g., 20, 50, 80, 100, 150, 200, 250, 300, 350, 400, 450, or 500 μm); in the present invention, it is preferable that the particle size of the aluminum magnesium spinel is 20 to 500 μm, if the particle size of the aluminum magnesium spinel is too small, agglomeration is easy, resulting in poor high temperature stability of the prepared phosphate binder, and if the particle size of the aluminum magnesium spinel is too large, the ball milling process is difficult to form a modified eutectic system with phosphate and chromium oxide, which is also unfavorable for improving the high temperature stability of the phosphate binder.
According to some preferred embodiments, the zirconium carbide whiskers have an aspect ratio of (5 to 100): 1, a step of; in the present invention, the particle diameter of the zirconium carbide whisker is, for example, 10 to 100nm; and/or the length (average length) of the aluminum nitride fiber is 3 to 8 μm; in the present invention, the diameter of the aluminum nitride fiber may be, for example, 100 to 1000nm; in the present invention, it is preferable that the aspect ratio of the zirconium carbide whisker is (5 to 100): 1, the length of the aluminum nitride fiber is 3-8 mu m, if the length-diameter ratio of the zirconium carbide whisker is too small, the length of the aluminum nitride fiber is too small, the effective toughening effect cannot be achieved, and if the length-diameter ratio of the zirconium carbide whisker is too large, the aluminum nitride fiber is too long, adhesion and caking are easy to occur, and the improvement of the overall bonding performance of the phosphate adhesive is also not facilitated.
The particle size of the chromium oxide and the magnesium oxide powder is not particularly limited, and the micro powder or the nano powder can be selected, and in some specific embodiments, the particle size of the magnesium oxide powder is, for example, 0.1-1 μm, and the particle size of the chromium oxide (chromium oxide powder) is, for example, 15-75 μm.
According to some preferred embodiments, the mass ratio of the silicon carbide whiskers to the pre-crosslinking system is 1: (20-30); the mass ratio of the aluminum nitride fiber to the pre-crosslinking system is 1: (30-60); and/or the mass ratio of the magnesia powder to the pre-crosslinking system is 1: (15-30); in the invention, in order to ensure the effective dispersion of toughening components and magnesium oxide powder components and the more effective high temperature resistance and high strength characteristics of the phosphate adhesive, the most preferred dosage of silicon carbide whisker, aluminum nitride fiber and magnesium oxide powder is obtained through a large number of creative experiments, and in the invention, the mass ratio of the silicon carbide whisker to the pre-crosslinking system is preferably 1: (20-30), wherein the mass ratio of the aluminum nitride fiber to the pre-crosslinking system is 1: (30-60), the mass ratio of the magnesia powder to the pre-crosslinking system is 1: (15-30).
The present invention provides in a second aspect a high strength, high temperature resistant insulation material made by the method of the invention described in the first aspect.
The invention will be further illustrated by way of example, but the scope of the invention is not limited to these examples.
In particular, in the present invention, "parts" refers to "parts by weight", and in the specific examples and comparative examples, the units of parts by weight may be collectively referred to as "g" or "kg", for example.
Example 1
(1) 80 parts of zirconia fiber (with the diameter of 3 mu m) and 20 parts of zirconium carbide fiber (with the diameter of 2 mu m) are weighed and uniformly dispersed in water to obtain fiber slurry with the mass fraction of 0.2% (the sum of the mass fractions of the zirconia fiber and the zirconium carbide fiber contained in the fiber slurry is 0.2%), and the fiber slurry is manufactured into a fiber wet sheet with the thickness of 0.5mm by a sheet machine.
(2) Mixing 6 parts of solid aluminum phosphate, 2 parts of magnesia (with the particle size of 200 mu m) and 1 part of chromium oxide, putting the mixture into a ball milling tank, ball milling for 8 hours to obtain filler, mixing 81 parts of aluminum dihydrogen phosphate solution with the solid content of 40wt% with the obtained filler, and stirring for 5 hours at 25 ℃ to obtain the high-temperature-resistant phosphate adhesive.
(3) And (3) pre-coating the high-temperature-resistant phosphate adhesive obtained in the step (2) on the surface of the reflecting screen (the graphite paper with the thickness of 0.025 mm) which is required to be contacted with the fiber wet sheet, controlling the coating thickness of the high-temperature-resistant phosphate adhesive to be 30 mu m, curing for 6 hours at 90 ℃, and then heating to 150 ℃ for curing for 12 hours to obtain the modified reflecting screen.
(4) And (3) alternately arranging 11 modified reflecting screens prepared by the method in the step (3) and 10 fiber wet sheets obtained in the step (1), wherein in the alternate arrangement, one fiber wet sheet is arranged between every two modified reflecting screens, the surface of the fiber wet sheet, which is contacted with the modified reflecting screens, is coated with the high-temperature-resistant phosphate adhesive obtained in the step (2), the coating thickness of the high-temperature-resistant phosphate adhesive is controlled to be 30 mu m, after the high-temperature-resistant phosphate adhesive is molded under the pressure of 1MPa for 60min, the high-temperature-resistant phosphate adhesive is cured for 6h at 90 ℃, and then the high-temperature-resistant phosphate adhesive is cured for 12h at the temperature of 150 ℃ to prepare the high-strength high-temperature-resistant heat insulation material.
Example 2
(1) 80 parts of zirconia fiber (with the diameter of 3 mu m) and 20 parts of zirconium carbide fiber (with the diameter of 2 mu m) are weighed and uniformly dispersed in water to obtain fiber slurry with the mass fraction of 3% (the sum of the mass fractions of the zirconia fiber and the zirconium carbide fiber contained in the fiber slurry is 3%), and the fiber slurry is manufactured into a fiber wet sheet with the thickness of 1mm by a sheet making machine.
(2) Mixing 13 parts of solid aluminum phosphate, 7 parts of magnesia (with the particle size of 200 mu m) and 3 parts of chromium oxide, putting the mixture into a ball milling tank, ball milling for 8 hours to obtain filler, mixing 100 parts of aluminum dihydrogen phosphate solution with the solid content of 40wt% with the obtained filler, and stirring for 5 hours at 25 ℃ to obtain the high-temperature-resistant phosphate adhesive.
(3) And (3) pre-coating the high-temperature-resistant phosphate adhesive obtained in the step (2) on the surface of the reflecting screen (the graphite paper with the thickness of 0.025 mm) which is required to be contacted with the fiber wet sheet, controlling the coating thickness of the high-temperature-resistant phosphate adhesive to be 50 mu m, curing for 6 hours at 90 ℃, and then heating to 150 ℃ for curing for 12 hours to obtain the modified reflecting screen.
(4) And (3) alternately arranging 6 modified reflecting screens prepared by the method in the step (3) and 5 fiber wet sheets obtained in the step (1), wherein in the alternate arrangement, one fiber wet sheet is arranged between every two modified reflecting screens, the surface of the fiber wet sheet, which is contacted with the modified reflecting screens, is coated with the high-temperature-resistant phosphate adhesive obtained in the step (2), the coating thickness of the high-temperature-resistant phosphate adhesive is controlled to be 50 mu m, after the high-temperature-resistant phosphate adhesive is molded under the pressure of 1MPa for 60min, the high-temperature-resistant phosphate adhesive is cured for 6h at 90 ℃, and then the high-temperature-resistant phosphate adhesive is cured for 12h at the temperature of 150 ℃ to prepare the high-strength high-temperature-resistant heat insulation material.
Example 3
(1) 85 parts of zirconia fiber (with the diameter of 3 mu m) and 15 parts of zirconium carbide fiber (with the diameter of 2 mu m) are weighed and uniformly dispersed in water to obtain fiber slurry with the mass fraction of 1% (the sum of the mass fractions of the zirconia fiber and the zirconium carbide fiber contained in the fiber slurry is 1%), and the fiber slurry is manufactured into a fiber wet sheet with the thickness of 3mm by a sheet making machine.
(2) 7 parts of solid aluminum phosphate, 4 parts of magnesia (with the particle size of 200 mu m) and 1 part of chromium oxide are mixed, and then are placed in a ball milling tank for ball milling for 8 hours to obtain filler, 24 parts of aluminum dihydrogen phosphate solution with the solid content of 40wt% are mixed with the obtained filler, and the mixture is stirred for 5 hours at the temperature of 25 ℃ to obtain the high-temperature-resistant phosphate adhesive.
(3) And (3) pre-coating the high-temperature-resistant phosphate adhesive obtained in the step (2) on the surface of the reflecting screen (the graphite paper with the thickness of 0.025 mm) which is required to be contacted with the fiber wet sheet, controlling the coating thickness of the high-temperature-resistant phosphate adhesive to be 90 mu m, curing for 6 hours at 90 ℃, and then heating to 150 ℃ for curing for 12 hours to obtain the modified reflecting screen.
(4) And (3) alternately arranging 4 modified reflecting screens prepared by the method in the step (3) and 3 fiber wet sheets obtained in the step (1), wherein in the alternate arrangement, one fiber wet sheet is arranged between every two modified reflecting screens, the surface of the fiber wet sheet, which is contacted with the modified reflecting screens, is coated with the high-temperature-resistant phosphate adhesive obtained in the step (2), the coating thickness of the high-temperature-resistant phosphate adhesive is controlled to be 90 mu m, after the high-temperature-resistant phosphate adhesive is molded under the pressure of 1MPa for 60min, the high-temperature-resistant phosphate adhesive is cured for 6h at 90 ℃, and then the high-temperature-resistant phosphate adhesive is cured for 12h at the temperature of 150 ℃ to prepare the high-strength high-temperature-resistant heat insulation material.
Example 4
(1) 85 parts of zirconia fiber (with the diameter of 3 mu m) and 15 parts of zirconium carbide fiber (with the diameter of 2 mu m) are weighed and uniformly dispersed in water to obtain fiber slurry with the mass fraction of 1% (the sum of the mass fractions of the zirconia fiber and the zirconium carbide fiber contained in the fiber slurry is 1%), and the fiber slurry is manufactured into a fiber wet sheet with the thickness of 3mm by a sheet making machine.
(2) 7 parts of solid zirconium phosphate, 4 parts of magnesia (with the grain diameter of 200 mu m) and 1 part of chromium oxide are mixed, then the mixture is placed in a ball milling tank for ball milling for 8 hours to obtain filler, 24 parts of aluminum dihydrogen phosphate solution with the solid content of 40wt% is mixed with the obtained filler, and the mixture is stirred for 5 hours at the temperature of 25 ℃ to obtain the high-temperature-resistant phosphate adhesive.
(3) And (3) pre-coating the high-temperature-resistant phosphate adhesive obtained in the step (2) on the surface of the reflecting screen (the graphite paper with the thickness of 0.025 mm) which is required to be contacted with the fiber wet sheet, controlling the coating thickness of the high-temperature-resistant phosphate adhesive to be 90 mu m, curing for 6 hours at 90 ℃, and then heating to 150 ℃ for curing for 12 hours to obtain the modified reflecting screen.
(4) And (3) alternately arranging 4 modified reflecting screens prepared by the method in the step (3) and 3 fiber wet sheets obtained in the step (1), wherein in the alternate arrangement, one fiber wet sheet is arranged between every two modified reflecting screens, the surface of the fiber wet sheet, which is contacted with the modified reflecting screens, is coated with the high-temperature-resistant phosphate adhesive obtained in the step (2), the coating thickness of the high-temperature-resistant phosphate adhesive is controlled to be 90 mu m, after the high-temperature-resistant phosphate adhesive is molded under the pressure of 1MPa for 60min, the high-temperature-resistant phosphate adhesive is cured for 6h at 90 ℃, and then the high-temperature-resistant phosphate adhesive is cured for 12h at the temperature of 150 ℃ to prepare the high-strength high-temperature-resistant heat insulation material.
Example 5
(1) 90 parts of zirconia fiber (with the diameter of 8 mu m) and 10 parts of zirconium carbide fiber (with the diameter of 5 mu m) are weighed and uniformly dispersed in water to obtain fiber slurry with the mass fraction of 1% (the sum of the mass fractions of the zirconia fiber and the zirconium carbide fiber contained in the fiber slurry is 1%), and the fiber slurry is manufactured into a fiber wet sheet with the thickness of 1mm by a sheet making machine.
(2) 7 parts of solid zirconium phosphate, 4 parts of magnesia (with the grain diameter of 200 mu m) and 1 part of chromium oxide are mixed, then the mixture is placed in a ball milling tank for ball milling for 8 hours to obtain filler, 24 parts of aluminum dihydrogen phosphate solution with the solid content of 40wt% is mixed with the obtained filler, and the mixture is stirred for 5 hours at the temperature of 25 ℃ to obtain the high-temperature-resistant phosphate adhesive.
(3) And (3) pre-coating the high-temperature-resistant phosphate adhesive obtained in the step (2) on the surface of the reflecting screen (the graphite paper with the thickness of 0.025 mm) which is required to be contacted with the fiber wet sheet, controlling the coating thickness of the high-temperature-resistant phosphate adhesive to be 90 mu m, curing for 6 hours at 90 ℃, and then heating to 150 ℃ for curing for 12 hours to obtain the modified reflecting screen.
(4) And (3) alternately arranging 6 modified reflecting screens prepared by the method in the step (3) and 5 fiber wet sheets obtained in the step (1), wherein in the alternate arrangement, one fiber wet sheet is arranged between every two modified reflecting screens, the surface of the fiber wet sheet, which is contacted with the modified reflecting screens, is coated with the high-temperature-resistant phosphate adhesive obtained in the step (2), the coating thickness of the high-temperature-resistant phosphate adhesive is controlled to be 90 mu m, after the high-temperature-resistant phosphate adhesive is molded under the pressure of 1MPa for 60min, the high-temperature-resistant phosphate adhesive is cured for 6h at 90 ℃, and then the high-temperature-resistant phosphate adhesive is cured for 12h at the temperature of 150 ℃ to prepare the high-strength high-temperature-resistant heat insulation material.
Example 6
(1) 80 parts of zirconia fiber (with the diameter of 3 mu m) and 20 parts of zirconium carbide fiber (with the diameter of 2 mu m) are weighed and uniformly dispersed in water to obtain fiber slurry with the mass fraction of 0.2% (the sum of the mass fractions of the zirconia fiber and the zirconium carbide fiber contained in the fiber slurry is 0.2%), and the fiber slurry is manufactured into a fiber wet sheet with the thickness of 0.5mm by a sheet machine.
(2) Mixing 6 parts of solid aluminum phosphate, 2 parts of magnesia (with the grain diameter of 200 mu m), 1 part of chromium oxide and 1 part of aluminum magnesium spinel (with the grain diameter of 20 mu m), placing the mixture in a ball milling tank, ball milling for 8 hours to obtain a filler, mixing 90 parts of aluminum dihydrogen phosphate solution with the solid content of 40wt% with the obtained filler, stirring for 5 hours at 25 ℃ to obtain a pre-crosslinking system, adding 5 parts of zirconium carbide whiskers (with the length-diameter ratio of 100) and 3.5 parts of aluminum nitride fibers with the length of 8 mu m into the obtained pre-crosslinking system, stirring and dispersing uniformly, adding 5 parts of magnesium oxide powder, stirring and dispersing uniformly to obtain the high-temperature-resistant phosphate adhesive.
(3) And (3) pre-coating the high-temperature-resistant phosphate adhesive obtained in the step (2) on the surface of the reflecting screen (the graphite paper with the thickness of 0.025 mm) which is required to be contacted with the fiber wet sheet, controlling the coating thickness of the high-temperature-resistant phosphate adhesive to be 30 mu m, curing for 6 hours at 90 ℃, and then heating to 150 ℃ for curing for 12 hours to obtain the modified reflecting screen.
(4) And (3) alternately arranging 11 modified reflecting screens prepared by the method in the step (3) and 10 fiber wet sheets obtained in the step (1), wherein in the alternate arrangement, one fiber wet sheet is arranged between every two modified reflecting screens, the surface of the fiber wet sheet, which is contacted with the modified reflecting screens, is coated with the high-temperature-resistant phosphate adhesive obtained in the step (2), the coating thickness of the high-temperature-resistant phosphate adhesive is controlled to be 30 mu m, after the high-temperature-resistant phosphate adhesive is molded under the pressure of 1MPa for 60min, the high-temperature-resistant phosphate adhesive is cured for 6h at 90 ℃, and then the high-temperature-resistant phosphate adhesive is cured for 12h at the temperature of 150 ℃ to prepare the high-strength high-temperature-resistant heat insulation material.
Comparative example 1
(1) 90 parts of zirconia fiber (with the diameter of 8 mu m) and 10 parts of zirconium carbide fiber (with the diameter of 5 mu m) are weighed and uniformly dispersed in water to obtain fiber slurry with the mass fraction of 1% (the sum of the mass fractions of the zirconia fiber and the zirconium carbide fiber contained in the fiber slurry is 1%), and the fiber slurry is manufactured into a fiber wet sheet with the thickness of 1mm by a sheet making machine.
(2) And (3) alternately arranging 6 reflecting screens (graphite paper with the thickness of 0.025 mm) and the fiber wet sheets obtained in the step (1), wherein in the alternate arrangement, one fiber wet sheet is arranged between every two reflecting screens, the surface of the fiber wet sheet, which is contacted with the reflecting screens, is coated with aluminum dihydrogen phosphate solution with the solid content of 40 weight percent, the coating thickness of the aluminum dihydrogen phosphate solution is controlled to be 90 mu m, and the aluminum dihydrogen phosphate solution is cured for 24 hours at the high temperature of 150 ℃ after being molded under the pressure of 1MPa for 60 minutes, so as to obtain the heat insulation material.
Comparative example 2
(1) 90 parts of zirconia fiber (with the diameter of 8 mu m) and 10 parts of zirconium carbide fiber (with the diameter of 5 mu m) are weighed and uniformly dispersed in water to obtain fiber slurry with the mass fraction of 1% (the sum of the mass fractions of the zirconia fiber and the zirconium carbide fiber contained in the fiber slurry is 1%), and the fiber slurry is manufactured into a fiber wet sheet with the thickness of 1mm by a sheet making machine.
(2) 7 parts of solid zirconium phosphate, 4 parts of magnesia (with the grain diameter of 200 mu m) and 1 part of chromium oxide are mixed, then the mixture is placed in a ball milling tank for ball milling for 8 hours to obtain filler, 24 parts of aluminum dihydrogen phosphate solution with the solid content of 40wt% is mixed with the obtained filler, and the mixture is stirred for 5 hours at the temperature of 25 ℃ to obtain the high-temperature-resistant phosphate adhesive.
(3) And (3) alternately arranging 6 reflecting screens (graphite paper with the thickness of 0.025 mm) and 5 fiber wet sheets obtained in the step (1), wherein in the alternate arrangement, one fiber wet sheet is arranged between every two reflecting screens, the surface of the fiber wet sheet, which is contacted with the reflecting screens, is coated with the high-temperature-resistant phosphate adhesive obtained in the step (2), the coating thickness of the high-temperature-resistant phosphate adhesive is controlled to be 90 mu m, after the high-temperature-resistant phosphate adhesive is molded for 60min under the pressure of 1MPa, the high-temperature-resistant phosphate adhesive is cured for 6h at 90 ℃, and then the high-temperature-resistant phosphate adhesive is heated to 150 ℃ and cured for 12h, so that the heat insulation material is prepared.
Comparative example 3
(1) 90 parts of zirconia fiber (with the diameter of 8 mu m) and 10 parts of zirconium carbide fiber (with the diameter of 5 mu m) are weighed and uniformly dispersed in water to obtain fiber slurry with the mass fraction of 1% (the sum of the mass fractions of the zirconia fiber and the zirconium carbide fiber contained in the fiber slurry is 1%), and the fiber slurry is manufactured into a fiber wet sheet with the thickness of 1mm by a sheet making machine.
(2) The surface of the reflecting screen (graphite paper with the thickness of 0.025 mm) which is required to be contacted with the wet fiber sheet is coated with an aluminum dihydrogen phosphate solution with the solid content of 40 weight percent in advance, the coating thickness of the aluminum dihydrogen phosphate solution is controlled to be 90 mu m, and then the reflecting screen is cured for 24 hours at the temperature of 150 ℃ to obtain the modified reflecting screen.
(3) And (3) alternately arranging 6 modified reflecting screens prepared by the method in the step (2) and 5 fiber wet sheets obtained in the step (1), wherein in the alternate arrangement, one fiber wet sheet is arranged between every two modified reflecting screens, the surface of the fiber wet sheet, which is in contact with the modified reflecting screens, is coated with aluminum dihydrogen phosphate solution with the solid content of 40 weight percent, the coating thickness of the aluminum dihydrogen phosphate solution is controlled to be 90 mu m, and after the aluminum dihydrogen phosphate solution is molded under the pressure of 1MPa for 60min, the aluminum dihydrogen phosphate solution is cured for 24 hours at the high temperature of 150 ℃ to prepare the heat insulation material.
Comparative example 4
(1) 90 parts of zirconia fiber (with the diameter of 8 mu m) and 10 parts of zirconium carbide fiber (with the diameter of 5 mu m) are weighed and uniformly dispersed in water to obtain fiber slurry with the mass fraction of 5% (the sum of the mass fractions of the zirconia fiber and the zirconium carbide fiber contained in the fiber slurry is 5%), and the fiber slurry is manufactured into a fiber wet sheet with the thickness of 1mm by a sheet making machine.
(2) 7 parts of solid zirconium phosphate, 4 parts of magnesia (with the grain diameter of 200 mu m) and 1 part of chromium oxide are mixed, then the mixture is placed in a ball milling tank for ball milling for 8 hours to obtain filler, 24 parts of aluminum dihydrogen phosphate solution with the solid content of 40wt% is mixed with the obtained filler, and the mixture is stirred for 5 hours at the temperature of 25 ℃ to obtain the high-temperature-resistant phosphate adhesive.
(3) And (3) pre-coating the high-temperature-resistant phosphate adhesive obtained in the step (2) on the surface of the reflecting screen (the graphite paper with the thickness of 0.025 mm) which is required to be contacted with the fiber wet sheet, controlling the coating thickness of the high-temperature-resistant phosphate adhesive to be 90 mu m, curing for 6 hours at 90 ℃, and then heating to 150 ℃ for curing for 12 hours to obtain the modified reflecting screen.
(4) And (3) alternately arranging 6 modified reflecting screens prepared by the method in the step (3) and 5 fiber wet sheets obtained in the step (1), wherein in the alternate arrangement, one fiber wet sheet is arranged between every two modified reflecting screens, the surface of the fiber wet sheet, which is contacted with the modified reflecting screens, is coated with the high-temperature-resistant phosphate adhesive obtained in the step (2), the coating thickness of the high-temperature-resistant phosphate adhesive is controlled to be 90 mu m, after the high-temperature-resistant phosphate adhesive is molded under the pressure of 1MPa for 60min, the high-temperature-resistant phosphate adhesive is cured for 6h at 90 ℃, and then the high-temperature-resistant phosphate adhesive is cured for 12h at the temperature of 150 ℃ to prepare the high-strength high-temperature-resistant heat insulation material.
Comparative example 5
(1) 90 parts of zirconia fiber (with the diameter of 8 mu m) and 10 parts of zirconium carbide fiber (with the diameter of 5 mu m) are weighed and uniformly dispersed in water to obtain fiber slurry with the mass fraction of 1% (the sum of the mass fractions of the zirconia fiber and the zirconium carbide fiber contained in the fiber slurry is 1%), and the fiber slurry is manufactured into a fiber wet sheet with the thickness of 1mm by a sheet making machine.
(2) After 7 parts of solid zirconium phosphate and 4 parts of magnesite (with the particle size of 200 mu m) are mixed, the mixture is placed in a ball milling tank for ball milling for 8 hours to obtain filler, 22 parts of aluminum dihydrogen phosphate solution with the solid content of 40wt% is mixed with the obtained filler, and the mixture is stirred for 5 hours at the temperature of 25 ℃ to obtain the phosphate adhesive.
(3) And (3) pre-coating the phosphate adhesive obtained in the step (2) on the surface of the reflecting screen (the graphite paper with the thickness of 0.025 mm) which is required to be contacted with the wet fiber sheet, controlling the coating thickness of the phosphate adhesive to be 90 mu m, curing for 6 hours at 90 ℃, and then heating to 150 ℃ for curing for 12 hours to obtain the modified reflecting screen.
(4) And (3) alternately arranging 6 modified reflecting screens prepared by the method in the step (3) and 5 fiber wet sheets obtained in the step (1), wherein in the alternate arrangement, one fiber wet sheet is arranged between every two modified reflecting screens, the surface of the fiber wet sheet, which is contacted with the modified reflecting screens, is coated with the phosphate adhesive obtained in the step (2), the coating thickness of the phosphate adhesive is controlled to be 90 mu m, after the phosphate adhesive is molded for 60min under the pressure of 1MPa, the fiber wet sheets are cured for 6h at 90 ℃, and then the fiber wet sheets are heated to 150 ℃ and cured for 12h, so that the heat insulation material is prepared.
Comparative example 6
(1) 80 parts of zirconia fiber (with the diameter of 3 mu m) and 20 parts of zirconium carbide fiber (with the diameter of 2 mu m) are weighed and uniformly dispersed in water to obtain fiber slurry with the mass fraction of 0.2% (the sum of the mass fractions of the zirconia fiber and the zirconium carbide fiber contained in the fiber slurry is 0.2%), and the fiber slurry is manufactured into a fiber wet sheet with the thickness of 0.5mm by a sheet machine.
(2) Mixing 6 parts of solid aluminum phosphate, 2 parts of magnesia (with the grain diameter of 200 mu m), 1 part of chromium oxide and 1 part of aluminum magnesium spinel (with the grain diameter of 20 mu m), placing the mixture in a ball milling tank, ball milling for 8 hours to obtain a filler, mixing 90 parts of aluminum dihydrogen phosphate solution with the solid content of 40wt% with the obtained filler, stirring for 20 minutes to uniformly disperse, adding 5 parts of zirconium carbide whisker (with the length-diameter ratio of 100) and 3.5 parts of aluminum nitride fiber with the length of 8 mu m, stirring to uniformly disperse, adding 5 parts of magnesium oxide powder, and stirring to uniformly disperse to obtain the phosphate adhesive.
(3) And (3) pre-coating the phosphate adhesive obtained in the step (2) on the surface of the reflecting screen (the graphite paper with the thickness of 0.025 mm) which is required to be contacted with the wet fiber sheet, controlling the coating thickness of the phosphate adhesive to be 30 mu m, curing for 6 hours at 90 ℃, and then heating to 150 ℃ for curing for 12 hours to obtain the modified reflecting screen.
(4) And (3) alternately arranging 11 modified reflecting screens prepared by the method in the step (3) and 10 fiber wet sheets obtained in the step (1), wherein in the alternate arrangement, one fiber wet sheet is arranged between every two modified reflecting screens, the surface of the fiber wet sheet, which is contacted with the modified reflecting screens, is coated with the phosphate adhesive obtained in the step (2), the coating thickness of the phosphate adhesive is controlled to be 30 mu m, after the phosphate adhesive is molded for 60min under the pressure of 1MPa, the fiber wet sheets are cured for 6h at 90 ℃, and then the temperature is raised to 150 ℃ for curing for 12h, so that the heat insulation material is prepared.
Comparative example 7
(1) 80 parts of zirconia fiber (with the diameter of 3 mu m) and 20 parts of zirconium carbide fiber (with the diameter of 2 mu m) are weighed and uniformly dispersed in water to obtain fiber slurry with the mass fraction of 0.2% (the sum of the mass fractions of the zirconia fiber and the zirconium carbide fiber contained in the fiber slurry is 0.2%), and the fiber slurry is manufactured into a fiber wet sheet with the thickness of 0.5mm by a sheet machine.
(2) Mixing 2 parts of magnesia (with the grain diameter of 200 mu m), 1 part of chromium oxide and 1 part of aluminum magnesium spinel (with the grain diameter of 20 mu m), putting the mixture into a ball milling tank, ball milling for 8 hours to obtain filler, mixing 90 parts of aluminum dihydrogen phosphate solution with the solid content of 40wt% with the obtained filler, stirring at 25 ℃ for 5 hours to obtain a pre-crosslinked system, adding 5 parts of zirconium carbide whisker (with the length-diameter ratio of 100) and 3.5 parts of aluminum nitride fiber with the length of 8 mu m into the obtained pre-crosslinked system, stirring and dispersing uniformly, adding 5 parts of magnesium oxide powder, stirring and dispersing uniformly to obtain the phosphate adhesive.
(3) And (3) pre-coating the high-temperature-resistant phosphate adhesive obtained in the step (2) on the surface of the reflecting screen (the graphite paper with the thickness of 0.025 mm) which is required to be contacted with the wet fiber sheet, controlling the coating thickness of the phosphate adhesive to be 30 mu m, curing for 6 hours at 90 ℃, and then heating to 150 ℃ for curing for 12 hours to obtain the modified reflecting screen.
(4) And (3) alternately arranging 11 modified reflecting screens prepared by the method in the step (3) and 10 fiber wet sheets obtained in the step (1), wherein in the alternate arrangement, one fiber wet sheet is arranged between every two modified reflecting screens, the surface of the fiber wet sheet, which is contacted with the modified reflecting screens, is coated with the phosphate adhesive obtained in the step (2), the coating thickness of the phosphate adhesive is controlled to be 30 mu m, after the phosphate adhesive is molded for 60min under the pressure of 1MPa, the fiber wet sheets are cured for 6h at 90 ℃, and then the fiber wet sheets are heated to 150 ℃ and cured for 12h, so that the high-strength high-temperature-resistant heat insulation material is prepared.
The present invention conducted performance tests on the insulation materials finally prepared in each example and each comparative example, and the results are shown in table 1, wherein 1500 ℃ compressive strength and 1800 ℃ compressive strength refer to compressive strength when the insulation materials are compression-damaged.
Table 1: results of comparison of the properties of the insulation materials prepared in examples and comparative examples
In table 1, the symbol "/" indicates that the performance index was not tested.
The invention is not described in detail in a manner known to those skilled in the art.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. The preparation method of the high-strength high-temperature-resistant heat insulation material is characterized by comprising the following steps of:
(1) Uniformly dispersing zirconia fibers and zirconium carbide fibers by using water to obtain fiber slurry, and manufacturing a fiber wet sheet from the fiber slurry;
(2) Mixing solid phosphate, magnesia and chromium oxide, performing ball milling to obtain a filler, and then mixing and stirring a phosphate solution and the filler to obtain a high-temperature-resistant phosphate adhesive;
(3) Coating the high-temperature-resistant phosphate adhesive on the surface of the reflecting screen, and curing to obtain a modified reflecting screen;
(4) Alternately arranging a plurality of modified reflecting screens and a plurality of fiber wet sheets, and then performing mould pressing and curing to obtain a high-strength high-temperature-resistant heat insulation material; in the alternate arrangement, a wet fiber sheet is arranged between every two modified reflecting screens, and the surface of the wet fiber sheet is coated with the high-temperature-resistant phosphate adhesive.
2. The method of manufacturing according to claim 1, characterized in that:
the diameter of the zirconia fiber is 3-10 mu m, and the diameter of the zirconium carbide fiber is 2-5 mu m;
the fiber slurry contains 0.2 to 3 percent of the sum of the mass percentages of zirconia fiber and zirconium carbide fiber; and/or
The mass ratio of the zirconia fiber to the zirconium carbide fiber is (4-10): 1.
3. the method of manufacturing according to claim 1, characterized in that:
the thickness of the fiber wet sheet is 0.5-3 mm.
4. The method of manufacturing according to claim 1, characterized in that:
the mass ratio of the solid phosphate to the magnesia to the chromium oxide is (6-13): (2-7): (1-3);
the solid phosphate is solid aluminum phosphate and/or solid zirconium phosphate;
The grain diameter of the magnesia is 10-200 mu m; and/or
The ball milling time is 6-12 h.
5. The method of manufacturing according to claim 1, characterized in that:
the stirring is carried out for 3-6 h at room temperature.
6. The method of manufacturing according to claim 1, characterized in that:
the solid content of the phosphate solution is 20-60 wt%;
the mass ratio of the phosphate solution to the filler is (2-9): 1, a step of; and/or
The phosphate solution is one or more of aluminum dihydrogen phosphate solution, aluminum phosphate solution and zirconium phosphate solution.
7. The method of manufacturing according to claim 1, characterized in that:
coating the high-temperature-resistant phosphate adhesive on the surface of the reflecting screen, wherein the thickness of the high-temperature-resistant phosphate adhesive is 30-90 mu m; and/or
The surface of the fiber wet sheet is coated with the high-temperature-resistant phosphate adhesive, and the thickness of the fiber wet sheet is 30-90 mu m.
8. The method of manufacturing according to claim 1, characterized in that:
in step (3) and/or step (4), the curing is: curing for 4-8 h at 80-100 ℃ and then curing for 10-15 h at 120-180 ℃.
9. The preparation method according to any one of claims 1 to 8, wherein in step (2):
the filler also comprises aluminum magnesium spinel, and preferably, in the filler, the mass ratio of the solid phosphate to the magnesia to the chromium oxide to the aluminum magnesium spinel is (6-13): (2-7): (1-3): (1-5); and/or
After stirring, zirconium carbide whisker and aluminum nitride fiber are added and uniformly dispersed, and then magnesia powder is added and uniformly dispersed, so that the high-temperature-resistant phosphate adhesive is obtained.
10. A high strength, high temperature resistant insulation material made by the method of any one of claims 1 to 9.
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