CN116514524A - Heat-resistant high-strength low-expansion ceramic and preparation method thereof - Google Patents
Heat-resistant high-strength low-expansion ceramic and preparation method thereof Download PDFInfo
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- CN116514524A CN116514524A CN202310494803.6A CN202310494803A CN116514524A CN 116514524 A CN116514524 A CN 116514524A CN 202310494803 A CN202310494803 A CN 202310494803A CN 116514524 A CN116514524 A CN 116514524A
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- resistant high
- strength low
- expansion ceramic
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- 239000000919 ceramic Substances 0.000 title claims abstract description 86
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 239000002689 soil Substances 0.000 claims abstract description 111
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 58
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000000843 powder Substances 0.000 claims abstract description 52
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 49
- CNLWCVNCHLKFHK-UHFFFAOYSA-N aluminum;lithium;dioxido(oxo)silane Chemical compound [Li+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O CNLWCVNCHLKFHK-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052642 spodumene Inorganic materials 0.000 claims abstract description 42
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 32
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052573 porcelain Inorganic materials 0.000 claims abstract description 27
- 239000010453 quartz Substances 0.000 claims abstract description 26
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000002699 waste material Substances 0.000 claims abstract description 25
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 23
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 8
- 239000003093 cationic surfactant Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 48
- 229910001868 water Inorganic materials 0.000 claims description 48
- 238000005245 sintering Methods 0.000 claims description 45
- 238000010438 heat treatment Methods 0.000 claims description 44
- 238000001035 drying Methods 0.000 claims description 39
- 239000002002 slurry Substances 0.000 claims description 28
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 27
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 25
- 238000002156 mixing Methods 0.000 claims description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 21
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 20
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 238000010791 quenching Methods 0.000 claims description 16
- 230000000171 quenching effect Effects 0.000 claims description 16
- 239000007921 spray Substances 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 15
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 15
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 230000032683 aging Effects 0.000 claims description 14
- 239000010439 graphite Substances 0.000 claims description 14
- 229910002804 graphite Inorganic materials 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000002480 mineral oil Substances 0.000 claims description 12
- 235000010446 mineral oil Nutrition 0.000 claims description 12
- 238000005498 polishing Methods 0.000 claims description 12
- 238000007873 sieving Methods 0.000 claims description 12
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 238000005507 spraying Methods 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 239000010419 fine particle Substances 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 15
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 12
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 12
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 12
- 238000000227 grinding Methods 0.000 description 12
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 12
- 238000004140 cleaning Methods 0.000 description 10
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 10
- 238000011049 filling Methods 0.000 description 9
- 230000035939 shock Effects 0.000 description 9
- OJLGWNFZMTVNCX-UHFFFAOYSA-N dioxido(dioxo)tungsten;zirconium(4+) Chemical compound [Zr+4].[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O OJLGWNFZMTVNCX-UHFFFAOYSA-N 0.000 description 7
- 229910001928 zirconium oxide Inorganic materials 0.000 description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 6
- 239000000292 calcium oxide Substances 0.000 description 6
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 6
- 230000006835 compression Effects 0.000 description 6
- 238000007906 compression Methods 0.000 description 6
- 239000000395 magnesium oxide Substances 0.000 description 6
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 6
- 239000011787 zinc oxide Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000007670 refining Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000010304 firing Methods 0.000 description 4
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000035515 penetration Effects 0.000 description 4
- 229920000962 poly(amidoamine) Polymers 0.000 description 4
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 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 3
- 229910052863 mullite Inorganic materials 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 3
- 229910001950 potassium oxide Inorganic materials 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 3
- 229910001948 sodium oxide Inorganic materials 0.000 description 3
- 238000005728 strengthening Methods 0.000 description 3
- 230000035882 stress Effects 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 229910000480 nickel oxide Inorganic materials 0.000 description 2
- 229910018068 Li 2 O Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 150000001412 amines Chemical group 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- 230000009693 chronic damage Effects 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000000930 thermomechanical effect Effects 0.000 description 1
- AAWZNWVCESLFTD-UHFFFAOYSA-N tungsten;hydrate Chemical compound O.[W] AAWZNWVCESLFTD-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/04—Clay; Kaolin
-
- 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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
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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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
- C04B33/1324—Recycled material, e.g. tile dust, stone waste, spent refractory material
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- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/16—Lean materials, e.g. grog, quartz
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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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
- C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
- C04B2235/3472—Alkali metal alumino-silicates other than clay, e.g. spodumene, alkali feldspars such as albite or orthoclase, micas such as muscovite, zeolites such as natrolite
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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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- C04B2235/00—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
- C04B2235/6567—Treatment time
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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
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/661—Multi-step sintering
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
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- Environmental & Geological Engineering (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a heat-resistant high-strength low-expansion ceramic, which comprises the following raw materials in percentage by mass: 15-25% of Guizhou soil, 15-25% of Zhangzhou soil, 3-7% of Xinyang soil, 10-14% of Datong soil, 8-12% of quartz powder, 4-6% of waste porcelain powder, 2-4% of talcum powder and the balance of spodumene. Further comprises: activated graphite, alpha-alumina, zirconia, tungsten trioxide, silica sol, and ammonium salt type cationic surfactants; the mass ratio of the activated graphite, the alpha-alumina, the zirconia, the tungsten trioxide, the silica sol and the ammonium salt cationic surfactant to the Guizhou soil is 1-5:1-6:1-2:1-3:1-3:1-2:15-25. The invention discloses a preparation method of the heat-resistant high-strength low-expansion ceramic. The invention discloses application of the heat-resistant high-strength low-expansion ceramic to kitchen utensils.
Description
Technical Field
The invention relates to the technical field of ceramics, in particular to a heat-resistant high-strength low-expansion ceramic, and a preparation method and application thereof.
Background
The traditional marmite is a ceramic product which is generally prepared by mixing raw materials such as quartz, feldspar, clay and the like which are difficult to transfer heat and firing at high temperature, and has the characteristic of uniform heat transfer. Due to the problems of the manufacturing process and raw materials, the traditional marmite cannot resist temperature difference change, is easy to crack and cannot burn dry. The spodumene is added to the raw materials after the traditional marmite is improved, so that the high-temperature resistant marmite is manufactured, and under the condition that the original advantages of the marmite are maintained, the marmite can also bear hundreds of high-temperature dry combustion without cracking, and the practicability of the marmite is greatly improved.
In recent years, along with the requirement of new energy, the use of spodumene for refining and producing lithium carbonate and for lithium batteries has led to the shortage of spodumene, while the use amount of spodumene in a marmite formula is generally more than 40%, the use amount is large, and the production of traditional heat-resistant marmite porcelain is limited. Meanwhile, most of marmite in market mainly uses full glaze marmite, although easy to clean and color lubricating, harmful substances such as lead and cadmium contained in the marmite can be separated out due to repeated heating, so that the marmite is easy to accumulate in the body to cause chronic damage, and the surface of the marmite is easy to crack alternately along with cold and hot.
Therefore, on the basis of ensuring the heat resistance of the marmite, the addition amount of spodumene in the marmite is reduced, and the precipitation of heavy metal is reduced, so that the marmite which is nontoxic and harmless and has a low expansion surface and is not easy to crack is obtained, and the marmite has great significance.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides heat-resistant high-strength low-expansion ceramic and a preparation method thereof.
The heat-resistant high-strength low-expansion ceramic comprises the following raw materials in percentage by mass: 15-25% of Guizhou soil, 15-25% of Zhangzhou soil, 3-7% of Xinyang soil, 10-14% of Datong soil, 8-12% of quartz powder, 4-6% of waste porcelain powder, 2-4% of talcum powder and the balance of spodumene.
The Guizhou soil, namely the porcelain clay of which the origin is Guizhou region, is randomly extracted and detected by the applicant, and the content of the porcelain clay is as follows:
| name of the name | Content of% | Name of the name | Content of% |
| SiO 2 (silica) | 39.07 | P 2 O 5 (phosphorus pentoxide) | 0.19 |
| Al 2 O 3 (aluminum oxide) | 34.97 | SO 3 (Sulfur trioxide) | 0.03 |
| Fe 2 O 3 (ferric oxide) | 9.08 | BaO (barium oxide) | 0.08 |
| CaO (calcium oxide) | 050 | ZnO (Zinc oxide) | 0.10 |
| MgO (magnesia) | 0.11 | ZrO2 (zirconium dioxide) | 0.02 |
| K 2 O (Potassium oxide) | 0.23 | NiO (Nickel oxide) | 0.16 |
| Na 2 O (sodium oxide) | 0.01 | Cr 2 O 3 (chromium oxide) | 0.03 |
| TiO 2 (titanium dioxide) | 0.18 | Burning loss | 15.03 |
| MnO (manganese oxide) | 0.23 |
The Zhangzhou soil, namely the porcelain clay of which the origin is Zhangzhou region, is randomly extracted and detected by the applicant, and the content of the Zhangzhou soil is as follows:
the Xinyang soil, namely porcelain soil in which the origin is Xinyang region, is randomly extracted and detected by the applicant, and the content of the Xinyang soil is as follows:
| name of the name | Content of% | Name of the name | Content of% |
| SiO 2 (silica) | 68.76 | MnO (manganese oxide) | 0.04 |
| Al 2 O 3 (aluminum oxide) | 14.58 | P 2 O 5 (phosphorus pentoxide) | <0.01 |
| Fe 2 O 3 (ferric oxide) | 1.86 | SO 3 (Sulfur trioxide) | <0.01 |
| CaO (calcium oxide) | 1.68 | BaO (barium oxide) | <0.01 |
| MgO (magnesia) | 2.52 | ZnO (Zinc oxide) | 0.01 |
| K 2 O (Potassium oxide) | 1.20 | ZrO 2 (zirconium dioxide) | 0.02 |
| Na 2 O (sodium oxide) | 0.88 | SrO (strontium oxide) | 0.02 |
| TiO 2 (titanium dioxide) | 0.11 | Burning loss | 8.31 |
The method comprises the steps that the large common soil, namely porcelain clay in the large common region, is extracted by the applicant randomly to be detected, and the content of the large common soil is as follows:
the applicant randomly extracts a batch of spodumene for detection, and the content of spodumene is as follows:
| name of the name | Content of% | Name of the name | Content of% |
| SiO 2 (silica) | 73.42 | MnO (manganese oxide) | 0.04 |
| Al 2 O 3 (aluminum oxide) | 19.53 | P 2 O 5 (phosphorus pentoxide) | 0.03 |
| Fe 2 O 3 (ferric oxide) | 0.13 | SO 3 (Sulfur trioxide) | <0.01 |
| CaO (calcium oxide) | 0.10 | BaO (barium oxide) | 0.02 |
| MgO (magnesia) | 0.07 | ZnO (Zinc oxide) | 0.01 |
| K 2 O (Potassium oxide) | 0.50 | ZrO 2 (zirconium dioxide) | 0.02 |
| Na 2 O (sodium oxide) | 0.41 | Li 2 O (lithium oxide) | 5.37 |
| TiO 2 (titanium dioxide) | 0.01 | Burning loss | 0.35 |
Preferably, the raw materials of the heat-resistant high-strength low-expansion ceramic further comprise: activated graphite, alpha-alumina, zirconia, tungsten trioxide, silica sol, and ammonium salt type cationic surfactants; the mass ratio of the activated graphite, the alpha-alumina, the zirconia, the tungsten trioxide, the silica sol and the ammonium salt cationic surfactant to the Guizhou soil is 1-5:1-6:1-2:1-3:1-2:15-25.
Preferably, the activated graphite is prepared by the steps of: soaking flake graphite in mixed acid for 1-2h, washing with water, drying, adding into methanol, adding ethylenediamine into the mixture under stirring, stirring for 1-2h, adding methyl acrylate under nitrogen atmosphere, adjusting temperature to 40-50deg.C, stirring for 10-20h, and distilling under reduced pressure to obtain activated graphite.
Preferably, the mixed acid comprises: sulfuric acid with a concentration of 1.5-1.7mol/L and nitric acid with a concentration of 14-16 mol/L.
Preferably, the mass ratio of the crystalline flake graphite to the ethylenediamine to the methyl acrylate is 5-15:1-3:1-3.
The preparation method of the heat-resistant high-strength low-expansion ceramic comprises the following steps:
s1, uniformly mixing spodumene, guizhou soil, zhangzhou soil, xinyang soil, quartz powder, datong soil, waste porcelain powder, talcum powder and activated graphite, then ball-milling, removing iron and ferric oxide, sieving, drying and crushing to obtain premix;
s2, uniformly mixing premix, alpha-alumina, zirconia and tungsten trioxide, and then spraying out to obtain purified slurry after pretreatment by a plasma spray gun;
s3, adding the purified slurry into a mud filter for dehydration, adding silica sol and ammonium salt cationic surfactant, stirring uniformly, then carrying out vacuum pugging in a vacuum pugging machine with the vacuum degree of 40-80kPa, then ageing for 5-10 days in an environment with the temperature of 15-22 ℃ and the relative humidity of 45-52RH%, and then feeding into a vacuum pugging machine with the vacuum degree of 20-50kPa again for vacuum pugging, and forming to obtain a blank;
s4, drying the blank to automatically release the film, vacuum freeze-drying to the water content of 1-1.5%, ultrasonic cleaning with absolute ethyl alcohol for 5-15min, polishing to be round, checking the blank, and drying in a blank warehouse at 20-30 ℃ to obtain green blank;
s5, kiln-loading green blanks, heating to 500-560 ℃ under nitrogen atmosphere, preserving heat for 20-30min, heating to 1000-1050 ℃, preserving heat for 1-2h, heating to 1100-1200 ℃ and sintering for 10-20h, maintaining sintering air pressure at 0.12-0.15MPa in the sintering process, and quenching in mineral oil to room temperature to obtain the heat-resistant high-strength low-expansion ceramic.
Preferably, in S1, ball milling is carried out to a fineness of 800-1000 meshes.
Preferably, in S2, the plasma torch parameters are as follows: argon is 20-30L/min, hydrogen is 5-15L/min, voltage is 70-80V, and current is 600-700A.
Preferably, in S4, the ultrasonic frequency is 5-12kHz, and the ultrasonic power is 300-400W.
Preferably, the specific temperature rising rate in S5 is as follows: heating to 500-560 deg.C at 1-5 deg.C/min under nitrogen atmosphere, heating to 1000-1050 deg.C at 1-2 deg.C/min, and heating to 1100-1200 deg.C at 2-4 deg.C/min.
The heat-resistant high-strength low-expansion ceramic is used for kitchen utensils.
The technical effects of the invention are as follows:
according to the invention, after ball milling of raw materials, the raw materials are pretreated by a plasma spray gun, powder components can be modified into a sphere-like state with good fluidity, then silica sol is added into the purified slurry to be matched with pugging and ageing treatment, the structure among particles is extremely compact, and the surface of a final ceramic product is smooth by matching with program sintering treatment.
Because spodumene has anisotropic thermal expansion coefficient, the applicant can effectively promote zirconium oxide and tungsten trioxide to be fully dispersed into spodumene by controlling the proportion of the zirconium oxide, the tungsten trioxide and the spodumene and carrying out plasma pretreatment, so that the zirconium oxide and the tungsten trioxide are more uniformly dispersed in microcosmic, then the zirconium tungstate with excellent isotropic negative thermal expansion is generated by matching with program sintering treatment and fully dispersed on the surface of the spodumene after transformation, and then the zirconium tungstate is not decomposed in the cooling process and has extremely low expansion coefficient, and meanwhile, the zirconium tungstate has uniformly distributed stress after quenching treatment under the matching action of activated graphite, so that the crack growth of materials is effectively prevented, and the product has excellent compression performance.
Wherein the flake graphite is immersed in strong acid for activation, and then reacts with ethylenediamine and methyl acrylate to form activated graphite with a polyamide amine structure grafted on the surface. The activated graphite is dispersed in the premix, so that not only can the lubrication function be achieved, the grinding process is promoted to be full, but also the skeleton structure of the dendritic polyamidoamine can play a role in connection in the ceramic structure in the subsequent temperature programming sintering process, different firing shrinkage components can be limited by the carbonized dendritic network structure, and the dendritic network carbon structure is further formed in the ceramic structure, so that the compressive strength is effectively enhanced.
The blank is subjected to vacuum freeze drying, so that moisture in the blank can be removed in a sublimation mode, interaction force between activated graphite and other components in a system is effectively reduced, a uniform pore structure is formed in the blank, meanwhile, on the basis of enhancing the compressive strength of the system after sintering, the porosity in the ceramic structure can be increased after the activated graphite is carbonized, and when thermal shock is received, crack formation and expansion are effectively inhibited.
The interface between the graphite phase and the ceramic phase is well combined, and the product of the silica sol after sintering can be doped with the alpha-alumina to form the mullite phase, so that the mutual penetration, the mutual penetration and the mutual support fully play the integral strengthening effect, and the silica sol has low expansion coefficient, heat resistance and excellent compression performance.
The product of the invention has the advantages of strong mechanical property, high regularity, more uniform heating, difficult deformation, beautiful appearance, practicability, and suitability for dry burning on open fire, and is safer and longer in service life due to the unglazed treatment.
The invention not only greatly reduces the addition amount of spodumene and controls the water absorption to be 1-1.5 percent, but also has no crack after heat exchange for 10 times in water with the thermal shock resistance of 1000-5 ℃, has extremely high heat resistance degree and is convenient for popularization and use.
Drawings
FIG. 1 is a graph showing the bulk density, apparent porosity and relative density of the ceramics obtained in example 3, example 8, comparative example 1 and comparative example 2.
FIG. 2 is a graph showing the thermal expansion coefficients of the ceramics obtained in example 3, example 8, comparative example 1, and comparative example 2.
FIG. 3 is a graph showing the compressive strength of the ceramics obtained in example 3, example 8, comparative example 1, and comparative example 2.
FIG. 4 is a graph showing the water absorption and thermal shock resistance of the ceramics obtained in example 3, example 8, comparative example 1, and comparative example 2.
Detailed Description
The invention is further illustrated below in connection with specific embodiments.
Example 1
The heat-resistant high-strength low-expansion ceramic comprises the following raw materials in percentage by mass: 25% of Guizhou soil, 15% of Zhangzhou soil, 3% of Xinyang soil, 10% of Datong soil, 8% of quartz powder, 4% of waste porcelain powder, 2% of talcum powder and the balance spodumene.
The preparation method of the heat-resistant high-strength low-expansion ceramic comprises the following steps:
i. adding spodumene, guizhou soil, zhangzhou soil, xinyang soil, quartz powder, datong soil, waste porcelain powder and talcum powder into a stirrer, uniformly mixing, adding into a wet ball mill, grinding to a fineness of 800 meshes, sending into a slurry tank to remove iron and ferric oxide, sieving, drying and crushing to obtain a premix;
ii. Adjusting the water content of the premix to 20%, then carrying out vacuum pugging in a vacuum pugging machine with the vacuum degree of 40kPa, ageing for 5 days in an environment with the temperature of 15 ℃ and the relative humidity of 45RH%, and then carrying out vacuum pugging in the vacuum pugging machine with the vacuum degree of 20kPa again, and forming to obtain a blank;
iii, drying the blank to automatically remove the film, vacuum freeze-drying to water content of 1%, putting into absolute ethyl alcohol, ultrasonically cleaning for 5min, wherein the ultrasonic frequency is 5kHz, the ultrasonic power is 300W, polishing to be round, inspecting the blank by clear water, and drying in a blank warehouse at 20 ℃ to obtain green blanks;
and iv, kiln filling the green blank, heating to 500 ℃ at a speed of 1 ℃/min under nitrogen atmosphere, preserving heat for 20min, heating to 1000 ℃ at a speed of 1 ℃/min, preserving heat for 1h, heating to 1100 ℃ at a speed of 2 ℃/min, sintering for 10h, maintaining sintering air pressure at 0.12MPa in the sintering process, and quenching in mineral oil to room temperature to obtain the heat-resistant high-strength low-expansion ceramic.
Example 2
The heat-resistant high-strength low-expansion ceramic comprises the following raw materials in percentage by mass: 15% of Guizhou soil, 25% of Zhangzhou soil, 7% of Xinyang soil, 14% of Datong soil, 12% of quartz powder, 6% of waste porcelain powder, 4% of talcum powder and the balance of spodumene.
The preparation method of the heat-resistant high-strength low-expansion ceramic comprises the following steps:
i. adding spodumene, guizhou soil, zhangzhou soil, xinyang soil, quartz powder, datong soil, waste porcelain powder and talcum powder into a stirrer, uniformly mixing, adding into a wet ball mill, grinding to 1000 meshes, sending into a slurry tank to remove iron and ferric oxide, sieving, drying and crushing to obtain premix;
ii. Adjusting the water content of the premix to 28%, then carrying out vacuum pugging in a vacuum pugging machine with the vacuum degree of 80kPa, then aging for 10 days in an environment with the temperature of 22 ℃ and the relative humidity of 52RH%, and then sending into the vacuum pugging machine with the vacuum degree of 50kPa again for vacuum pugging, and forming to obtain a blank;
iii, drying the blank to automatically remove the film, vacuum freeze-drying to water content of 1.5%, putting into absolute ethyl alcohol, ultrasonically cleaning for 15min, wherein the ultrasonic frequency is 12kHz, the ultrasonic power is 400W, polishing to be round, inspecting the blank by clear water, and drying in a blank warehouse at 30 ℃ to obtain green blanks;
and iv, kiln filling the green blank, heating to 560 ℃ at a speed of 5 ℃/min under nitrogen atmosphere, preserving heat for 30min, heating to 1050 ℃ at a speed of 2 ℃/min, preserving heat for 2h, heating to 1200 ℃ at a speed of 4 ℃/min, sintering for 20h, maintaining sintering air pressure at 0.15MPa in the sintering process, and quenching in mineral oil to room temperature to obtain the heat-resistant high-strength low-expansion ceramic.
Example 3
The heat-resistant high-strength low-expansion ceramic comprises the following raw materials in percentage by mass: 20% of Guizhou soil, 20% of Zhangzhou soil, 5% of Xinyang soil, 12% of Datong soil, 10% of quartz powder, 5% of waste porcelain powder, 3% of talcum powder and the balance spodumene.
The preparation method of the heat-resistant high-strength low-expansion ceramic comprises the following steps:
i. adding spodumene, guizhou soil, zhangzhou soil, xinyang soil, quartz powder, datong soil, waste porcelain powder and talcum powder into a stirrer, uniformly mixing, adding into a wet ball mill, grinding to a fineness of 900 meshes, sending into a slurry tank to remove iron and ferric oxide, sieving, drying and crushing to obtain a premix;
ii. Adjusting the water content of the premix to 24%, then carrying out vacuum pugging in a vacuum pugging machine with the vacuum degree of 60kPa, ageing for 7 days in an environment with the temperature of 18 ℃ and the relative humidity of 48RH%, and then carrying out vacuum pugging in the vacuum pugging machine with the vacuum degree of 35kPa again, and forming to obtain a blank;
iii, drying the blank to automatically remove the film, vacuum freeze-drying to water content of 1.2%, putting into absolute ethyl alcohol, ultrasonically cleaning for 10min, wherein the ultrasonic frequency is 8kHz, the ultrasonic power is 350W, polishing to be round, inspecting the blank by clear water, and drying in a blank warehouse at 25 ℃ to obtain green blanks;
and iv, kiln filling the green blank, heating to 530 ℃ at a speed of 3 ℃/min under nitrogen atmosphere, preserving heat for 25min, heating to 1030 ℃ at a speed of 1.5 ℃/min, preserving heat for 1.5h, heating to 1150 ℃ at a speed of 3 ℃/min, sintering for 15h, maintaining sintering air pressure at 0.14MPa in the sintering process, and quenching in mineral oil to room temperature to obtain the heat-resistant high-strength low-expansion ceramic.
Example 4
The heat-resistant high-strength low-expansion ceramic comprises the following raw materials in percentage by mass: 18% of Guizhou soil, 22% of Zhangzhou soil, 4% of Xinyang soil, 13% of Datong soil, 9% of quartz powder, 5.5% of waste porcelain powder, 2.5% of talcum powder, 4% of activated graphite, 2% of alpha-alumina, 1.8% of zirconia, 1.5% of tungsten trioxide, 2.5% of silica sol, 1.2% of A Ke Weier and the balance spodumene.
The activated graphite is prepared by the following steps: 15kg of 30-mesh flake graphite was immersed in 50kg of a mixed acid (the mixed acid consists of sulfuric acid having a concentration of 1.7mol/L and nitric acid having a concentration of 14 mol/L) for 2 hours, washed with water, dried, added to 50kg of methanol, 3kg of ethylenediamine was added thereto in a stirred state, stirred for 1 hour, 3kg of methyl acrylate was added thereto in a nitrogen atmosphere, stirred for 20 hours at a temperature of 40℃and distilled under reduced pressure to obtain activated graphite.
The preparation method of the heat-resistant high-strength low-expansion ceramic comprises the following steps:
s1, adding spodumene, guizhou soil, zhangzhou soil, xinyang soil, quartz powder, datong soil, waste porcelain powder, talcum powder and activated graphite into a stirrer, uniformly mixing, adding into a wet ball mill, grinding to a fineness of 850 meshes, sending into a slurry tank to remove iron and ferric oxide, sieving, drying and crushing to obtain a premix;
s2, uniformly mixing premix, alpha-alumina, zirconia and tungsten trioxide, and then spraying out after pretreatment by a plasma spray gun, wherein the parameters of the spray gun are as follows: argon is 30L/min, hydrogen is 5L/min, the voltage is 80V, and the current is 600A, so that purified slurry is obtained;
s3, adding the purified slurry into a mud filter to dehydrate until the water content is 28%, adding silica sol and A Ke Weier A, stirring uniformly, then carrying out vacuum pugging in a vacuum pugging machine with the vacuum degree of 50kPa, ageing for 8 days in an environment with the temperature of 20 ℃ and the relative humidity of 46RH%, and then carrying out vacuum pugging in the vacuum pugging machine with the vacuum degree of 30kPa again, and forming to obtain a blank;
s4, drying the blank to automatically release the film, vacuum freeze-drying to water content of 1.3%, putting into absolute ethyl alcohol, ultrasonically cleaning for 8min, wherein the ultrasonic frequency is 10kHz, the ultrasonic power is 330W, polishing to be round, inspecting the blank by clear water, and drying in a blank warehouse at 28 ℃ to obtain green blanks;
s5, kiln-filling green blanks, heating to 540 ℃ at a speed of 2 ℃/min under nitrogen atmosphere, preserving heat for 22min, heating to 1020 ℃ at a speed of 1.7 ℃/min, preserving heat for 1.7h, heating to 1180 ℃ at a speed of 2.5 ℃/min, sintering for 13h, maintaining sintering air pressure at 0.14MPa in the sintering process, and quenching in mineral oil to room temperature to obtain the heat-resistant high-strength low-expansion ceramic.
Example 5
The heat-resistant high-strength low-expansion ceramic comprises the following raw materials in percentage by mass: 22% of Guizhou soil, 18% of Zhangzhou soil, 6% of Xinyang soil, 11% of Datong soil, 11% of quartz powder, 4.5% of waste porcelain powder, 3.5% of talcum powder, 2% of activated graphite, 4% of alpha-alumina, 1.2% of zirconia, 2.5% of tungsten trioxide, 1.5% of silica sol, 1.8% of A Ke Weier A and the balance spodumene.
The activated graphite is prepared by the following steps: 5kg of 30-mesh flake graphite is added into 100kg of mixed acid (the mixed acid consists of sulfuric acid with the concentration of 1.5mol/L and nitric acid with the concentration of 16 mol/L) to be soaked for 1h, washed with water, dried, added into 100kg of methanol, added with 1kg of ethylenediamine under stirring, stirred for 2h, added with 1kg of methyl acrylate under nitrogen, stirred for 10h at the temperature of 50 ℃ under regulation, and distilled under reduced pressure to obtain activated graphite.
The preparation method of the heat-resistant high-strength low-expansion ceramic comprises the following steps:
s1, adding spodumene, guizhou soil, zhangzhou soil, xinyang soil, quartz powder, datong soil, waste porcelain powder, talcum powder and activated graphite into a stirrer, uniformly mixing, adding into a wet ball mill, grinding to 950 meshes, sending into a slurry tank to remove iron and ferric oxide, sieving, drying and crushing to obtain a premix;
s2, uniformly mixing premix, alpha-alumina, zirconia and tungsten trioxide, and then spraying out after pretreatment by a plasma spray gun, wherein the parameters of the spray gun are as follows: argon is 20L/min, hydrogen is 15L/min, the voltage is 70V, and the current is 700A, so that purified slurry is obtained;
s3, adding the purified slurry into a mud filter to dehydrate until the water content is 20%, adding silica sol and A Ke Weier A, stirring uniformly, then carrying out vacuum pugging in a vacuum pugging machine with the vacuum degree of 70kPa, ageing for 6 days in an environment with the temperature of 16 ℃ and the relative humidity of 50RH%, and then carrying out vacuum pugging in a vacuum pugging machine with the vacuum degree of 40kPa again, and forming to obtain a blank;
s4, drying the blank to automatically release the film, vacuum freeze-drying to water content of 1.1%, putting into absolute ethyl alcohol, ultrasonically cleaning for 12min, wherein the ultrasonic frequency is 6kHz, the ultrasonic power is 370W, polishing to be round, inspecting the blank by clear water, and drying in a blank warehouse at 22 ℃ to obtain green blanks;
s5, kiln-filling green blanks, heating to 520 ℃ at a speed of 4 ℃/min under nitrogen atmosphere, preserving heat for 28min, heating to 1040 ℃ at a speed of 1.3 ℃/min, preserving heat for 1.3h, heating to 1120 ℃ at a speed of 3.5 ℃/min, sintering for 17h, maintaining sintering air pressure at 0.13MPa in the sintering process, and quenching in mineral oil to room temperature to obtain the heat-resistant high-strength low-expansion ceramic.
Example 6
The heat-resistant high-strength low-expansion ceramic comprises the following raw materials in percentage by mass: 19% of Guizhou soil, 21% of Zhangzhou soil, 4.5% of Xinyang soil, 12.5% of Datong soil, 9.5% of quartz powder, 5.2% of waste porcelain powder, 2.8% of talcum powder, 3.5% of activated graphite, 2.5% of alpha-alumina, 1.6% of zirconia, 1.8% of tungsten trioxide, 2.2% of silica sol, 1.4% of A Ke Weier and the balance spodumene.
The activated graphite is prepared by the following steps: adding 12kg of 30-mesh flake graphite into 70kg of mixed acid (the mixed acid consists of sulfuric acid with the concentration of 1.65mol/L and nitric acid with the concentration of 14.5 mol/L), immersing for 1.7h, washing with water, drying, adding into 60kg of methanol, adding 2.5kg of ethylenediamine into the mixture under stirring, stirring for 1.3h, adding 2.5kg of methyl acrylate under nitrogen atmosphere, regulating the temperature to 43 ℃ and stirring for 18h, and carrying out reduced pressure distillation to obtain the activated graphite.
The preparation method of the heat-resistant high-strength low-expansion ceramic comprises the following steps:
s1, adding spodumene, guizhou soil, zhangzhou soil, xinyang soil, quartz powder, datong soil, waste porcelain powder, talcum powder and activated graphite into a stirrer, uniformly mixing, adding into a wet ball mill, grinding to the fineness of 880 meshes, sending into a slurry pond to remove iron and ferric oxide, sieving, drying and crushing to obtain a premix;
s2, uniformly mixing premix, alpha-alumina, zirconia and tungsten trioxide, and then spraying out after pretreatment by a plasma spray gun, wherein the parameters of the spray gun are as follows: argon is 28L/min, hydrogen is 8L/min, the voltage is 77V, and the current is 620A, so as to obtain purified slurry;
s3, adding the purified slurry into a mud filter to dehydrate until the water content is 26%, adding silica sol and A Ke Weier A, stirring uniformly, then carrying out vacuum pugging in a vacuum pugging machine with the vacuum degree of 55kPa, ageing for 7.5 days in an environment with the temperature of 19 ℃ and the relative humidity of 47RH%, and then carrying out vacuum pugging in a vacuum pugging machine with the vacuum degree of 33kPa again, and forming to obtain a blank;
s4, drying the blank to automatically release the film, vacuum freeze-drying to the water content of 1.25%, putting into absolute ethyl alcohol, ultrasonically cleaning for 9min, wherein the ultrasonic frequency is 9kHz, the ultrasonic power is 340W, polishing to be round, checking the blank with clear water, and drying in a blank warehouse at 26 ℃ to obtain a green blank;
s5, kiln-filling green blanks, heating to 535 ℃ at a speed of 2.5 ℃/min under nitrogen atmosphere, preserving heat for 24min, heating to 1025 ℃ at a speed of 1.6 ℃/min, preserving heat for 1.6h, heating to 1160 ℃ at a speed of 2.8 ℃/min, sintering for 14h, maintaining sintering air pressure at 0.137MPa in the sintering process, and quenching in mineral oil to room temperature to obtain the heat-resistant high-strength low-expansion ceramic.
Example 7
The heat-resistant high-strength low-expansion ceramic comprises the following raw materials in percentage by mass: 21% of Guizhou soil, 19% of Zhangzhou soil, 5.5% of Xinyang soil, 11.5% of Datong soil, 10.5% of quartz powder, 4.8% of waste porcelain powder, 3.2% of talcum powder, 2.5% of activated graphite, 3.5% of alpha-alumina, 1.4% of zirconia, 2.2% of tungsten trioxide, 1.8% of silica sol, 1.6% of A Ke Weier and the balance spodumene.
The activated graphite is prepared by the following steps: 8kg of 30-mesh flake graphite was immersed in 90kg of a mixed acid (the mixed acid is composed of sulfuric acid having a concentration of 1.55mol/L and nitric acid having a concentration of 15.5 mol/L) for 1.3 hours, washed with water, dried, added to 80kg of methanol, 1.5kg of ethylenediamine was added thereto under stirring for 1.7 hours, 1.5kg of methyl acrylate was added under nitrogen atmosphere, stirred at a temperature of 47℃for 12 hours, and distilled under reduced pressure to obtain activated graphite.
The preparation method of the heat-resistant high-strength low-expansion ceramic comprises the following steps:
s1, adding spodumene, guizhou soil, zhangzhou soil, xinyang soil, quartz powder, datong soil, waste porcelain powder, talcum powder and activated graphite into a stirrer, uniformly mixing, adding into a wet ball mill, grinding to a fineness of 920 meshes, sending into a slurry tank to remove iron and ferric oxide, sieving, drying and crushing to obtain a premix;
s2, uniformly mixing premix, alpha-alumina, zirconia and tungsten trioxide, and then spraying out after pretreatment by a plasma spray gun, wherein the parameters of the spray gun are as follows: argon is 22L/min, hydrogen is 12L/min, the voltage is 73V, and the current is 680A, so that purified slurry is obtained;
s3, adding the purified slurry into a mud filter to dehydrate until the water content is 22%, adding silica sol and A Ke Weier A, stirring uniformly, then carrying out vacuum pugging in a vacuum pugging machine with the vacuum degree of 65kPa, ageing for 6.5 days in an environment with the temperature of 17 ℃ and the relative humidity of 49RH%, and then carrying out vacuum pugging in a vacuum pugging machine with the vacuum degree of 37kPa again, and forming to obtain a blank;
s4, drying the blank to automatically release the film, vacuum freeze-drying to water content of 1.15%, putting into absolute ethyl alcohol, ultrasonically cleaning for 11min, wherein the ultrasonic frequency is 7kHz, the ultrasonic power is 360W, polishing to be round, checking the blank with clear water, and drying in a blank warehouse at 24 ℃ to obtain green blanks;
s5, kiln-loading green blanks, heating to 525 ℃ at a speed of 3.5 ℃/min under nitrogen atmosphere, preserving heat for 26min, heating to 1035 ℃ at a speed of 1.4 ℃/min, preserving heat for 1.4h, heating to 1140 ℃ at a speed of 3.2 ℃/min, sintering for 16h, maintaining sintering air pressure at 0.133MPa in the sintering process, and quenching in mineral oil to room temperature to obtain the heat-resistant high-strength low-expansion ceramic.
Example 8
The heat-resistant high-strength low-expansion ceramic comprises the following raw materials in percentage by mass: 20% of Guizhou soil, 20% of Zhangzhou soil, 5% of Xinyang soil, 12% of Datong soil, 10% of quartz powder, 5% of waste porcelain powder, 3% of talcum powder, 3% of activated graphite, 3% of alpha-alumina, 1.5% of zirconia, 2% of tungsten trioxide, 2% of silica sol, 1.5% of A Ke Weier A and the balance spodumene.
The activated graphite is prepared by the following steps: 10kg of 30-mesh flake graphite is added into 80kg of mixed acid (the mixed acid consists of sulfuric acid with the concentration of 1.6mol/L and nitric acid with the concentration of 15 mol/L) to be soaked for 1.5h, washed with water, dried, added into 70kg of methanol, added with 2kg of ethylenediamine under stirring, stirred for 1.5h, added with 1.5-2.5kg of methyl acrylate under nitrogen atmosphere, stirred for 15h at the temperature of 45 ℃ and distilled under reduced pressure to obtain activated graphite.
The preparation method of the heat-resistant high-strength low-expansion ceramic comprises the following steps:
s1, adding spodumene, guizhou soil, zhangzhou soil, xinyang soil, quartz powder, datong soil, waste porcelain powder, talcum powder and activated graphite into a stirrer, uniformly mixing, adding into a wet ball mill, grinding to a fineness of 900 meshes, sending into a slurry pond to remove iron and ferric oxide, sieving, drying and crushing to obtain a premix;
s2, uniformly mixing premix, alpha-alumina, zirconia and tungsten trioxide, and then spraying out after pretreatment by a plasma spray gun, wherein the parameters of the spray gun are as follows: argon is 25L/min, hydrogen is 10L/min, voltage is 75V, and current is 650A, so that purified slurry is obtained;
s3, adding the purified slurry into a mud filter to dehydrate until the water content is 24%, adding silica sol and A Ke Weier A, stirring uniformly, then carrying out vacuum pugging in a vacuum pugging machine with the vacuum degree of 60kPa, ageing for 7 days in an environment with the temperature of 18 ℃ and the relative humidity of 48RH%, and then carrying out vacuum pugging in a vacuum pugging machine with the vacuum degree of 35kPa again, and forming to obtain a blank;
s4, drying the blank to automatically release the film, vacuum freeze-drying to water content of 1.2%, putting into absolute ethyl alcohol, ultrasonically cleaning for 10min, wherein the ultrasonic frequency is 8kHz, the ultrasonic power is 350W, polishing to be round, inspecting the blank by clear water, and drying in a blank warehouse at 25 ℃ to obtain green blanks;
s5, kiln-filling green blanks, heating to 530 ℃ at a speed of 3 ℃/min under nitrogen atmosphere, preserving heat for 25min, heating to 1030 ℃ at a speed of 1.5 ℃/min, preserving heat for 1.5h, heating to 1150 ℃ at a speed of 3 ℃/min, sintering for 15h, maintaining sintering air pressure at 0.135MPa in the sintering process, and quenching in mineral oil to room temperature to obtain the heat-resistant high-strength low-expansion ceramic.
Comparative example 1
The heat-resistant high-strength low-expansion ceramic comprises the following raw materials in percentage by mass: 20% of Guizhou soil, 20% of Zhangzhou soil, 5% of Xinyang soil, 12% of Datong soil, 10% of quartz powder, 5% of waste porcelain powder, 3% of talcum powder, 3% of alpha-alumina, 1.5% of zirconia, 2% of tungsten trioxide, 2% of silica sol, 1.5% of A Ke Weier and the balance spodumene.
The preparation method of the heat-resistant high-strength low-expansion ceramic comprises the following steps:
s1, adding spodumene, guizhou soil, zhangzhou soil, xinyang soil, quartz powder, datong soil, waste porcelain powder and talcum powder into a stirrer, uniformly mixing, adding into a wet ball mill, grinding to a fineness of 900 meshes, sending into a slurry tank to remove iron and ferric oxide, sieving, drying and crushing to obtain a premix;
s2, uniformly mixing premix, alpha-alumina, zirconia and tungsten trioxide, and then spraying out after pretreatment by a plasma spray gun, wherein the parameters of the spray gun are as follows: argon is 25L/min, hydrogen is 10L/min, voltage is 75V, and current is 650A, so that purified slurry is obtained;
s3, adding the purified slurry into a mud filter to dehydrate until the water content is 24%, adding silica sol and A Ke Weier A, stirring uniformly, then carrying out vacuum pugging in a vacuum pugging machine with the vacuum degree of 60kPa, ageing for 7 days in an environment with the temperature of 18 ℃ and the relative humidity of 48RH%, and then carrying out vacuum pugging in a vacuum pugging machine with the vacuum degree of 35kPa again, and forming to obtain a blank;
s4, drying the blank to automatically release the film, vacuum freeze-drying to water content of 1.2%, putting into absolute ethyl alcohol, ultrasonically cleaning for 10min, wherein the ultrasonic frequency is 8kHz, the ultrasonic power is 350W, polishing to be round, inspecting the blank by clear water, and drying in a blank warehouse at 25 ℃ to obtain green blanks;
s5, kiln-filling green blanks, heating to 530 ℃ at a speed of 3 ℃/min under nitrogen atmosphere, preserving heat for 25min, heating to 1030 ℃ at a speed of 1.5 ℃/min, preserving heat for 1.5h, heating to 1150 ℃ at a speed of 3 ℃/min, sintering for 15h, maintaining sintering air pressure at 0.135MPa in the sintering process, and quenching in mineral oil to room temperature to obtain the heat-resistant high-strength low-expansion ceramic.
Comparative example 2
The heat-resistant high-strength low-expansion ceramic comprises the following raw materials in percentage by mass: 20% of Guizhou soil, 20% of Zhangzhou soil, 5% of Xinyang soil, 12% of Datong soil, 10% of quartz powder, 5% of waste porcelain powder, 3% of talcum powder, 3% of alpha-alumina, 1.5% of zirconia, 2% of tungsten trioxide, 2% of silica sol, 1.5% of A Ke Weier and the balance spodumene.
The preparation method of the heat-resistant high-strength low-expansion ceramic comprises the following steps:
(1) Adding spodumene, guizhou soil, zhangzhou soil, xinyang soil, quartz powder, datong soil, waste porcelain powder and talcum powder into a stirrer, uniformly mixing, adding into a wet ball mill, grinding to a fineness of 900 meshes, sending into a slurry tank to remove iron and ferric oxide, sieving, drying and crushing to obtain a premix;
(2) Uniformly mixing premix, alpha-alumina, zirconia, tungsten trioxide and water, adding the mixture into a mud filter for dehydration until the water content is 24%, adding silica sol and A Ke Weier A for uniform stirring, then carrying out vacuum mud refining in a vacuum mud refining machine with the vacuum degree of 60kPa, then carrying out ageing for 7 days in an environment with the temperature of 18 ℃ and the relative humidity of 48RH%, and then carrying out vacuum mud refining in a vacuum mud refining machine with the vacuum degree of 35kPa again, and forming to obtain a blank;
(3) Drying the blank to automatically remove the film, vacuum freeze-drying to water content of 1.2%, placing into absolute ethyl alcohol, ultrasonically cleaning for 10min, wherein the ultrasonic frequency is 8kHz, the ultrasonic power is 350W, polishing to be round, inspecting the blank by clear water, and drying in a blank warehouse at 25 ℃ to obtain green blanks;
(4) Kiln filling the green blank, heating to 530 ℃ at a speed of 3 ℃/min under nitrogen atmosphere, preserving heat for 25min, heating to 1030 ℃ at a speed of 1.5 ℃/min, preserving heat for 1.5h, heating to 1150 ℃ at a speed of 3 ℃/min, sintering for 15h, maintaining sintering air pressure at 0.135MPa in the sintering process, and quenching in mineral oil to room temperature to obtain the heat-resistant high-strength low-expansion ceramic.
The ceramics obtained in example 3, example 8 and comparative examples 1 and 2 were subjected to the following comparative tests:
1. the Archimedes drainage method is adopted to measure the volume density rho (g/cm) of each group of ceramics by referring to GB/T25995-2010 fine ceramic density and apparent porosity test method 3 ) The apparent porosity P and the relative density omega are tested.
As shown in FIG. 1, the volume density of each group has no significant difference (P is more than 0.05), but the apparent porosity and the relative density of the embodiment 8 have significant differences (P is less than 0.05) with the other groups, because the activated graphite is adopted to be compatible with the other raw materials, and the green blank is further increased in the internal porosity of the ceramic structure on the basis of forming uniform pores by vacuum freeze drying in the sintering process, so that the apparent porosity of the embodiment 8 is higher and the relative density is lower. However, as the raw materials are ball-milled and then pretreated by a plasma spray gun, the powder components can be modified into a spheroidic state with good fluidity, and then silica sol is added into the purified slurry to be matched with pugging and ageing treatment, so that the sintering density of the embodiment 8 is still better.
2. Referring to the push rod method of the test method of the thermal expansion coefficient of fine ceramic wire of GB/T16535-2008, the size of a tested sample is 5mm multiplied by 10mm, the test temperature range is 50-770 ℃, and the temperature rising rate is 5 ℃/min. The thermal expansion coefficients of each group of samples were measured using a Setsys Evo TMA model static thermo-mechanical analyzer from setram corporation, france.
As shown in FIG. 2, the average linear thermal expansion coefficient of the ceramic obtained in example 8 is closest to zero and better than that of the other groups, and the applicant believes that the average linear thermal expansion coefficient of the ceramic is due to the fact that by controlling the proportion of zirconium oxide, tungsten trioxide and spodumene and performing plasma pretreatment, the zirconium oxide and the tungsten trioxide can be effectively promoted to be fully dispersed into the spodumene, so that the three are more uniformly dispersed microscopically, then the ceramic is matched with a program sintering treatment to generate excellent isotropic negative thermal expansion zirconium tungstate and fully dispersed onto the surface of the spodumene after transformation, and the quenching treatment can effectively ensure that the zirconium tungstate is not decomposed in the cooling process and has extremely low expansion coefficient; meanwhile, activated graphite is dispersed in the premix, so that the skeleton structure of the dendritic polyamidoamine continuously plays a role in connection in the ceramic structure in the subsequent temperature programming sintering process, and different firing shrinkage components are limited by the carbonized dendritic network structure. The interface between the graphite phase and the ceramic phase is well combined, and the product of the silica sol after sintering can be doped with the alpha-alumina-generated mullite phase, so that the integral strengthening effect is fully exerted through interpenetration, interpenetration and mutual support, and the expansion coefficient is further reduced.
3. Referring to GB/T8489-2006 method for testing the compression strength of fine ceramics, an HY-3080 type electronic universal material tester is adopted to test the compression strength of each group of samples.
The results are shown in fig. 3, and as can be seen from fig. 3: the ceramic obtained in example 8 had the highest compressive strength, which was superior to that of comparative example 1. The applicant believes that: on one hand, the activated graphite is dispersed in the premix, so that the lubrication effect is achieved, the grinding process is promoted to be full, and in the subsequent temperature programming sintering process, the polyamidoamine on the crystalline flake graphite is melted, so that the number and strength of system connection points can be increased, the skeleton structure of the dendritic polyamidoamine is enabled to continue to play a role in connection in the ceramic structure, different firing shrinkage components can be limited by the carbonized dendritic network structure, and the dendritic network structure is further formed in the ceramic structure, so that the compressive strength is effectively enhanced; on the other hand, the interface combination of the graphite phase and the ceramic phase is good, and the product of the silica sol after sintering can be doped with the alpha-alumina-generated mullite phase, so that the mutual penetration, the mutual penetration and the mutual support fully play the role of strengthening the whole body, and the compression performance is excellent.
However, the ceramic obtained in example 8 had a high apparent porosity and had a certain effect on the strength, so that example 8 was slightly superior to comparative example 1.
The compressive strength of the ceramics obtained in comparative examples 1 and 2 is superior to that of example 3, because the zirconium oxide and tungsten trioxide are sufficiently dispersed into spodumene by controlling the ratio of the zirconium oxide to the tungsten trioxide and performing the plasma pretreatment, so that the three are microscopically more uniformly dispersed, and then the ceramics are sintered by a program to generate zirconium tungstate with excellent isotropic negative thermal expansion and sufficiently dispersed on the surface of the spodumene after transformation, and the ceramics have uniformly distributed stress after quenching treatment under the cooperation of activated graphite, thereby effectively preventing crack propagation of materials and having excellent compression performance of products.
4. The water absorption and thermal shock resistance of each group were examined. Thermal shock resistance reference part 3 of the thermal shock resistance test method for YB/T376.3-2004 refractory articles: water quenching-crack determination method, the sample is heated to 1000 ℃, kept for 20min, then immersed in flowing water at 5 ℃ and cooled for 10min. Each time the cold and hot alternation is counted as 1 cycle, the test pieces are placed in the air for 5 minutes after each cycle, whether cracks exist or not is observed, and each group of test pieces are tested until the cracks appear or 20 cycles are stopped.
The results are shown in fig. 4, and as can be seen from fig. 4: the water absorption rate of each group of samples is within 1-1.5%, and the heat-shock-resistant ceramic material is suitable for kitchen ceramic utensils, has no crack after heat exchange for at least 10 times in water with the heat shock resistance of 1000-5 ℃, has extremely high heat resistance degree, and can be used for open flame dry combustion.
The thermal shock resistance of the ceramics obtained in example 8 is that, due to the fact that zirconium tungstate generated by plasma pretreatment is matched with activated graphite, stress is uniformly distributed after quenching treatment of the ceramics, crack growth of materials is effectively prevented, and on the other hand, due to the fact that activated graphite is used as a raw material, the blank is subjected to vacuum freeze drying, a uniform pore structure can be further formed in the blank, and meanwhile crack formation and crack growth are effectively prevented when thermal shock is received.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (10)
1. The heat-resistant high-strength low-expansion ceramic is characterized by comprising the following raw materials in percentage by mass: 15-25% of Guizhou soil, 15-25% of Zhangzhou soil, 3-7% of Xinyang soil, 10-14% of Datong soil, 8-12% of quartz powder, 4-6% of waste porcelain powder, 2-4% of talcum powder and the balance of spodumene.
2. The heat resistant high strength low expansion ceramic according to claim 1, wherein the raw materials further comprise: activated graphite, alpha-alumina, zirconia, tungsten trioxide, silica sol, and ammonium salt type cationic surfactants; the mass ratio of the activated graphite, the alpha-alumina, the zirconia, the tungsten trioxide, the silica sol and the ammonium salt cationic surfactant to the Guizhou soil is 1-5:1-6:1-2:1-3:1-3:1-2:15-25.
3. The heat resistant high strength low expansion ceramic according to claim 2, wherein the activated graphite is prepared by the steps of: soaking flake graphite in mixed acid for 1-2h, washing with water, drying, adding into methanol, adding ethylenediamine into the mixture under stirring, stirring for 1-2h, adding methyl acrylate under nitrogen atmosphere, adjusting temperature to 40-50deg.C, stirring for 10-20h, and distilling under reduced pressure to obtain activated graphite.
4. A heat resistant high strength low expansion ceramic according to claim 3, wherein the mixed acid comprises: sulfuric acid with the concentration of 1.5-1.7mol/L and nitric acid with the concentration of 14-16 mol/L; the mass ratio of the flake graphite to the methyl acrylate is 5-15:1-3.
5. A method for producing the heat-resistant high-strength low-expansion ceramic according to any one of claims 2 to 4, comprising the steps of:
s1, uniformly mixing spodumene, guizhou soil, zhangzhou soil, xinyang soil, quartz powder, datong soil, waste porcelain powder, talcum powder and activated graphite, then ball-milling, removing iron and ferric oxide, sieving, drying and crushing to obtain premix;
s2, uniformly mixing premix, alpha-alumina, zirconia and tungsten trioxide, and then spraying out to obtain purified slurry after pretreatment by a plasma spray gun;
s3, adding the purified slurry into a mud filter for dehydration, adding silica sol and ammonium salt cationic surfactant, stirring uniformly, then carrying out vacuum pugging in a vacuum pugging machine with the vacuum degree of 40-80kPa, then ageing for 5-10 days in an environment with the temperature of 15-22 ℃ and the relative humidity of 45-52RH%, and then feeding into a vacuum pugging machine with the vacuum degree of 20-50kPa again for vacuum pugging, and forming to obtain a blank;
s4, drying the blank to automatically release the film, vacuum freeze-drying to the water content of 1-1.5%, ultrasonic cleaning with absolute ethyl alcohol for 5-15min, polishing to be round, checking the blank, and drying in a blank warehouse at 20-30 ℃ to obtain green blank;
s5, kiln-loading green blanks, heating to 500-560 ℃ under nitrogen atmosphere, preserving heat for 20-30min, heating to 1000-1050 ℃, preserving heat for 1-2h, heating to 1100-1200 ℃ and sintering for 10-20h, maintaining sintering air pressure at 0.12-0.15MPa in the sintering process, and quenching in mineral oil to room temperature to obtain the heat-resistant high-strength low-expansion ceramic.
6. The method for producing a heat-resistant high-strength low-expansion ceramic according to claim 5, wherein in S1, the fine particles are ball-milled to 800 to 1000 mesh.
7. The method for producing a heat-resistant high-strength low-expansion ceramic according to claim 5, wherein in S2, the parameters of the plasma torch are as follows: argon is 20-30L/min, hydrogen is 5-15L/min, voltage is 70-80V, and current is 600-700A.
8. The method for producing a heat-resistant high-strength low-expansion ceramic according to claim 5, wherein in S4, the ultrasonic frequency is 5 to 12kHz and the ultrasonic power is 300 to 400W.
9. The method for producing a heat-resistant high-strength low-expansion ceramic according to claim 5, wherein the specific temperature rising rate in S5 is as follows: heating to 500-560 deg.C at 1-5 deg.C/min under nitrogen atmosphere, heating to 1000-1050 deg.C at 1-2 deg.C/min, and heating to 1100-1200 deg.C at 2-4 deg.C/min.
10. A heat resistant high strength low expansion ceramic as claimed in any of claims 1 to 4 for use in kitchen ware.
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