CN116751036A - Prestressed alumina ceramic composite material and preparation method thereof - Google Patents
Prestressed alumina ceramic composite material and preparation method thereof Download PDFInfo
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- CN116751036A CN116751036A CN202310860463.4A CN202310860463A CN116751036A CN 116751036 A CN116751036 A CN 116751036A CN 202310860463 A CN202310860463 A CN 202310860463A CN 116751036 A CN116751036 A CN 116751036A
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 239000002131 composite material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000000576 coating method Methods 0.000 claims abstract description 49
- 239000011248 coating agent Substances 0.000 claims abstract description 47
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 16
- 239000006255 coating slurry Substances 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 239000011230 binding agent Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000002270 dispersing agent Substances 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000000875 high-speed ball milling Methods 0.000 claims abstract description 3
- 239000010453 quartz Substances 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 239000011159 matrix material Substances 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 239000000758 substrate Substances 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 3
- 239000004359 castor oil Substances 0.000 claims description 3
- 235000019438 castor oil Nutrition 0.000 claims description 3
- 238000009694 cold isostatic pressing Methods 0.000 claims description 3
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 abstract description 7
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 3
- 239000002002 slurry Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 14
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 12
- 239000000463 material Substances 0.000 description 12
- 229910052863 mullite Inorganic materials 0.000 description 12
- 230000035939 shock Effects 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000001680 brushing effect Effects 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 102100038720 Histone deacetylase 9 Human genes 0.000 description 1
- 101001032092 Homo sapiens Histone deacetylase 9 Proteins 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000007676 flexural strength test Methods 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011664 nicotinic acid Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—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
- C04B35/10—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 aluminium oxide
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
- C04B41/5031—Alumina
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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Abstract
The invention discloses a prestressed alumina ceramic composite material and a preparation method thereof, and belongs to the technical field of ceramic material preparation. The method comprises the following steps: (1) preparation of coating slurry: mixing the coating powder, the dispersing agent and the binding agent in alcohol, and performing high-speed ball milling and dispersing to obtain coating slurry; (2) preparing a coating on the blank: uniformly coating the coating slurry on the alumina pre-sintered blank, repeating for several times, and drying in the shade for 2 hours; (3) sintering of the prestressed composite: heating to 500-800 ℃, and preserving heat for 0.5-1 h; then heating to 1600 ℃ at 5-20 ℃/min, preserving heat for 1-2 hours, and cooling along with a furnace. The invention brushes coating slurry on the surface of unsintered densified alumina ceramic, and the slurry is sintered and densified into prestressed composite ceramic at high temperature after being dried.
Description
Technical Field
The invention relates to the technical field of ceramic material synthesis, in particular to a prestressed alumina ceramic composite material and a preparation method thereof.
Background
The alumina ceramic is alpha-Al 2 O 3 The structural ceramic is a main crystalline phase, has high strength, high hardness, high temperature resistance and good electrical insulation property, particularly has excellent chemical stability and oxidation resistance, has wide raw material sources and low cost, and has been widely applied to the engineering fields of electronics, aviation, machinery, chemical industry, construction and the like.
However, the alumina ceramic material has the problems of high thermal expansion coefficient, inferior thermal shock resistance and thermal conductivity as compared with non-oxide materials, and is used as a typical brittle material which resists compression but does not resist tension, has small fracture stress during damage and is easy to generate sudden brittle fracture. Therefore, the simple realization of the reinforcement and the toughening of the alumina and the improvement of the reliability are decisive factors for realizing the re-development of the alumina.
At present, methods for improving the strength of alumina ceramics include improvement of sintering process, introduction of particle reinforced phase (particles and fibers), bionic layered structure, surface treatment and the like, but the methods are mainly applied to important fields of military industry, aerospace and the like, and are limited by cost and shape and size, for example, the layered structure has complicated process and limited size.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a prestressed alumina ceramic composite material and a preparation method thereof. According to the invention, the quartz-alumina mixed coating is prepared on the surface of unsintered alumina, and the mullite-alumina mixed coating is formed after co-sintering densification, and the coating can form residual compressive stress in the cooling process, so that the problem of lower mechanical strength and toughness of alumina ceramic is solved, and meanwhile, the high-temperature strength and corrosion resistance of alumina can be improved.
In order to solve the technical problems, the invention provides the following technical scheme:
in one aspect, the invention provides a prestressed alumina ceramic composite material, wherein alumina is used as a matrix, mullite coatings with the thickness of 20-150 mu m are arranged on the upper surface and the lower surface of the composite material, and the thickness ratio of the matrix to the coatings is more than 10.
Furthermore, the coating is prepared from a mixture of quartz and alumina, and the coating is coated on the surface of a substrate and then sintered together with the substrate to form the composite material.
Preferably, the mass fraction of quartz in the mixture is 10-15% and the mass fraction of alumina is 85-90%.
In another aspect, the present invention also provides a method for preparing a prestressed alumina ceramic composite, comprising:
(1) Preparing an alumina blank: the green body is formed by dry pressing, 50-70MPa dry pressing, 150-300MPa cold isostatic pressing, and the green body is presintered at 800-1100 ℃ to increase the strength and remove the organic matters;
(2) Preparation of coating slurry: mixing quartz and alumina mixed coating powder, a dispersing agent and a binder in alcohol, and performing high-speed ball milling and dispersing to obtain coating slurry;
(3) Preparing a coating on the blank: uniformly coating the coating slurry on the alumina pre-sintered blank, repeating for 5-10 times, and finally drying in the shade for 2h;
(4) Sintering of the pre-stress composite: heating to 500-800 ℃, and preserving heat for 0.5-1 h; then heating to 1600 ℃ at 5-20 ℃/min, preserving heat for 1-2 hours, and cooling along with a furnace.
Further, in the step (2), the coating powder is a mixture of quartz and alumina, the particle size of the alumina is less than 500nm, and the particle size of the quartz is less than 1 μm, so as to improve the sintering activity of the coating powder.
Further, the binder is polyvinyl alcohol Ding Quanzhi.
Further, the dispersing agent is castor oil.
Further, the consumption of the binder is 1-10% of the mass of the coating powder; the consumption of the dispersing agent is 0.1-1% of the mass of the coating powder.
Further, the ball milling speed is 200-500 r/min, and the time is more than 2 h.
Mullite as Al 2 O 3 -SiO 2 The compound is stable in a binary system, has low heat conductivity, high-temperature strength, good thermal shock resistance, low thermal expansion coefficient, oxidation resistance and chemical corrosion resistance, and has good high-temperature stability and thermal shock resistance. Therefore, the quartz-alumina coating prepared on the surface of the unsintered alumina not only can form mullite at high temperature, but also can form compressive stress in the cooling process, thereby achieving the aim of greatly improving the strength of the alumina, or being called as (toughened ceramic).
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a method for preparing a mullite pre-stress coating on the surface of alumina, which can endow the alumina with better strength (improved by more than 25 percent) and thermal shock resistance through the compressive stress formed by the surface coating; meanwhile, the alumina blank has stable strength after dry pressing and isostatic pressing, and strong processability; the coating has good matching property with the matrix after sintering, and has no large buckling deformation; the lower dielectric constant of mullite can also reduce the dielectric constant of alumina, so that the mullite is more beneficial to the field of electronic packaging. The structure is shown in fig. 1. In the preparation process of the coating slurry, the solvent is alcohol, so that the defect that the coating cannot be sintered due to direct cracking after being coated by adopting a water-based formula coating is avoided.
Drawings
FIG. 1 is a schematic structural diagram of a material prepared by the method of example 1 of the present invention and a schematic stress diagram of a section thereof;
fig. 2 is an SEM image of the material prepared by the method of example 1 of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved more apparent, the following detailed description will be given with reference to the accompanying drawings and specific embodiments.
The reagents and materials used in the examples and comparative examples were all commercially available unless otherwise specified.
The invention provides a prestressed alumina ceramic composite material and a preparation method thereof, and specific embodiments are as follows.
Example 1
A preparation method of a prestressed alumina ceramic composite material comprises the following steps:
(1) Preparing an alumina blank: the green body is formed by dry pressing, 65MPa dry pressing, 300MPa cold isostatic pressing, and the green body organic matters are removed by presintering at 1000 ℃ at low temperature, so that the strip with the size of 3.5 multiplied by 4.5 multiplied by 41.9 is processed.
(2) Preparation of coating slurry: quartz (SiO) with an amount of 15wt% was dissolved in ethanol 2 ) With 85wt% alumina (d50=400 nm Al 2 O 3 ) Mixing, adding a binder PVB (polyvinyl butyral) accounting for 5% of the powder mass and a dispersant castor oil accounting for 0.5% of the powder mass, transferring into a planetary ball mill (YXQM-1L, MITR, china) for ball milling and dispersing for 5 hours, wherein the ball-to-material ratio is 10:1, the rotating speed is 300r/min.
(3) Preparing a coating on the blank: dipping a small amount of dispersed coating slurry by using a fine brush, uniformly brushing the upper and lower surfaces of the alumina blank, brushing the upper and lower surfaces for 5 times respectively, drying in the shade for more than 2 hours after brushing, and then putting into a sintering furnace for sintering.
(4) Sintering of the pre-stress composite: heating to 500 ℃, and preserving heat for 0.5h; then the temperature is raised to 1600 ℃ at 5 ℃/min, the temperature is kept for 2 hours, and the temperature is cooled along with a furnace, and the size of the sintered composite body is about 3 multiplied by 4 multiplied by 36.
As can be seen from FIG. 2, the coating prepared by the method is uniformly adhered to the alumina matrix ceramic, the thickness of the single-sided coating is about 25 mu m, and the coating is tightly combined with the matrix, so that the defects of cracks, interface sliding and the like are avoided.
Example 2
In this example, the coating material was quartz: alumina = 5:95, the other conditions were the same as in example 1.
Example 3
In this example, the coating material was quartz: alumina = 10:90, the rest of the conditions are the same as in example 1.
Example 4
In this example, the coating material was quartz: alumina = 30:70, the other conditions were the same as in example 1.
Example 5
In this example, the coating paste was brushed onto and off the substrate 10 times each, with the other conditions being the same as in example 1.
To highlight the beneficial effects of the materials prepared by the method of the present invention, the inventors devised comparative examples as follows.
Comparative example 1
Coating raw material quartz in this comparative example: alumina = 40:60, the other conditions are the same as in example 1.
Comparative example 2
In this example, the coating material was mullite in the crystalline phase only, the grain size was 2.6 μm, and the other conditions were the same as in example 1.
Comparative example 3
The step (4) of the comparative example is specifically as follows: heating to 500 ℃, and preserving heat for 0.5h; then raising the temperature to 1700 ℃ at 5 ℃/min, preserving heat for 2 hours, and cooling along with a furnace, wherein the size of the sintered composite is about 3 multiplied by 4 multiplied by 36; the other conditions were the same as in example 1.
Comparative example 4
The step (5) of the comparative example is specifically as follows: heating to 500 ℃, and preserving heat for 0.5h; then raising the temperature to 1500 ℃ at 5 ℃/min, preserving heat for 2 hours, and cooling along with a furnace, wherein the size of the sintered composite is about 3 multiplied by 4 multiplied by 36; the other conditions were the same as in example 1.
The materials prepared by the methods of examples 1 to 5 and comparative examples 1 to 4 described above were subjected to flexural strength performance test, the test methods being referred to "GBT 6569-2006-Fine ceramic flexural Strength test method", and the results are shown in Table 1.
TABLE 1 bending strength of alumina and prestressed alumina ceramics
As shown in Table 1, the original strength of the alumina ceramic is 400.50 + -37.25 MP, and the bending strength of the prestressed alumina ceramic composite material prepared by the invention can be improved by 37% compared with that of the alumina ceramic matrix.
When the proportion of quartz to alumina is regulated and the doping amount of quartz in comparative example 1 is higher, the composite is easy to warp and deform due to the fact that the sintering of the coating and the matrix is not matched, and the strength is greatly reduced; in comparative example 2, pure crystalline phase mullite is used as a coating, and the strength improvement is not obvious, mainly because the sintering densification temperature of the crystalline phase mullite is higher, a better strong interface cannot be formed with a matrix, and the strong interface is a necessary condition for generating residual compressive stress.
In comparative example 3, when the sintering temperature (1700 ℃) is too high, the strength of the composite material is not greatly improved, and the mullite in the coating is easily decomposed due to the too high sintering temperature; in comparative example 4, when the sintering temperature (1500 ℃) is too low, the strength of the composite material starts to decrease, firstly, the densified composite cannot be formed because the sintering densification temperature of the matrix alumina is not reached, and secondly, quartz and alumina in the coating do not sufficiently react to form mullite.
The process parameters of each step in the invention are adjusted within the limit range, and the performance of the prepared composite material is consistent with that of the previous embodiment, and the description is omitted here.
In summary, the invention utilizes quartz-alumina to prepare the mullite coating with low expansion coefficient on the surface of alumina ceramic, the shrinkage of the matrix is large in the cooling process, the shrinkage of the coating is small, proper residual compressive stress can be formed in the coating, and the strength of the alumina is greatly improved.
The foregoing is a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention and are intended to be comprehended within the scope of the present invention.
Claims (9)
1. The prestressed alumina ceramic composite material is characterized in that alumina is used as a matrix, mullite-alumina mixed coating with the thickness of 20-150 mu m is arranged on the upper surface and the lower surface of the composite material, and the thickness ratio of the matrix to the coating is more than 10.
2. The pre-stressed alumina ceramic composite of claim 1, wherein the coating is prepared from a mixture of quartz and alumina, and the coating is applied to the surface of the substrate and co-sintered with the substrate to form the composite.
3. The pre-stressed alumina ceramic composite of claim 2, wherein the mass fraction of quartz in the mixture is 10-15% and the mass fraction of alumina is 85-90%.
4. The preparation method of the prestressed alumina ceramic composite material is characterized by comprising the following steps:
(1) Preparing an alumina blank: the green body is formed by adopting dry pressing of 50-70MPa, then is subjected to cold isostatic pressing of 150-300MPa, and finally is presintered at 800-1100 ℃ to increase the strength and remove the organic matters of the green body;
(2) Preparation of coating slurry: mixing the coating powder, the dispersing agent and the binding agent in alcohol, and performing high-speed ball milling and dispersing to obtain coating slurry;
(3) Preparing a coating on the blank: uniformly coating the coating slurry on the alumina pre-sintered blank, repeating for 5-10 times, and finally drying in the shade for 2h;
(4) Sintering of the pre-stress composite: heating to 500-800 deg.c and maintaining for 0.5-1 hr; then heating to 1600 ℃ at 5-20 ℃/min, preserving heat for 1-2 hours, and cooling along with a furnace.
5. The method of producing a prestressed alumina ceramic composite according to claim 4, wherein in said step (2), the alumina particle size is less than 500nm, and the quartz particle size is less than 1 μm.
6. The method of claim 5, wherein the binder is polyvinyl alcohol Ding Quanzhi.
7. The method of claim 6, wherein the dispersant is castor oil.
8. The method for preparing the prestressed alumina ceramic composite material according to claim 7, wherein the binder is used in an amount of 1-10% of the mass of the coating powder; the consumption of the dispersing agent is 0.1-1% of the mass of the coating powder.
9. The method for preparing the prestressed alumina ceramic composite according to claim 8, wherein the ball milling speed is 200-500 rpm for more than 2 hours.
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| CN202210854454.XA CN115043648A (en) | 2022-07-15 | 2022-07-15 | Prestressed alumina ceramic composite material and preparation method thereof |
| CN202210854454X | 2022-07-15 |
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| CN110877975B (en) * | 2018-09-05 | 2021-09-24 | 中国建材检验认证集团股份有限公司 | Prestressed ceramic and preparation method thereof |
| CN112390627B (en) * | 2020-11-20 | 2022-06-17 | 广东大角鹿新材料有限公司 | Kyanite/alumina prestressed ceramic and preparation method thereof |
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