CN116924785A - High-performance ceramic sagger and preparation method thereof - Google Patents
High-performance ceramic sagger and preparation method thereof Download PDFInfo
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- CN116924785A CN116924785A CN202310923392.8A CN202310923392A CN116924785A CN 116924785 A CN116924785 A CN 116924785A CN 202310923392 A CN202310923392 A CN 202310923392A CN 116924785 A CN116924785 A CN 116924785A
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- cordierite
- mullite
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- 239000000919 ceramic Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 82
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims abstract description 58
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 58
- 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 claims abstract description 57
- 239000000463 material Substances 0.000 claims abstract description 55
- 229910052878 cordierite Inorganic materials 0.000 claims abstract description 53
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000002994 raw material Substances 0.000 claims abstract description 29
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 22
- 239000011029 spinel Substances 0.000 claims abstract description 22
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 15
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 15
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims description 51
- 239000003607 modifier Substances 0.000 claims description 34
- 238000003756 stirring Methods 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 18
- 238000005245 sintering Methods 0.000 claims description 18
- 238000009826 distribution Methods 0.000 claims description 16
- 238000010304 firing Methods 0.000 claims description 16
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 13
- 229920001353 Dextrin Polymers 0.000 claims description 13
- 239000004375 Dextrin Substances 0.000 claims description 13
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 13
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 13
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 13
- 235000019425 dextrin Nutrition 0.000 claims description 13
- 230000008569 process Effects 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 12
- 238000005507 spraying Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000000748 compression moulding Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 6
- 230000005484 gravity Effects 0.000 claims description 5
- 238000002715 modification method Methods 0.000 claims description 5
- 238000012216 screening Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims 1
- 230000035939 shock Effects 0.000 abstract description 30
- 230000007797 corrosion Effects 0.000 abstract description 27
- 238000005260 corrosion Methods 0.000 abstract description 27
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 9
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 9
- 238000005516 engineering process Methods 0.000 abstract description 7
- 230000002035 prolonged effect Effects 0.000 abstract description 7
- 229920006316 polyvinylpyrrolidine Polymers 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- 230000002195 synergetic effect Effects 0.000 description 6
- 230000006835 compression Effects 0.000 description 5
- 238000007906 compression Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 239000007774 positive electrode material Substances 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 239000010405 anode material Substances 0.000 description 3
- 238000010835 comparative analysis Methods 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 229910052744 lithium 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
- 230000008859 change Effects 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 239000011362 coarse particle Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 206010067482 No adverse event Diseases 0.000 description 1
- PSMHQAOEOARJDH-UHFFFAOYSA-L [Co]=O.C([O-])([O-])=O.[Li+].[Li+] Chemical compound [Co]=O.C([O-])([O-])=O.[Li+].[Li+] PSMHQAOEOARJDH-UHFFFAOYSA-L 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- LBFUKZWYPLNNJC-UHFFFAOYSA-N cobalt(ii,iii) oxide Chemical compound [Co]=O.O=[Co]O[Co]=O LBFUKZWYPLNNJC-UHFFFAOYSA-N 0.000 description 1
- 238000012669 compression test Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000011549 displacement method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910052566 spinel group Inorganic materials 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 238000005303 weighing Methods 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
- 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
- C04B35/16—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 silicates other than clay
- C04B35/18—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 silicates other than clay rich in aluminium oxide
- C04B35/185—Mullite 3Al2O3-2SiO2
-
- 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
- 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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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D5/00—Supports, screens, or the like for the charge within the furnace
- F27D5/0006—Composite supporting structures
- F27D5/0012—Modules of the sagger or setter type; Supports built up from them
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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
- 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
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- 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
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
- C04B2235/3222—Aluminates other than alumino-silicates, e.g. spinel (MgAl2O4)
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- 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
- C04B2235/3481—Alkaline earth metal alumino-silicates other than clay, e.g. cordierite, beryl, micas such as margarite, plagioclase feldspars such as anorthite, zeolites such as chabazite
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- 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
- C04B2235/349—Clays, e.g. bentonites, smectites such as montmorillonite, vermiculites or kaolines, e.g. illite, talc or sepiolite
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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
- C04B2235/6567—Treatment time
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- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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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
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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
Abstract
The application relates to the technical field of lithium ion batteries, in particular to a high-performance ceramic sagger and a preparation method thereof. The high-performance ceramic sagger comprises the following raw materials in parts by weight: 10-30 parts of cordierite, 10-20 parts of mullite, 10-40 parts of metazate, 10-40 parts of alumina and 10-20 parts of kaolin; through the mode of using fine materials to wrap modified aggregate, cordierite and mullite with coarser particles are used as aggregate, spinel and alumina with better corrosion resistance are used as fine materials while thermal shock resistance of the sagger is guaranteed, and the fine materials with better corrosion resistance are wrapped on the surface of the modified aggregate with better thermal shock resistance by using a wrapping technology, so that the obtained sagger has both thermal stability and excellent corrosion resistance, and the service life of the sagger is prolonged.
Description
Technical Field
The application relates to the technical field of lithium ion batteries, in particular to a high-performance ceramic sagger and a preparation method thereof.
Background
Cordierite-mullite ceramics are widely used as kiln furniture at present, such as hollow sheds and upright posts for sintering sanitary wares, such as saggers and crucibles for calcining various chemical raw materials, fine ceramic materials, magnetic materials and semiconductor materials; particularly in the lithium battery industry which is used as a new energy source and rapidly developed, the lithium salt of the positive electrode material is required to be calcined, the demand of the used cordierite-mullite sagger is very large, however, the ceramic sagger which is used at present uses a large amount of cordierite and mullite for the purpose of considering the heat stability, but the service life of the ceramic sagger is obviously influenced due to the fact that the corrosion resistance of the cordierite and the mullite is not high, the problem of insufficient thermal shock resistance and corrosion resistance exists in the sagger material used for firing lithium cobaltate, the service life of the sagger is limited, the use of the conventional ceramic sagger of lithium cobaltate is basically only 14 times, and therefore, the development of the high-performance ceramic sagger with longer service life is required.
Disclosure of Invention
In order to improve the service life of the ceramic sagger, the application provides the high-performance ceramic sagger and the preparation method thereof, and fine materials with better corrosion resistance are wrapped on the surface of modified aggregate with better thermal shock resistance by utilizing a wrapping technology, so that the service life of the sagger is improved.
In a first aspect, the present application provides a high performance ceramic sagger, which adopts the following technical scheme:
the high-performance ceramic sagger comprises the following raw materials in parts by weight: 10-30 parts of cordierite, 10-20 parts of mullite, 10-40 parts of metazate, 10-40 parts of alumina and 10-20 parts of kaolin; the particle size of the cordierite is 1-3 mm, the particle size of the mullite is 1-2 mm, the particle size of the metaaluminate spinel is 15-44 microns, the particle size of the alumina is 6-30 microns, wherein the spinel and the alumina are fine materials, the cordierite and the mullite are aggregate, the aggregate is modified aggregate, and the fine materials are coated on the surface of the modified aggregate.
Preferably, the high-performance ceramic sagger comprises the following raw materials in parts by weight: 18-22 parts of cordierite, 15-17 parts of mullite, 25-30 parts of metazate, 25-30 parts of alumina and 12-14 parts of kaolin; the particle size of the cordierite is 1-3 mm, the particle size of the mullite is 1-2 mm, the particle size of the metaaluminate spinel is 15-44 microns, and the particle size of the alumina is 6-30 microns, wherein the spinel and the alumina are fine materials, the cordierite and the mullite are aggregate, the aggregate is modified aggregate, and the fine materials are coated on the surface of the modified aggregate.
Through adopting above-mentioned technical scheme, cordierite: as aggregate, the mortar has higher thermal shock resistance. Cordierite particles are relatively coarse, have relatively good thermal stability, and can withstand relatively high temperature changes without cracking. In addition, cordierite can also increase the strength and hardness of the sagger and improve the durability thereof. Mullite: also as aggregate, provides thermal shock resistance to the sagger. The mullite has good thermal stability and wear resistance, and can resist high-temperature impact and wear, so that the service life of the sagger is prolonged. Metazalepite: as fine materials, the corrosion resistance is good. The aluminum spinelle surface is coated on the modified aggregate, so that the aluminum spinelle has a protective effect, reduces the sensitivity of the sagger to corrosive environments and improves the corrosion resistance of the sagger. Alumina: also as fine material, has excellent corrosion resistance. The synergy of these materials in the sagger preparation process is mainly characterized in the following aspects: synergistic effect of thermal shock resistance: the modified aggregate has better thermal shock resistance, and can bear temperature change and thermal shock without cracking. Meanwhile, the metaaluminate spinel and the alumina are used as fine materials, and gaps among the modified aggregates can be filled in a mode of coating the surfaces of the modified aggregate particles, so that the density and compactness of the ceramic sagger are increased. The combination can effectively improve the thermal shock resistance of the sagger, reduce the stress generated by the thermal expansion difference, and ensure that the sagger has better thermal stability. Synergistic effect of corrosion resistance: the metaaluminate spinel and the alumina are used as fine materials, and have excellent corrosion resistance. The aluminum metaspinel surface is coated on the modified cordierite and modified mullite particles, so that a protective layer can be formed, and the corrosion of corrosive medium to the sagger is reduced. In addition, the aluminum oxide can fill gaps among aggregate particles, so that the compactness of the sagger is improved, and the corrosion resistance is further improved.
Preferably, the modification method of the modified aggregate comprises the steps of adding cordierite with the particle size of 6-30 microns and mullite with the particle size of 1-2 mm into a high-speed stirrer for stirring according to parts by weight, spraying a modifier solution in the stirring process, and stirring until the cordierite and mullite particles uniformly wrap the modifier, thus obtaining the modified aggregate.
Preferably, the modifier is a composition of carboxymethyl cellulose, polyvinylpyrrolidone k30 and dextrin according to a mass ratio of 3:1:1, and the mass concentration of the modifier solution is 25-35g/L.
Preferably, the spraying mass of the modifier solution is 4.5% of the total mass of cordierite and mullite.
Preferably, the stirring process parameters are that the stirring speed is 300-500 rpm and the stirring time is 5-10 minutes.
Through adopting above-mentioned technical scheme, accurate control carboxymethyl cellulose, polyvinylpyrrolidone k30 and dextrin's composition is modified cordierite and mullite, promotes the cladding of follow-up fine material metaaluminate spinel and aluminium oxide more even at its granule surface, also has fine bonding strength simultaneously. These materials have the following functions: carboxymethyl cellulose: carboxymethyl cellulose is a water-soluble polymer with better adhesiveness and reinforcement. Polyvinylpyrrolidone k30: polyvinylpyrrolidone k30 is a high molecular polymer with better plasticity and formability. Dextrin: dextrin is a natural polysaccharide with good adhesiveness and viscosity-reducing property. The modifier is carboxymethyl cellulose, polyvinylpyrrolidone k30 and dextrin, and the composition with the mass ratio of 3:1:1 has a synergistic effect on the modification of cordierite and mullite, so that fine materials can be better wrapped on the surface of aggregate, the wrapped particles are more complete, stronger and better in plasticity, the binding force between the fine materials and the aggregate is stronger, and the subsequent compression molding efficiency and the density and strength of products are improved.
Preferably, the coating method of the fine materials on the surface of the modified aggregate comprises the steps of adding metazate and aluminum oxide into the modified aggregate according to parts by weight, stirring at a stirring speed of 600-800 rpm for 10-20 minutes, and obtaining a mixture A of the fine materials on the surface of the modified aggregate.
Through adopting above-mentioned technical scheme, fine material metaplasia spinel and aluminium oxide more even cladding are at modified aggregate particle surface, also have fine joint strength simultaneously, and in the profiling in-process, these raw materials of different particle diameter are inseparable to be connected each other, have guaranteed in the follow-up use, and modified aggregate is difficult for corroding to obtain high performance long-life ceramic sagger.
In a second aspect, the application provides a preparation method of a high-performance ceramic sagger, which adopts the following technical scheme:
the preparation method of the high-performance ceramic sagger adopts the raw materials of the high-performance ceramic sagger, and comprises the following steps:
s81, mixing: uniformly mixing and screening the mixture A and kaolin according to the parts by weight to obtain a mixture B, wherein the water content in the mixture B is controlled to be less than 5%;
s82, molding: putting the mixed mixture B into a die of a ceramic sagger for compression molding, and then drying; s83, firing: the dried sagger is put into a sintering furnace for sintering treatment, and the sintering process parameters are as follows: the firing temperature is 1340-1360 ℃, the firing heat preservation time is 3-4 hours, the ceramic sagger is cooled to room temperature, and finally the quality is inspected to be qualified, thus obtaining the high-performance ceramic sagger.
Preferably, in the step S81 of mixing, the particle size distribution of the mixture B is: more than 8 meshes are 5-20%,8-10 meshes are 10-30%,10-20 meshes are 10-30%,20-40 meshes are 10-20%,40-60 meshes are 5-15%,60-80 meshes are 5-15%,80-100 meshes are 5-15%, and less than or equal to 35% of 100 meshes.
Preferably, in the step S82 molding, the pressure of the compression molding is 17-20MPa, and the bulk specific gravity of the mixture B is controlled to be more than 150g/100mL.
By adopting the technical scheme, the performance of the sagger is maximally improved by selecting the raw materials with proper proportion and grain size range and utilizing the wrapping technology, and the functions and the synergistic effect among different raw materials, so that the sagger has the characteristics of high performance and long service life. The raw materials with different particle sizes have different characteristics and functions, including the following aspects: thermal shock resistance: the cordierite and the mullite with coarser particles are used as aggregate, so that the thermal shock resistance of the sagger can be improved, namely, the sagger can bear abrupt temperature change and is not easy to break. Corrosion resistance: the spinel and the alumina have better corrosion resistance as fine materials, and can prevent the sagger from being corroded by chemical substances in use. Thermal stability: because the modified aggregate with coarser particles can improve the thermal shock resistance of the sagger, the fine materials can be wrapped on the surface of the modified aggregate by the wrapping technology, so that the thermal stability of the sagger is further enhanced. Service life is as follows: the service life of the sagger can be prolonged due to the excellent corrosion resistance and thermal shock resistance.
In the application, the particle distribution is 5-20% above 8 meshes, 10-30% above 8-10 meshes, 10-30% below 10-20 meshes, 10-20% below 20-40 meshes, 5-15% below 40-60 meshes, 5-15% below 60-80 meshes, 5-15% below 80-100 meshes and less than or equal to 35% below 100 meshes. Through the distribution mode, raw materials with different particle sizes can be fully mixed in raw materials, and a mutually compact arrangement structure can be formed, so that the overall performance of the sagger is improved. The raw materials with different particle sizes can be fully mixed through the specified particle distribution, so that a more uniform raw material mixture is formed. The larger particles (more than 8 meshes) can provide better support and backbone structure, and the strength and stability of the sagger are enhanced. The raw materials with the particles distributed between 8-10 meshes, 10-20 meshes and 20-40 meshes can fill gaps among larger particles, so that the compactness of the sagger is improved. The fine particles with the particle distribution between 40-60 meshes, 60-80 meshes and 80-100 meshes can fill gaps among smaller particles, so that the compactness of the sagger is improved. Finer particles with the particle distribution below 100 meshes can fill the gaps of the whole mixture, further enhance the compactness of the sagger and enable the sagger to have better thermal shock resistance at high temperature. Through the combination of coarse particles and fine particles, the optimal design of the sagger material is realized. Coarse particles can provide skeleton support and thermal shock resistance, while fine particles fill skeleton gaps, so that compactness and corrosion resistance of the sagger are improved. Such synergy can provide the resulting ceramic sagger with high performance and long life characteristics.
Therefore, the raw materials with different particle sizes are jointly acted by adopting the specified particle distribution, so that the thermal shock resistance, corrosion resistance and thermal stability of the sagger are enhanced, the service life of the sagger is further prolonged, and the sagger is used for 48 times.
In summary, the beneficial technical effects of the application are as follows:
1) The method has the advantages that through adopting a mode of wrapping the modified aggregate by using fine materials, adopting coarse cordierite and mullite as the aggregate, ensuring the thermal shock resistance of the sagger, adopting spinel and alumina with better corrosion resistance as the fine materials, and adopting a wrapping technology, wrapping the fine materials with better corrosion resistance on the surface of the modified aggregate with better thermal shock resistance, the obtained sagger can be compatible with thermal stability and can obtain excellent corrosion resistance, so that the service life of the sagger is prolonged;
2) By precisely controlling the particle size distribution of the raw material particles, the compactness of the high-performance ceramic sagger is improved, and the obtained high-performance ceramic sagger has thermal shock resistance, corrosion resistance, thermal stability and service life;
3) The sagger raw material with good thermal shock resistance and corrosion resistance is formed by mixing materials with different particle sizes and components and utilizing a wrapping technology, so that the corrosion resistance of the sagger is improved;
4) The preparation process of the traditional sagger material is improved by adopting a mode of wrapping the modified aggregate with fine materials, so that the sagger has good thermal shock resistance and corrosion resistance. Meanwhile, the service life of the sagger is prolonged by optimizing the material components and the process conditions, and the sagger raw material preparation method provided by the application has the characteristics of simplicity, high efficiency and economy and is applied to industrial production.
Detailed Description
Embodiments of the present application will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only for illustrating the present application and should not be construed as limiting the scope of the present application. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
The high-performance ceramic sagger comprises the following raw materials by mass: 10kg of cordierite, 30kg of mullite, 10kg of metazate, 40kg of alumina and 10kg of kaolin; the particle size of the cordierite is 1-3 mm, the particle size of the mullite is 1-2 mm, the particle size of the metaaluminate spinel is 15-44 microns, the particle size of the alumina is 6-30 microns, wherein the spinel and the alumina are fine materials, the cordierite and the mullite are aggregate, the aggregate is modified aggregate, and the fine materials are coated on the surface of the modified aggregate.
The modification method of the modified aggregate comprises the steps of adding cordierite with particle size of 1-3 mm and mullite with particle size of 1-2 mm into a high-speed stirrer for stirring according to parts by weight, spraying modifier solution in the stirring process, stirring at the stirring speed of 300 rpm for 10 minutes, and obtaining the modified aggregate, wherein the modifier is a composition of carboxymethyl cellulose, polyvinylpyrrolidone k30 and dextrin according to the mass ratio of 3:1:1, the mass concentration of the modifier solution is 25g/L, and the spraying mass of the modifier solution is 4.5% of the total mass of the cordierite and the mullite.
The coating method of the fine materials coated on the surface of the modified aggregate comprises the steps of adding metazate and alumina into the modified aggregate according to parts by weight, stirring at the stirring speed of 600 revolutions per minute for 20 minutes, and obtaining a mixture A of the fine materials coated on the surface of the modified aggregate.
The preparation method of the high-performance ceramic sagger comprises the following steps:
s81, mixing: uniformly mixing and screening the mixture A and kaolin according to the parts by weight to obtain a mixture B, wherein the water content in the mixture B is controlled to be 4.5%, and the particle size distribution of the mixture B is as follows: more than 8 meshes are 5%,8-10 meshes are 10%,10-20 meshes are 30%,20-40 meshes are 20%,40-60 meshes are 5%,60-80 meshes are 5%,80-100 meshes are 5%, and less than 100 meshes are 20%;
s82, molding: placing the mixed mixture B into a die of a ceramic sagger for compression molding, controlling the loose specific gravity of the mixture B to 160g/100mL under the pressure of 17MPa, and then drying;
s83, firing: the dried sagger is put into a sintering furnace for sintering treatment, and the sintering process parameters are as follows: the firing temperature is 1340 ℃, the firing heat preservation time is 3 hours, the ceramic sagger is cooled to room temperature, and finally the quality is inspected to be qualified, thus obtaining the high-performance ceramic sagger.
Example 2
The high-performance ceramic sagger comprises the following raw materials by mass: 30kg of cordierite, 20kg of mullite, 40kg of metazate, 40kg of alumina and 20kg of kaolin; the particle size of the cordierite is 1-3 mm, the particle size of the mullite is 1-2 mm, the particle size of the metaaluminate spinel is 15-44 microns, and the particle size of the alumina is 6-30 microns, wherein the spinel and the alumina are fine materials, the cordierite and the mullite are aggregate, the aggregate is modified aggregate, and the fine materials are coated on the surface of the modified aggregate;
the modification method of the modified aggregate comprises the steps of adding cordierite with particle size of 1-3 mm and mullite with particle size of 1-2 mm into a high-speed stirrer for stirring according to parts by weight, spraying modifier solution in the stirring process, stirring at the stirring speed of 500 rpm for 5 minutes, and obtaining the modified aggregate, wherein the modifier is a composition of carboxymethyl cellulose, polyvinylpyrrolidone k30 and dextrin according to the mass ratio of 3:1:1, the mass concentration of the modifier solution is 35g/L, and the spraying mass of the modifier solution is 4.5% of the total mass of the cordierite and the mullite.
The coating method of the fine materials coated on the surface of the modified aggregate comprises the steps of adding metazate and alumina into the modified aggregate according to parts by weight, stirring at a stirring speed of 800 rpm for 10 minutes, and obtaining a mixture A of the fine materials coated on the surface of the modified aggregate.
The preparation method of the high-performance ceramic sagger comprises the following steps:
s81, mixing: uniformly mixing and screening the mixture A and kaolin according to the parts by weight to obtain a mixture B, wherein the water content in the mixture B is controlled to be 3.5%, and the particle size distribution of the mixture B is as follows: more than 8 meshes are 20%,8-10 meshes are 10%,10-20 meshes are 10%,20-40 meshes are 10%,40-60 meshes are 5%,60-80 meshes are 5%,80-100 meshes are 5%, and less than 100 meshes are 35%;
s82, molding: placing the mixed mixture B into a die of a ceramic sagger for compression molding, wherein the compression molding pressure is 20MPa, the loose specific gravity of the mixture B is controlled to be 155g/100mL, and then drying treatment is carried out;
s83, firing: the dried sagger is put into a sintering furnace for sintering treatment, and the sintering process parameters are as follows: the firing temperature is 1360 ℃, the firing time is 4 hours, the ceramic sagger is cooled to room temperature, and finally the quality is inspected to be qualified, thus obtaining the high-performance ceramic sagger.
Example 3
The high-performance ceramic sagger comprises the following raw materials by mass: 20kg of cordierite, 15kg of mullite, 28kg of metazate, 28kg of alumina and 13kg of kaolin; the particle size of the cordierite is 1-3 mm, the particle size of the mullite is 1-2 mm, the particle size of the metaaluminate spinel is 15-44 microns, and the particle size of the alumina is 6-30 microns, wherein the spinel and the alumina are fine materials, the cordierite and the mullite are aggregate, the aggregate is modified aggregate, and the fine materials are coated on the surface of the modified aggregate;
the modification method of the modified aggregate comprises the steps of adding cordierite with the particle size of 6-30 microns and mullite with the particle size of 1-2 mm into a high-speed stirrer for stirring according to parts by weight, spraying modifier solution in the stirring process, stirring at the stirring speed of 400 rpm for 8 minutes, and obtaining the modified aggregate, wherein the modifier is a composition of carboxymethyl cellulose, polyvinylpyrrolidone k30 and dextrin according to the mass ratio of 3:1:1, the mass concentration of the modifier solution is 30g/L, and the spraying mass of the modifier solution is 4.5% of the total mass of the cordierite and the mullite.
The coating method of the fine materials coated on the surface of the modified aggregate comprises the steps of adding metaaluminate spinel and alumina into the modified aggregate according to parts by weight, stirring at the stirring speed of 700 rpm for 15 minutes, and obtaining a mixture A of the fine materials coated on the surface of the modified aggregate.
The preparation method of the high-performance ceramic sagger comprises the following steps:
s81, mixing: uniformly mixing and screening the mixture A and kaolin according to the parts by weight to obtain a mixture B, wherein the water content in the mixture B is controlled to be 4%, and the particle size distribution of the mixture B is as follows: more than 8 meshes are 10%,8-10 meshes are 15%,10-20 meshes are 15%,20-40 meshes are 15%,40-60 meshes are 10%,60-80 meshes are 10%,80-100 meshes are 10%, and less than 100 meshes are 15%;
s82, molding: placing the mixed mixture B into a die of a ceramic sagger for compression molding, wherein the compression molding pressure is 18MPa, the apparent specific gravity of the mixture B is controlled to be 151g/100mL, and then drying treatment is carried out;
s83, firing: the dried sagger is put into a sintering furnace for sintering treatment, and the sintering process parameters are as follows: the firing temperature is 1350 ℃, the firing time is 3.5 hours, the ceramic sagger is cooled to room temperature, and finally the ceramic sagger with high performance is obtained after quality inspection is qualified.
Example 4
The same as in example 3, except that: the material comprises the following raw materials in parts by weight: 18kg of cordierite, 15kg of mullite, 25kg of metazate, 25kg of alumina and 12kg of kaolin.
Example 5
The same as in example 3, except that: the material comprises the following raw materials in parts by weight: 22kg of cordierite, 17kg of mullite, 30kg of metazate, 30kg of alumina and 14kg of kaolin.
Comparative example 1
The same as in example 3, except that: the modifier is carboxymethyl cellulose, the mass concentration of the modifier is 30g/L, and the spraying mass of the modifier is 4.5% of the total mass of cordierite and mullite, namely 5.22kg.
Comparative example 2
The same as in example 3, except that: the modifier is polyvinylpyrrolidone k30, the mass concentration is 30g/L, and the spraying mass is 4.5% of the total mass of cordierite and mullite, namely 5.22kg.
Comparative example 3
The same as in example 3, except that: the modifier is dextrin, the mass concentration of the modifier is 30g/L, and the spraying mass of the modifier is 4.5% of the total mass of cordierite and mullite, namely 5.22kg.
Comparative example 4
The same as in example 3, except that: the modified aggregate of the application is replaced by common cordierite and mullite.
Comparative example 5
The same as in example 3, except that: the particle size of the mixture B is larger, and the particle size distribution is as follows: the content of the particles is 70% above 8 meshes, 20% between 8 and 10 meshes, and 10% below 10 meshes.
Comparative example 6
The same as in example 3, except that: the particle size of the mixture B is smaller, and the particle size distribution is as follows: more than 80 meshes are 10%,80-100 meshes are 20%, and less than 100 meshes are 70%.
Performance testing
The high performance ceramic sagger obtained in examples 1 to 5 and comparative examples 1 to 6 were sampled and tested, respectively, and the test results are shown in table 1.
The stacking density of the sagger can be obtained through measurement and calculation of weight and volume;
the porosity of the sagger was measured by a liquid phase displacement method (automatic TRUE DENSER MAT-7000, available from fagaku corporation);
durability test: the lithium carbonate powder and the cobalt oxide powder were mixed at a high speed in a ball mill for 1 hour in a molar ratio of Li to Co of 1:1. The well-mixed lithium carbonate cobalt oxide mixture was stacked on top of the sagger in parallel (about 5 kg). The sagger filled with the mixture was then placed in a large electric furnace, raised from room temperature to 800 ℃ for 3 hours, and maintained at 800 ℃ for 5 hours, and then the sagger and the lithium ion battery cathode material therein were naturally cooled to 150 ℃ in the large electric furnace (about 6 hours), taken out, and observed. If the positive electrode material of the lithium ion battery can be easily poured out from the sagger, the surface of the sagger has no residues of the positive electrode material of the lithium ion battery, and the sagger has no adverse reactions such as cracking, peeling and the like, the sagger can be regarded as continuously carrying out sintering experiments of the positive electrode material of the lithium ion battery. If the situation that the lithium ion battery anode material cannot be smoothly poured out of the sagger, or a small amount of lithium ion battery anode material remains in the sagger, or the sagger itself is cracked and peeled, the service life of the sagger is considered to be reached, and the sintering experiment of the lithium ion battery anode material is terminated;
water absorption rate: the ceramic sample is completely soaked in water, boiled for 2 hours and soaked for 20 hours, taken out, and the surface moisture is wiped by dry cloth and then weighed. Then placing the sample into an oven for drying until the weight is not changed, weighing, and calculating the water absorption rate, wherein the water absorption rate is = (weight-dry weight after drying)/dry weight multiplied by 100%;
thermal shock resistance test: after the sample is kept at 1100 ℃ for 15min, cooling in water and repeating operation until the sample is cracked or broken, recording the number of thermal shock before damage, and representing the thermal shock resistance of the sagger by the number of thermal shock cycle;
150KPa compression test: and (3) testing the sample at 150KPa on a sample compression resistance tester until the product is destroyed, and recording compression resistance times.
TABLE 1
From the analysis of examples 1 to 5 in Table 1, the high-performance ceramic sagger obtained was prepared to have a bulk density of 2.25 to 2.55g/cm 3 The porosity is 22.5-23.5%, the water absorption is 8.5-9.3%, the durability is 38-48 times, the compression resistance is 29-38 times at 150KPa, the thermal shock resistance is 13-18 times, the fine materials with better corrosion resistance are wrapped on the modified aggregate with better thermal shock resistance to form raw materials by wrapping technology, and the pressed sagger has both thermal stability and excellent corrosion resistance, so that the service life of the sagger is prolonged.
From Table 1, the comparative analysis of example 3 and comparative examples 1-3 shows that the composition of the modifier, carboxymethyl cellulose, polyvinylpyrrolidone k30 and dextrin, which are used as the materials, is used for modifying cordierite and mullite according to the mass ratio of 3:1:1, and compared with the composition of the modifier, which is used for modifying cordierite and mullite by using single carboxymethyl cellulose, polyvinylpyrrolidone k30 or dextrin, the obtained high-performance ceramic sagger has more excellent performance in terms of durability, 150KPa compression resistance, thermal shock cycle number and the like, the composition of the modifier has synergistic effect on the modification of cordierite and mullite, the carboxymethyl cellulose provides the bonding and reinforcing effects, the polyvinylpyrrolidone k30 increases the toughness and plasticity of the materials, and the dextrin increases the bonding force among particles. The synergistic effect of the modifier ensures that the modified cordierite and mullite have better strength, heat resistance, formability and adhesion, and the fine aluminum spinels and the aluminum oxide are more uniformly coated on the particle surfaces of the modified cordierite and the mullite, so that the modified cordierite and the mullite are not corroded in the subsequent use, thereby improving the strength and the service life of the ceramic sagger.
From comparative analysis of example 3 and comparative example 5 or comparative example 6 in table 1, the high performance ceramic sagger obtained by using the particle size distribution of the present application is more excellent in performance than the particle distribution is larger or smaller, and the present application improves the overall performance of the sagger by allowing raw materials of different particle sizes to be sufficiently mixed in raw materials and being able to form a mutually compact arrangement structure.
From Table 1, the comparative analysis of example 3 and comparative example 4 shows that the high-performance ceramic sagger obtained by the modified aggregate of the application has more excellent performances in terms of durability, 150KPa compression resistance, thermal shock resistance cycle number and the like compared with common cordierite and mullite.
The above embodiments are only for illustrating the technical solution of the present application and not for limiting the same, and although the above embodiments specifically illustrate the present application, it should be understood by those skilled in the art that modifications and equivalents may be made to the specific embodiments of the present application without departing from the spirit and scope of the present application, and any modifications and equivalents are intended to be covered by the scope of the claims of the present application.
Claims (10)
1. The high-performance ceramic sagger is characterized by comprising the following raw materials in parts by weight: 10-30 parts of cordierite, 10-20 parts of mullite, 10-40 parts of metazate, 10-40 parts of alumina and 10-20 parts of kaolin; the particle size of the cordierite is 1-3 mm, the particle size of the mullite is 1-2 mm, the particle size of the metaaluminate spinel is 15-44 microns, and the particle size of the alumina is 6-30 microns, wherein the spinel and the alumina are fine materials, the cordierite and the mullite are aggregate, the aggregate is modified aggregate, and the fine materials are coated on the surface of the modified aggregate.
2. The high-performance ceramic sagger is characterized by comprising the following raw materials in parts by weight: 18-22 parts of cordierite, 15-17 parts of mullite, 25-30 parts of metazate, 25-30 parts of alumina and 12-14 parts of kaolin; the particle size of the cordierite is 1-3 mm, the particle size of the mullite is 1-2 mm, the particle size of the metaaluminate spinel is 15-44 microns, and the particle size of the alumina is 6-30 microns, wherein the spinel and the alumina are fine materials, the cordierite and the mullite are aggregate, the aggregate is modified aggregate, and the fine materials are coated on the surface of the modified aggregate.
3. The high-performance ceramic sagger according to claim 1 or 2, wherein the modification method of the modified aggregate is as follows: according to the parts by weight, adding cordierite with the particle size of 1-3 mm and mullite with the particle size of 1-2 mm into a high-speed stirrer for stirring, spraying modifier solution in the stirring process, and stirring until the cordierite and mullite particles are uniformly coated with the modifier, thus obtaining modified aggregate.
4. A high performance ceramic sagger according to claim 3, characterized in that the modifier is a composition of carboxymethyl cellulose, k30 and dextrin according to a mass ratio of 3:1:1, and the mass concentration of the modifier solution is 25-35g/L.
5. A high performance ceramic sagger according to claim 3, characterized in that the modifier solution spray mass is 4.5% of the sum of cordierite and mullite masses.
6. A high performance ceramic sagger according to claim 3, characterized in that the stirring process parameter is stirring speed of 300-500 rpm and stirring time of 5-10 minutes.
7. The high-performance ceramic sagger according to claim 1 or 2, wherein the coating method of the fine materials on the surface of the modified aggregate is characterized in that the metazalcite and the alumina are added into the modified aggregate according to parts by weight and stirred at a speed of 600-800 rpm for 10-20 minutes, so as to obtain the mixture A of the fine materials coated on the surface of the modified aggregate.
8. A method for preparing a high-performance ceramic sagger, which is characterized by adopting the raw materials of the high-performance ceramic sagger according to claim 7, comprising the following steps:
s81, mixing: uniformly mixing and screening the mixture A and kaolin according to the parts by weight to obtain a mixture B, wherein the water content in the mixture B is controlled to be less than 5%;
s82, molding: putting the mixed mixture B into a die of a ceramic sagger for compression molding, and then drying;
s83, firing: the dried sagger is put into a sintering furnace for sintering treatment, and the sintering process parameters are as follows: the firing temperature is 1340-1360 ℃, the firing heat preservation time is 3-4 hours, the ceramic sagger is cooled to room temperature, and finally the quality is inspected to be qualified, thus obtaining the high-performance ceramic sagger.
9. The method for preparing a high-performance ceramic sagger according to claim 8, wherein in the step S81, the particle size distribution of the mixture B is: more than 8 meshes are 5-20%,8-10 meshes are 10-30%,10-20 meshes are 10-30%,20-40 meshes are 10-20%,40-60 meshes are 5-15%,60-80 meshes are 5-15%,80-100 meshes are 5-15%, and less than or equal to 35% of 100 meshes.
10. The method for preparing a high performance ceramic sagger according to claim 8, wherein in the step S82, the pressure of the press forming is 17-20MPa, and the loose specific gravity of the mixture B is controlled to be more than 150g/100mL.
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