CN113943151A - Sagger for preparing lithium aluminum titanium phosphate solid electrolyte material and preparation method thereof - Google Patents
Sagger for preparing lithium aluminum titanium phosphate solid electrolyte material and preparation method thereof Download PDFInfo
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- CN113943151A CN113943151A CN202111198363.7A CN202111198363A CN113943151A CN 113943151 A CN113943151 A CN 113943151A CN 202111198363 A CN202111198363 A CN 202111198363A CN 113943151 A CN113943151 A CN 113943151A
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- 239000000463 material Substances 0.000 title claims abstract description 36
- CVJYOKLQNGVTIS-UHFFFAOYSA-K aluminum;lithium;titanium(4+);phosphate Chemical compound [Li+].[Al+3].[Ti+4].[O-]P([O-])([O-])=O CVJYOKLQNGVTIS-UHFFFAOYSA-K 0.000 title claims abstract description 35
- 239000007784 solid electrolyte Substances 0.000 title claims abstract description 35
- 229910000664 lithium aluminum titanium phosphates (LATP) Inorganic materials 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000011241 protective layer Substances 0.000 claims abstract description 52
- 239000000843 powder Substances 0.000 claims abstract description 48
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000000758 substrate Substances 0.000 claims abstract description 38
- 229910052582 BN Inorganic materials 0.000 claims abstract description 30
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 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 24
- 229910001579 aluminosilicate mineral Inorganic materials 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 239000000679 carrageenan Substances 0.000 claims abstract description 13
- 235000010418 carrageenan Nutrition 0.000 claims abstract description 13
- 229920001525 carrageenan Polymers 0.000 claims abstract description 13
- 229940113118 carrageenan Drugs 0.000 claims abstract description 13
- 239000004927 clay Substances 0.000 claims abstract description 13
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 claims abstract description 13
- 239000011230 binding agent Substances 0.000 claims abstract description 12
- 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 12
- 238000002156 mixing Methods 0.000 claims description 33
- 238000001035 drying Methods 0.000 claims description 29
- 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 description 19
- 229910052863 mullite Inorganic materials 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 19
- 239000002002 slurry Substances 0.000 claims description 18
- 238000000576 coating method Methods 0.000 claims description 17
- 238000000748 compression moulding Methods 0.000 claims description 16
- 238000005245 sintering Methods 0.000 claims description 15
- 238000003825 pressing Methods 0.000 claims description 13
- 239000011248 coating agent Substances 0.000 claims description 12
- 229910052878 cordierite Inorganic materials 0.000 claims description 11
- 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 description 11
- 238000001816 cooling Methods 0.000 claims description 9
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 8
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 7
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 7
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 7
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 239000011812 mixed powder Substances 0.000 claims description 3
- 229910052570 clay Inorganic materials 0.000 claims description 2
- 235000019353 potassium silicate Nutrition 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000010304 firing Methods 0.000 abstract description 4
- 229910052744 lithium Inorganic materials 0.000 description 10
- 239000010410 layer Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 6
- 210000001787 dendrite Anatomy 0.000 description 5
- 238000003618 dip coating Methods 0.000 description 4
- 238000004146 energy storage Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 239000011232 storage material Substances 0.000 description 2
- 239000002000 Electrolyte additive Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000002228 NASICON Substances 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000005518 polymer electrolyte Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- -1 uniformly stirring Substances 0.000 description 1
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—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
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
- C04B41/5062—Borides, Nitrides or Silicides
- C04B41/5064—Boron nitride
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
-
- 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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- 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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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/34—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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- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
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- C04B2235/6567—Treatment time
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Abstract
The invention discloses a sagger for preparing a lithium aluminum titanium phosphate solid electrolyte material and a preparation method thereof, and relates to the technical field of solid electrolytes, the sagger comprises a sagger substrate and a protective layer coated on the inner surface of the sagger substrate, and the sagger substrate is prepared from the following raw materials in parts by weight: 50-60 parts of aluminosilicate mineral powder, 10-15 parts of boron nitride, 20-25 parts of clay, 2.5-5 parts of zirconia micro powder, 2.5-5 parts of alumina micro powder, 5-10 parts of binder and 10-15 parts of water; the protective layer is prepared from the following raw materials in parts by weight: 20-35 parts of aluminosilicate mineral powder, 10-15 parts of boron nitride, 10-15 parts of carrageenan, 2.5-5 parts of nano zirconia, 2.5-5 parts of nano alumina, 5-10 parts of talcum powder, 1-5 parts of graphene and 25-35 parts of water. The sagger effectively prevents the reaction between the raw materials of the lithium titanium aluminum phosphate and the sagger during firing, is easier to separate the fired materials in the sagger from the sagger body, and prolongs the service life of the sagger.
Description
Technical Field
The invention relates to the technical field of solid electrolytes, in particular to a sagger for preparing a lithium aluminum titanium phosphate solid electrolyte material and a preparation method thereof.
Background
With the progress of science and technology and humanityThe improvement of the activity level, the development of electronic industries such as electric automobiles, portable electronic equipment, large-scale energy storage networks and the like is changing day by day, and the traditional commercial graphite cathode material of the lithium ion battery tends to the theoretical capacity (372mAh g)-1) The method reaches the development bottleneck and is difficult to meet the requirements of human society on high-endurance and high-power energy storage devices. Therefore, the vigorous development of battery energy storage materials with excellent performance has great significance for promoting the development of sustainable society. The lithium cathode in the lithium metal battery has high theoretical specific capacity (3860mAh/g), low electrochemical potential (-3.04V vs. standard hydrogen electrode) and small density (0.534 g/cm)3) However, although the lithium metal battery has many advantages, the battery has a series of problems of low coulombic efficiency, short cycle life and the like due to the violent volume change of the lithium metal, the instability of the SEI film and the uneven growth of lithium dendrites during continuous charge and discharge cycles, and the growth of the lithium dendrites even pierces the diaphragm to cause potential safety hazards, thereby causing short circuit and explosion of the lithium metal battery. Therefore, the inhibition of the growth of lithium dendrites becomes one of the research hotspots of the current battery energy storage materials, and researchers have conducted a great deal of research, and the inhibition of the growth of lithium dendrites is mainly achieved through the following research ideas: (1) a solid electrolyte; (2) a gel polymer electrolyte; (3) establishing electrode/electrolyte interface stability; (4) adding an electrolyte additive; (5) constructing an artificial SEI film; (6) and modifying the functional electrode.
Li of NASICON structure1.4Al0.4Ti1.6(PO4)3(LATP) has a relatively high electrical conductivity, about 7X 10 at ambient temperature-4S/cm, high melting point, good safety and stability at high temperature, high mechanical strength, and capability of well inhibiting the growth of lithium dendrites so as to avoid short circuit, however, LATP is very easy to chemically react with a sagger material in the firing process, and is tightly bonded with the inner surface of the sagger so as to be difficult to fall off.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides the sagger for preparing the lithium titanium aluminum phosphate solid electrolyte material and the preparation method thereof.
The sagger for preparing the lithium titanium aluminum phosphate solid electrolyte material comprises a sagger substrate and a protective layer coated on the inner surface of the sagger substrate, and is characterized in that the sagger substrate is prepared from the following raw materials in parts by weight: 50-60 parts of aluminosilicate mineral powder, 10-15 parts of boron nitride, 20-25 parts of clay, 2.5-5 parts of zirconia micro powder, 2.5-5 parts of alumina micro powder, 5-10 parts of binder and 10-15 parts of water;
the protective layer is prepared from the following raw materials in parts by weight: 20-35 parts of aluminosilicate mineral powder, 10-15 parts of boron nitride, 10-15 parts of carrageenan, 2.5-5 parts of nano zirconia, 2.5-5 parts of nano alumina, 5-10 parts of talcum powder, 1-5 parts of graphene and 25-35 parts of water.
Preferably, the aluminosilicate mineral powder is mullite or cordierite or a mixed powder of the mullite and the cordierite.
Preferably, in the sagger substrate raw material, the aluminosilicate mineral powder and the boron nitride powder have the particle size D50 of 10-50 mm.
Preferably, in the raw material of the protective layer, the particle size D50 of the aluminosilicate mineral powder and the boron nitride powder is 0.5-5 mm.
Preferably, the binder is one or more of alkaline silica sol, water glass and carboxymethyl cellulose.
Preferably, the thickness of the protective layer is 1-5 mm.
The invention also provides a preparation method of the sagger for preparing the lithium titanium aluminum phosphate solid electrolyte material, which comprises the following steps:
s1, taking aluminosilicate mineral powder, boron nitride, clay, zirconia micro powder, alumina micro powder and a binder as raw materials of the sagger substrate according to parts by weight, mixing, adding water, stirring, and performing compression molding to obtain the sagger substrate;
s2, mixing the aluminosilicate mineral powder, the boron nitride, the carrageenan, the nano-zirconia, the nano-alumina, the talcum powder and the graphene according to the weight part, and adding water to stir to obtain protective layer slurry;
and S3, coating the protective layer slurry on the inner surface of the sagger substrate, pre-drying, mechanically pressing, drying, sintering and cooling to obtain the sagger substrate.
In S2, the coating may be performed by a dip coating method, a spray coating method, or a brush coating method.
Preferably, in S3, the pre-drying temperature is 60-80 ℃, and the drying time is 1-5 h; the drying temperature after machine pressing is 80-100 ℃, and the drying time is 3-8 h.
Preferably, in S3, the sintering temperature is 1200-1400 ℃, and the sintering time is 1-5 h.
Has the advantages that: the sagger consists of a sagger substrate and a protective layer on the surface of the sagger substrate, so that the reaction between raw materials of lithium titanium aluminum phosphate and the sagger during firing is effectively prevented, and the fired materials in the sagger are easier to separate from the sagger body; boron nitride, aluminum oxide and graphene are added into the protective layer, and the synergistic effect of the boron nitride, the aluminum oxide and the graphene effectively improves the corrosion resistance and the wear resistance of the sagger and prolongs the service life of the sagger. The method adopts a mode of directly coating on the surface of the sagger, and effectively improves the bonding performance of the sagger substrate and the protective layer through high-temperature sintering, thereby prolonging the service life of the sagger.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A sagger for preparing lithium aluminum titanium phosphate solid electrolyte material comprises a sagger base body and a protective layer, wherein the protective layer at least covers the inner surface of the sagger base body;
the preparation method comprises the following steps:
(1) mixing 50 parts of mullite (10 mm in terms of D50), 10 parts of boron nitride (10 mm in terms of D50), 20 parts of clay, 2.5 parts of zirconia micro powder, 2.5 parts of alumina micro powder and 5 parts of binder alkaline silica sol in parts by weight, adding 10 parts of water, uniformly stirring and mixing, and then carrying out compression molding by compression molding equipment to obtain a sagger substrate preliminarily;
(2) mixing 20 parts of mullite (D50 is 0.5mm), 10 parts of boron nitride (D50 is 0.5mm), 10 parts of carrageenan, 2.5 parts of nano zirconia, 2.5 parts of nano alumina, 5 parts of talcum powder and 1 part of graphene according to parts by weight, adding 25 parts of water, and stirring and mixing uniformly to obtain a protective layer slurry;
(3) coating the protective layer slurry on the inner surface of the sagger substrate by adopting a dip coating method, pre-drying for 5 hours at 60 ℃, then performing mechanical pressing, and drying for 8 hours at 80 ℃, wherein the thickness of a material layer of the protective layer is controlled to be 1 mm;
(4) and (4) placing the sagger dried in the step (3) into a high-temperature kiln, sintering for 5 hours at 1200 ℃, and cooling to room temperature to obtain the sagger for preparing the lithium titanium aluminum phosphate solid electrolyte.
Example 2
A sagger for preparing lithium aluminum titanium phosphate solid electrolyte material comprises a sagger base body and a protective layer, wherein the protective layer at least covers the inner surface of the sagger base body;
the preparation method comprises the following steps:
(1) mixing 50 parts of mullite (50 mm in terms of D50), 10 parts of boron nitride (50 mm in terms of D50), 20 parts of clay, 2.5 parts of zirconia micro powder, 2.5 parts of alumina micro powder and 5 parts of binder alkaline silica sol in parts by weight, adding 10 parts of water, uniformly stirring and mixing, and then carrying out compression molding by compression molding equipment to obtain a sagger substrate preliminarily;
(2) mixing 35 parts of mullite (5 mm in terms of D50), 15 parts of boron nitride (5 mm in terms of D50), 15 parts of carrageenan, 5 parts of nano-zirconia, 5 parts of nano-alumina, 10 parts of talcum powder and 5 parts of graphene in parts by weight, adding 35 parts of water, and uniformly stirring and mixing to obtain a protective layer slurry;
(3) coating the protective layer slurry on the inner surface of the sagger substrate by adopting a dip coating method, pre-drying for 5 hours at 60 ℃, then performing mechanical pressing, and drying for 8 hours at 80 ℃, wherein the thickness of a material layer of the protective layer is controlled to be 5 mm;
(4) and (4) placing the sagger dried in the step (3) into a high-temperature kiln, sintering for 5 hours at 1200 ℃, and cooling to room temperature to obtain the sagger for preparing the lithium titanium aluminum phosphate solid electrolyte.
Example 3
A sagger for preparing lithium aluminum titanium phosphate solid electrolyte material comprises a sagger base body and a protective layer, wherein the protective layer at least covers the inner surface of the sagger base body;
the preparation method comprises the following steps:
(1) mixing 50 parts of mullite (10 mm in terms of D50), 10 parts of boron nitride (10 mm in terms of D50), 20 parts of clay, 2.5 parts of zirconia micro powder, 2.5 parts of alumina micro powder and 5 parts of binder alkaline silica sol in parts by weight, adding 10 parts of water, uniformly stirring and mixing, and then carrying out compression molding by compression molding equipment to obtain a sagger substrate preliminarily;
(2) mixing 20 parts of mullite (D50 is 0.5mm), 10 parts of boron nitride (D50 is 0.5mm), 10 parts of carrageenan, 2.5 parts of nano zirconia, 2.5 parts of nano alumina, 5 parts of talcum powder and 1 part of graphene according to parts by weight, adding 25 parts of water, and stirring and mixing uniformly to obtain a protective layer slurry;
(3) coating the protective layer slurry on the inner surface of the sagger substrate by adopting a dip coating method, pre-drying for 1h at 80 ℃, then performing mechanical pressing, and drying for 3h at 100 ℃, wherein the thickness of a material layer of the protective layer is controlled to be 1 mm;
(4) and (4) placing the sagger dried in the step (3) into a high-temperature kiln, sintering for 1h at 1400 ℃, and cooling to room temperature to obtain the sagger for preparing the lithium titanium aluminum phosphate solid electrolyte.
Example 4
A sagger for preparing lithium aluminum titanium phosphate solid electrolyte material comprises a sagger base body and a protective layer, wherein the protective layer at least covers the inner surface of the sagger base body;
the preparation method comprises the following steps:
(1) mixing 60 parts of mullite and cordierite mixture powder (1: 1 mass ratio, 10mm for D50), 15 parts of boron nitride (10 mm for D50), 25 parts of clay, 5 parts of zirconia micro powder, 5 parts of alumina micro powder, 5 parts of alkaline silica sol and 5 parts of carboxymethyl cellulose according to parts by weight, adding 15 parts of water, uniformly stirring and mixing, and then carrying out compression molding by compression molding equipment to obtain a sagger substrate preliminarily;
(2) mixing 20 parts of mullite and cordierite mixture powder (1: 1 mass ratio, D50 is 0.5mm), 10 parts of boron nitride (D50 is 0.5mm), 10 parts of carrageenan, 2.5 parts of nano zirconia, 2.5 parts of nano alumina, 5 parts of talcum powder and 1 part of graphene according to parts by weight, adding 25 parts of water, and uniformly stirring and mixing to obtain a protective layer slurry;
(3) coating the protective layer slurry on the inner surface of the sagger substrate by adopting a brush coating method, pre-drying for 5 hours at the temperature of 60 ℃, then performing mechanical pressing, and drying for 8 hours at the temperature of 80 ℃, wherein the thickness of a material layer of the protective layer is controlled to be 1 mm;
(4) and (4) placing the sagger dried in the step (3) into a high-temperature kiln, sintering for 5 hours at 1200 ℃, and cooling to room temperature to obtain the sagger for preparing the lithium titanium aluminum phosphate solid electrolyte.
Example 5
A sagger for preparing lithium aluminum titanium phosphate solid electrolyte material comprises a sagger base body and a protective layer, wherein the protective layer at least covers the inner surface of the sagger base body;
the preparation method comprises the following steps:
(1) mixing 60 parts of mullite and cordierite mixture powder (1: 1 mass ratio, 50mm D50), 15 parts of boron nitride (50 mm D50), 25 parts of clay, 5 parts of zirconia micro powder, 5 parts of alumina micro powder, 5 parts of alkaline silica sol and 5 parts of carboxymethyl cellulose according to parts by weight, adding 15 parts of water, uniformly stirring and mixing, and then carrying out compression molding by compression molding equipment to obtain a sagger substrate preliminarily;
(2) mixing 35 parts of mullite and cordierite mixture powder (1: 1 mass ratio, 5mm D50), 15 parts of boron nitride (5 mm D50), 15 parts of carrageenan, 5 parts of nano zirconia, 5 parts of nano alumina, 10 parts of talcum powder and 5 parts of graphene according to parts by weight, adding 35 parts of water, and uniformly stirring and mixing to obtain a protective layer slurry;
(3) coating the protective layer slurry on the inner surface of the sagger substrate by adopting a brush coating method, pre-drying for 5 hours at the temperature of 60 ℃, then performing mechanical pressing, and drying for 8 hours at the temperature of 80 ℃, wherein the thickness of a material layer of the protective layer is controlled to be 5 mm;
(4) and (4) placing the sagger dried in the step (3) into a high-temperature kiln, sintering for 5 hours at 1200 ℃, and cooling to room temperature to obtain the sagger for preparing the lithium titanium aluminum phosphate solid electrolyte.
Example 6
A sagger for preparing lithium aluminum titanium phosphate solid electrolyte material comprises a sagger base body and a protective layer, wherein the protective layer at least covers the inner surface of the sagger base body;
the preparation method comprises the following steps:
(1) mixing 60 parts of mullite and cordierite mixture powder (1: 1 mass ratio, 10mm for D50), 15 parts of boron nitride (10 mm for D50), 25 parts of clay, 5 parts of zirconia micro powder, 5 parts of alumina micro powder, 5 parts of alkaline silica sol and 5 parts of carboxymethyl cellulose in parts by weight, adding 15 parts of water, uniformly stirring and mixing, and then carrying out compression molding by compression molding equipment to obtain a sagger substrate preliminarily;
(2) mixing 20 parts of mullite and cordierite mixture powder (1: 1 mass ratio, D50 is 0.5mm), 10 parts of boron nitride (D50 is 0.5mm), 10 parts of carrageenan, 2.5 parts of nano zirconia, 2.5 parts of nano alumina, 5 parts of talcum powder and 1 part of graphene, adding 25 parts of water, and uniformly stirring and mixing to obtain a protective layer slurry;
(3) coating the protective layer slurry on the inner surface of the sagger substrate by adopting a brush coating method, pre-drying for 1 hour at 80 ℃, then performing mechanical pressing, and drying for 3 hours at 100 ℃, wherein the thickness of a material layer of the protective layer is controlled to be 1 mm;
(4) and (4) placing the sagger dried in the step (3) into a high-temperature kiln, sintering for 1h at 1400 ℃, and cooling to room temperature to obtain the sagger for preparing the lithium titanium aluminum phosphate solid electrolyte.
Example 7
A sagger for preparing lithium aluminum titanium phosphate solid electrolyte material comprises a sagger base body and a protective layer, wherein the protective layer at least covers the inner surface of the sagger base body;
the preparation method comprises the following steps:
(1) mixing 55 parts of mullite and cordierite mixture powder (1: 1 mass ratio, D50 is 30mm), 13 parts of boron nitride (D50 is 30mm), 22 parts of clay, 3 parts of zirconia micropowder, 3 parts of alumina micropowder and 8 parts of binder carboxymethyl cellulose according to the parts by weight, adding 12 parts of water, stirring and mixing uniformly, and then carrying out compression molding by compression molding equipment to obtain a sagger substrate preliminarily;
(2) mixing 30 parts of mullite (D50 is 2mm), 12 parts of boron nitride (D50 is 2mm), 13 parts of carrageenan, 3.5 parts of nano zirconia, 3 parts of nano alumina, 7 parts of talcum powder and 2 parts of graphene according to parts by weight, adding 30 parts of water, and stirring and mixing uniformly to obtain a protective layer slurry;
(3) coating the protective layer slurry on the inner surface of the sagger substrate by adopting a brush coating method, pre-drying for 3 hours at 75 ℃, then performing mechanical pressing, and drying for 4 hours at 95 ℃, wherein the thickness of a material layer of the protective layer is controlled to be 2 mm;
(4) and (4) placing the sagger dried in the step (3) into a high-temperature kiln, sintering for 1.5h at 1360 ℃, and cooling to room temperature to obtain the sagger for preparing the lithium titanium aluminum phosphate solid electrolyte.
Comparative example
A sagger for preparing a lithium aluminum titanium phosphate solid electrolyte material comprises the following steps:
(1) 55 parts of mullite and cordierite mixed powder (1: 1 mass ratio, D50 is 30mm), 22 parts of clay and 8 parts of binder carboxymethyl cellulose are mixed according to the parts by weight, 12 parts of water is added, and the mixture is uniformly stirred and then is pressed and molded by pressing and molding equipment to obtain a sagger substrate;
(2) mixing 30 parts of mullite and 13 parts of carrageenan according to parts by weight, adding 30 parts of water, uniformly stirring, coating on the inner surface of the sagger substrate prepared in the step (1), controlling the thickness of a material layer of a coating layer to be 2mm, pre-drying for 3 hours at 75 ℃, then carrying out mechanical pressing, drying for 4 hours at 95 ℃, drying twice, and sintering for 1.5 hours at 1360 ℃ in a high-temperature kiln to prepare the common sagger.
Application tests show that when the saggars prepared in the embodiments 1-7 of the invention are fired with lithium aluminum titanium phosphate, the fired materials and the saggars are not bonded together, and the saggars are still normal after being recycled for a plurality of times; the conventional sagger prepared in the comparative example reacts with the sagger when firing the lithium titanium aluminum phosphate solid electrolyte, and is tightly combined with the sagger, so that the sagger is difficult to separate.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. A sagger for preparing a lithium aluminum titanium phosphate solid electrolyte material comprises a sagger substrate and a protective layer coated on the inner surface of the sagger substrate, and is characterized in that the sagger substrate is prepared from the following raw materials in parts by weight: 50-60 parts of aluminosilicate mineral powder, 10-15 parts of boron nitride, 20-25 parts of clay, 2.5-5 parts of zirconia micro powder, 2.5-5 parts of alumina micro powder, 5-10 parts of binder and 10-15 parts of water;
the protective layer is prepared from the following raw materials in parts by weight: 20-35 parts of aluminosilicate mineral powder, 10-15 parts of boron nitride, 10-15 parts of carrageenan, 2.5-5 parts of nano zirconia, 2.5-5 parts of nano alumina, 5-10 parts of talcum powder, 1-5 parts of graphene and 25-35 parts of water.
2. The sagger for producing lithium aluminum titanium phosphate solid electrolyte material according to claim 1, wherein the aluminosilicate mineral powder is a mixed powder of mullite or cordierite or both.
3. The sagger for preparing lithium aluminum titanium phosphate solid electrolyte material according to claim 1, wherein in the raw material of the sagger substrate, the powder particle diameter D50 of aluminosilicate mineral powder and boron nitride is 10-50 mm.
4. The sagger for preparing lithium aluminum titanium phosphate solid electrolyte material according to claim 1, wherein the particle size D50 of the aluminosilicate mineral powder and the boron nitride in the raw material of the protective layer is 0.5-5 mm.
5. The sagger for preparing lithium aluminum titanium phosphate solid electrolyte material according to claim 1, wherein the binder is one or more of alkaline silica sol, water glass, and carboxymethyl cellulose.
6. The sagger for producing lithium aluminum titanium phosphate solid electrolyte material according to claim 1, wherein the thickness of the protective layer is 1 to 5 mm.
7. A method for producing a sagger for producing a lithium aluminum titanium phosphate solid electrolyte material according to any one of claims 1 to 6, comprising the steps of:
s1, taking aluminosilicate mineral powder, boron nitride, clay, zirconia micro powder, alumina micro powder and a binder as raw materials of the sagger substrate according to parts by weight, mixing, adding water, stirring, and performing compression molding to obtain the sagger substrate;
s2, mixing the aluminosilicate mineral powder, the boron nitride, the carrageenan, the nano-zirconia, the nano-alumina, the talcum powder and the graphene according to the weight part, and adding water to stir to obtain protective layer slurry;
and S3, coating the protective layer slurry on the inner surface of the sagger substrate, pre-drying, mechanically pressing, drying, sintering and cooling to obtain the sagger substrate.
8. The method for producing a sagger for producing a lithium titanium aluminum phosphate solid electrolyte material according to claim 7, wherein in S3, the pre-drying temperature is 60 to 80 ℃, and the drying time is 1 to 5 hours; the drying temperature after machine pressing is 80-100 ℃, and the drying time is 3-8 h.
9. The method for preparing a sagger for preparing lithium aluminum titanium phosphate solid electrolyte material as claimed in claim 7, wherein in S3, the sintering temperature is 1200-1400 ℃, and the sintering time is 1-5 h.
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