CN115819076A - Casket-like bowl and preparation method thereof and application of casket-like bowl in preparation of anode material - Google Patents
Casket-like bowl and preparation method thereof and application of casket-like bowl in preparation of anode material Download PDFInfo
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- CN115819076A CN115819076A CN202211614754.7A CN202211614754A CN115819076A CN 115819076 A CN115819076 A CN 115819076A CN 202211614754 A CN202211614754 A CN 202211614754A CN 115819076 A CN115819076 A CN 115819076A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- 239000010405 anode material Substances 0.000 title description 5
- 239000011248 coating agent Substances 0.000 claims abstract description 70
- 238000000576 coating method Methods 0.000 claims abstract description 70
- 239000002994 raw material Substances 0.000 claims abstract description 51
- 239000004575 stone Substances 0.000 claims abstract description 26
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 25
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 25
- 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 25
- 238000005245 sintering Methods 0.000 claims abstract description 24
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 21
- 239000010431 corundum Substances 0.000 claims abstract description 21
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 21
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 21
- 239000011230 binding agent Substances 0.000 claims abstract description 17
- 150000004767 nitrides Chemical class 0.000 claims abstract description 17
- 239000000758 substrate Substances 0.000 claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 39
- 239000011159 matrix material Substances 0.000 claims description 31
- 229910052878 cordierite Inorganic materials 0.000 claims description 27
- 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 27
- 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 27
- 229910052863 mullite Inorganic materials 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 238000002156 mixing Methods 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 18
- 230000032683 aging Effects 0.000 claims description 16
- 238000003825 pressing Methods 0.000 claims description 15
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 14
- 229910052744 lithium Inorganic materials 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 11
- 238000003483 aging Methods 0.000 claims description 10
- 239000007774 positive electrode material Substances 0.000 claims description 5
- 238000000748 compression moulding Methods 0.000 claims description 4
- 239000010453 quartz Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 13
- 239000000853 adhesive Substances 0.000 description 11
- 239000010410 layer Substances 0.000 description 11
- 229910052581 Si3N4 Inorganic materials 0.000 description 9
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 9
- 230000001070 adhesive effect Effects 0.000 description 8
- 229910052500 inorganic mineral Inorganic materials 0.000 description 8
- 239000011707 mineral Substances 0.000 description 8
- 238000012545 processing Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 230000007797 corrosion Effects 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 230000002035 prolonged effect Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000003628 erosive effect Effects 0.000 description 3
- 230000009970 fire resistant effect Effects 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000002457 bidirectional effect Effects 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 2
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical group O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000009545 invasion Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a sagger which comprises a substrate and a coating coated on the surface, wherein the coating comprises the following preparation raw materials in parts by weight: 40-50 parts of stone, 10-16 parts of corundum, 18-24 parts of kaolin, 7-10 parts of nitride, 2-6 parts of metal oxide and 2-6 parts of binder. According to the invention, by changing the formula of the sagger raw material coating, the coating has a good protection effect on the sagger substrate under the combined action of corundum, nitride and other raw materials, so that the damage to the sagger during sintering is reduced as much as possible. Therefore, the sagger in the invention is used for a far higher time than the conventional sagger, so that the sagger replacement time is reduced, the production stability is improved, and the cost is saved.
Description
Technical Field
The invention relates to the field of natural stone compositions, in particular to a casket and a preparation method thereof and application thereof in preparing a positive electrode material.
Background
The lithium ion battery has the advantages of large energy density, high output voltage, small self-discharge, excellent cycle performance and long service life, and is widely applied to electronic products such as mobile phones and the like. In the production of lithium batteries, electrode material sintering is a key ring, saggars are devices for storing electrode materials during sintering, and the saggars can be broken and scrapped after being sintered for multiple times, so that the production cost is increased, and development of the saggars with long service life on the basis of not influencing the sintering performance is of great importance. At present, most of common saggers are made of cordierite and mullite as aggregates through casting, pressing and sintering, but the service life is short and the rejection is fast. In the sintering process of lithium cobaltate, after reaching a certain number of times of use, the problems of cracking and bulging can occur, and particularly in the sintering process of high-voltage lithium cobaltate, the sagger faces more severe tests and has more strict requirements on the performance of the sagger.
The Chinese invention patent CN201910892444.3 discloses a special sagger for sintering a lithium battery anode material and a preparation method thereof, wherein a corrosion-resistant layer is additionally arranged on the inner bottom layer of a common sagger, and the corrosion-resistant layer comprises aluminum magnesium spinel, fused corundum, zirconia powder and the like; the sagger main body comprises cordierite, sintered mullite and the like, the difference between the corrosion-resistant layer and the raw materials of the sagger main body is large, the coating is easy to fall off on the surface of the sagger after being used for many times, and the service life of the sagger is shortened.
Disclosure of Invention
In order to improve the service life of the sagger for sintering lithium cobaltate and reduce the manufacturing cost of the sagger, the invention provides a sagger which comprises a substrate and a coating coated on the surface, wherein the coating is prepared from the following raw materials in parts by weight: 40-50 parts of stone, 10-16 parts of corundum, 18-24 parts of kaolin, 7-10 parts of nitride, 2-6 parts of metal oxide and 2-6 parts of binder.
According to the sagger coating, corundum and nitride are introduced into the preparation raw materials of the sagger coating, the erosion resistance of the sagger is improved through the combined action of the corundum and the nitride, the sagger coating has high density under the action of the corundum and the nitride, the invasion corrosion of cobalt and lithium materials to the sagger is reduced, and the service life of the sagger is prolonged.
As a preferred embodiment, the preparation raw materials of the matrix comprise, by weight: 50-70 parts of stone, 20-30 parts of kaolin, 2-4 parts of metal oxide and 4-8 parts of binder.
As a preferred embodiment, the thickness of the coating is 1 to 5mm.
The sagger outer layer is compounded with the coating with the thickness of 1-5mm, the problem that the coating is easy to separate from the sagger base body is solved by optimizing the sagger base body and the coating, the coating with the thickness of 1-5mm is adopted, the combination performance of the base body and the coating is good, the low cost is maintained, the sintering performance is good, and the service life is long.
As a preferred embodiment, the stone material is selected from one or a combination of more of mullite, quartz and cordierite.
As a preferred embodiment, the stone material is a combination of cordierite and mullite.
As a preferred embodiment, the weight ratio of cordierite to mullite in the matrix is (33-40): (23-34).
As a preferred embodiment, the weight ratio of cordierite to mullite in the coating is (20-28): (22-34).
In a preferred embodiment, the nitride is selected from one or a combination of several of silicon nitride, aluminum nitride and boron nitride.
In a preferred embodiment, the metal oxide is selected from one or more of alumina, magnesia and zirconia.
In a preferred embodiment, the cordierite particle size is 0.5-1.25 μm, the kaolin particle size is 0.3-3 μm, the mullite particle size is 8-12 μm, the corundum particle size is 5-5.5 μm, the silicon nitride particle size is 1.3-1.8 μm, and the alumina particle size is 5.2-6 μm.
As a preferred embodiment, the preparation raw materials of the substrate and the coating comprise fine aggregate and coarse aggregate, the particle size of the fine aggregate is less than 4.75 mu m, the particle size of the coarse aggregate is more than or equal to 4.75 mu m, and the weight ratio of the fine aggregate to the coarse aggregate is 1: (0.4-1).
The applicant adjusts various performance parameters of the sagger by adjusting the raw materials and the grain diameter proportion of the stone in the sagger, particularly the weight ratio of the fine aggregate to the coarse aggregate is 1: (0.4-1), the sagger density can be increased, the damage of the positive electrode material to the sagger when the high-pressure lithium cobaltate is sintered can be reduced, and the purposes of increasing the use times, prolonging the service life and reducing the cost are achieved.
The second aspect of the present invention provides a method for preparing the sagger, comprising the following steps:
(1) Mixing the preparation raw materials of the matrix and water in a stirrer, uniformly mixing, and ageing at room temperature to obtain a matrix material;
(2) Mixing the coating preparation raw materials and water in a stirrer, uniformly mixing and stirring, and ageing at room temperature to obtain a coating material;
(3) Laying a layer of coating material at the bottom of the die, adding a base material, laying a layer of coating material above the base material, and performing compression molding to obtain a blank;
(4) Drying and drying the pressed green body;
(5) And roasting the dried green body to obtain the sagger.
As a preferred embodiment, the ratio of the water to the total mass of the raw materials for preparing the matrix in step 1 is 3: (90-110); the ratio of the water to the total mass of the raw materials for preparing the coating in the step 2 is 3: (90-110).
During the experiments, the applicant found that the ratio of the raw material to water is 3: (90-110), the mechanical strength of the sagger prepared after sintering is higher, probably because the raw materials and water are matched with a proper sagger sintering temperature under a proper weight ratio, so that the sagger is beneficial to the migration of ions in the sagger, the growth and development of crystals, the sintering promotion effect is realized, the combination between particles in the sagger is enhanced, the preferable weight ratio range is exceeded, the sintering promotion effect is not obvious, and liquid is deposited among the particles to influence the growth of the grains, so that the internal combination is not facilitated, the mechanical property of the sagger is influenced, and the sagger is cracked and scrapped.
As a preferred embodiment, the stirring speed of the step 1,2 is 13-18r/min, the stirring time is 15-30min, and the ageing time is 30-40h.
In the experimental process, the applicant finds that the weight ratio of cordierite to mullite to kaolin is (33-40): (23-30): the raw material combination of (22-30) can improve the service life of the sagger, and the probable reason is guessed to be that: under the optimal weight ratio, in the process of sintering the anode material lithium cobaltate, aggregate of cordierite, mullite and kaolin jointly acts to form a reaction protective layer resisting corrosion of the anode material in the box body, so that the penetration of reactants in heat treatment is effectively resisted, and the service life is prolonged. The applicant further finds that the surface density of the sagger can be further increased by compounding the corundum-containing composite coating on the surface of the sagger, cobalt is reduced, lithium materials enter the sagger and react to generate lithium cobalt oxide, and volume expansion is generated to damage the sagger materials. However, the applicant further finds that if the binding property of the base body and the coating material of the saggar is poor, the coating is easy to peel off after sintering, so that the service life of the saggar is influenced, the applicant can improve the binding degree of the coating and the base body by adopting raw materials with matched types through the base body and the coating, and respectively allows the raw materials to be aged before sintering, so that the mixing and permeation among the raw materials are more uniform, the binding effect is better due to the similar types of the raw materials during sintering reaction, and the coating is not easy to fall off during later use.
As a preferred embodiment, the pressing pressure of step 3 is 25000-35000MPa, and the pressing time is 20-40s.
In a preferred embodiment, the roasting temperature of the step 5 is 1200-1400 ℃, and the roasting time is 5-7h.
The sagger sintered according to the formula has the advantages of erosion resistance, stability and low thermal expansion coefficient, so that the comprehensive performance of the sagger is remarkably improved. And the addition of the nitride in the coating material further improves the erosion resistance of the sagger, so that the sagger can be sintered by the high-voltage lithium cobaltate with the voltage of more than 4.45V, the performance is stable, the positive electrode material has less influence on the sagger, the use frequency is increased, and the service life is longer compared with that of a common sagger.
The third aspect of the invention provides an application of a sagger in preparing a positive electrode material, wherein the sagger is mainly applied to a sintering process of high-voltage lithium cobaltate with the voltage of more than 4.45V.
Compared with the prior art, the invention has the following beneficial effects:
(1) The preparation raw materials of the sagger adopt the following steps of 1: (0.4-1), the density of the sagger can be increased by adjusting the raw material and the grain size ratio of the stone in the sagger, the damage of the positive material to the sagger when the high-pressure lithium cobaltate is sintered by the sagger is reduced, the use frequency is increased, the service life is prolonged, and the cost is reduced.
(2) The sagger water and the sagger raw materials adopt the following steps: (90-110) the weight ratio can increase the mechanical strength of the sagger after sintering and improve the particle bonding in the sagger.
(3) According to the sagger, the coating containing corundum and nitride is compounded on the surface of the base body of the sagger, so that the surface density of the sagger can be further increased, lithium cobalt oxide generated by reaction in the sagger is reduced, and the damage of sagger materials caused by volume expansion is avoided.
(4) According to the invention, by changing the formula of the sagger raw material coating, the coating has a good protection effect on the sagger substrate under the combined action of corundum, nitride and other raw materials, so that the damage to the sagger during sintering is reduced as much as possible. Therefore, the sagger in the invention is used for a far higher time than the conventional sagger, so that the sagger replacement time is reduced, the production stability is improved, and the cost is saved.
Detailed Description
The stone material in the embodiment comprises a base stone material and a coating stone material, the metal oxide comprises a base metal oxide and a coating metal oxide, and the binder comprises a base binder and a coating binder.
Example 1
A sagger comprises a substrate and a coating coated on the surface, wherein the coating comprises the following preparation raw materials in parts by weight: 50 parts of stone, 13 parts of corundum, 21 parts of kaolin, 7 parts of nitride, 4 parts of metal oxide and 5 parts of binder. The stone in the coating is a combination of cordierite and mullite in a weight ratio of 23:27.
the preparation raw materials of the matrix comprise the following components in parts by weight: 67 parts of stone, 25 parts of kaolin, 2 parts of metal oxide and 6 parts of binder. The stone in the matrix is a combination of cordierite and mullite in a weight ratio of 35:32.
the nitride is silicon nitride, and the metal oxide is aluminum oxide. The adhesive is a silicate inorganic high-temperature adhesive which is purchased from the poly-adhesive products Co.Ltd of Dongguan city and has the model of JL-767C.
The grain size of the cordierite is 0.5-1.25 mu m, the grain size of the kaolin is 0.3-3 mu m, the grain size of the mullite is 8-12 mu m, the grain size of the corundum is 5-5.5 mu m, the grain size of the silicon nitride is 1.3-1.8 mu m, and the grain size of the alumina is 5.2-6 mu m.
The cordierite is purchased from dry mineral processing factory in Lingshou county; the kaolin is purchased from Guangzhou Changyue chemical Co., ltd; the mullite is purchased from a constant yang mineral product processing factory in Lingshou county; the corundum is purchased from Huahui refractory Co., ltd, hiroshi city; the silicon nitride is purchased from a vessel shop for a tripod welding material; the alumina was purchased from a strength supplier of the fire-resistant material of heonangkei ltd.
Fine aggregate (the grain diameter is less than 4.75 mu m) and coarse aggregate (the grain diameter is more than or equal to 4.75 mu m) in the preparation raw materials of the substrate and the coating, wherein the weight ratio of the fine aggregate to the coarse aggregate in the substrate is 1:0.56, wherein the weight ratio of the fine aggregate to the coarse aggregate in the coating is 1:0.86.
the preparation method of the sagger comprises the following steps:
(1) Putting the preparation raw materials of the matrix and water into a stirrer for mixing, using a planetary edge runner mill, uniformly mixing and stirring, and then aging at 25 ℃ to obtain a matrix material;
(2) Mixing the coating preparation raw materials and water in a stirrer, uniformly mixing and stirring by using a planetary edge runner mill, and ageing at 25 ℃ to obtain a coating material;
(3) Uniformly paving a layer of coating material with the thickness of 2mm at the bottom of the die, then adding a base material, paving a layer of coating material with the thickness of 2mm above the base material, and performing compression molding to obtain a blank with the thickness of 13 mm;
(4) Drying the pressed green body in the shade at 25 ℃ for 24 hours, then putting the green body into a drying room for drying for 5 hours, and finally putting the green body into a drying kiln for drying at 110 ℃ for 4 hours;
(5) And roasting the dried green body to obtain the sagger.
The ratio of the water to the total mass of the matrix in the step 1 is 3:100, respectively; the ratio of the water to the total mass of the coating in the step 2 is 3:100.
the stirring speed of the steps 1 and 2 is 16r/min, the stirring time is 20min, and the ageing time is 36h.
The pressing pressure of the step 3 is 28000MPa, and the pressing time is 30s.
The roasting temperature in the step 5 is 1300 ℃, and the roasting time is 6h.
Example 2
A sagger comprises a substrate and a coating coated on the surface, wherein the coating comprises the following preparation raw materials in parts by weight: 51 parts of stone, 12 parts of corundum, 22 parts of kaolin, 9 parts of nitride, 3 parts of metal oxide and 5 parts of binder. The stone in the coating is a combination of cordierite and mullite in a weight ratio of 26:25.
the preparation raw materials of the matrix comprise the following components in parts by weight: 65 parts of stone, 27 parts of kaolin, 3 parts of metal oxide and 6 parts of binder. The stone in the matrix is a combination of cordierite and mullite in a weight ratio of 38:27.
the nitride is silicon nitride, and the metal oxide is aluminum oxide. The adhesive is a silicate inorganic high-temperature adhesive which is purchased from the poly-adhesive products Co.Ltd of Dongguan city and has the model of JL-767C.
The grain size of the cordierite is 0.5-1.25 mu m, the grain size of the kaolin is 0.3-3 mu m, the grain size of the mullite is 8-12 mu m, the grain size of the corundum is 5-5.5 mu m, the grain size of the silicon nitride is 1.3-1.8 mu m, and the grain size of the alumina is 5.2-6 mu m.
The cordierite is purchased from dry mineral processing factory in Lingshou county; the kaolin is purchased from Guangzhou Changyue chemical Co., ltd; the mullite is purchased from a constant yang mineral product processing factory in Lingshou county; the corundum is purchased from Huahui refractory Co., ltd, hiroshi city; the silicon nitride is purchased from a vessel shop for a tripod welding material; the alumina was purchased from a strength supplier of henanfeng ka refractory.
Fine aggregate (the grain diameter is less than 4.75 mu m) and coarse aggregate (the grain diameter is more than or equal to 4.75 mu m) in the preparation raw materials of the substrate and the coating, wherein the weight ratio of the fine aggregate to the coarse aggregate in the substrate is 1:0.46, wherein the weight ratio of the fine aggregate to the coarse aggregate in the coating is 1:0.7.
the preparation method of the sagger comprises the following steps:
(1) Putting the preparation raw materials of the matrix and water into a stirrer for mixing, using a planetary edge runner mill, uniformly mixing and stirring, and then aging at 25 ℃ to obtain a matrix material;
(2) Mixing the coating preparation raw materials and water in a stirrer, uniformly mixing and stirring by using a planetary edge runner mill, and ageing at 25 ℃ to obtain a coating material;
(3) Uniformly paving a layer of coating material with the thickness of 4mm at the bottom of the die, then adding a base material, paving a layer of coating material with the thickness of 4mm above the base material, and performing compression molding to obtain a blank with the thickness of 15 mm;
(4) Drying the pressed green body in the shade at 25 ℃ for 24 hours, then putting the green body into a drying room for drying for 5 hours, and finally putting the green body into a drying kiln for drying at 110 ℃ for 4 hours;
(5) And roasting the dried green body to obtain the sagger.
The ratio of the water to the total mass of the matrix in the step 1 is 3:105; the ratio of the water to the total mass of the coating in the step 2 is 3:105.
the stirring speed of the steps 1 and 2 is 14r/min, the stirring time is 25min, and the ageing time is 38h.
The pressing pressure of the step 3 is 33000MPa, and the pressing time is 20s.
The roasting temperature in the step 5 is 1350 ℃, and the roasting time is 5.5h.
Comparative example 1
A sagger comprises a base body, wherein the base body is prepared from the following raw materials in parts by weight: 65 parts of stone, 28 parts of kaolin, 2 parts of metal oxide and 5 parts of binder. The stone in the matrix is a combination of cordierite and mullite in a weight ratio of 38:27.
the metal oxide is alumina. The adhesive is a silicate inorganic high-temperature adhesive which is purchased from a poly-strength adhesive product limited company in Dongguan and has the model of JL-767C.
The grain diameter of the cordierite is 0.5-1.25 mu m, the grain diameter of the kaolin is 0.3-3 mu m, the grain diameter of the mullite is 8-12 mu m, and the grain diameter of the alumina is 5.2-6 mu m.
The cordierite is purchased from dry mineral processing factory in Lingshou county; the kaolin is purchased from Guangzhou Changyue chemical Co., ltd; the mullite is purchased from a constant yang mineral product processing factory in Lingshou county; the alumina was purchased from a strength supplier of the fire-resistant material of heonangkei ltd.
Fine aggregate (the particle size is less than 4.75 mu m) and coarse aggregate (the particle size is more than or equal to 4.75 mu m) in the preparation raw materials of the matrix, wherein the weight ratio of the fine aggregate to the coarse aggregate in the matrix is 1:0.44.
the preparation method of the sagger comprises the following steps:
(1) Putting the preparation raw materials of the matrix and water into a stirrer for mixing, using a planetary edge runner mill, uniformly mixing and stirring, and then aging at 25 ℃ to obtain a matrix material;
(2) Pouring the mixed material into a die, and pressing and forming by using a bidirectional press to obtain a blank body;
(3) Drying the pressed green body in the shade at 25 ℃ for 24 hours, then putting the green body into a drying room for drying for 5 hours, and finally putting the green body into a drying kiln for drying at 110 ℃ for 4 hours;
(4) And roasting the dried green body to obtain the sagger.
The ratio of the water to the total mass of the matrix in the step 1 is 3:100.
the stirring speed of the step 1 is 16r/min, the stirring time is 20min, and the ageing time is 36h.
The pressing pressure of the step 2 is 30000MPa, and the pressing time is 30s.
The roasting temperature in the step 4 is 1300 ℃, and the roasting time is 6 hours.
Comparative example 2
A sagger comprises a substrate, wherein the substrate is prepared from the following raw materials in parts by weight: 67 parts of stone, 25 parts of kaolin, 3 parts of metal oxide and 5 parts of binder. The stone in the matrix is a combination of cordierite and mullite in a weight ratio of 35:32.
the metal oxide is alumina. The binder is a silicate inorganic high-temperature adhesive. Available from poly-adhesive products, inc. of Dongguan, model JL-767C.
The grain diameter of the cordierite is 0.5-1.25 mu m, the grain diameter of the kaolin is 0.3-3 mu m, the grain diameter of the mullite is 8-12 mu m, and the grain diameter of the alumina is 5.2-6 mu m.
The cordierite is purchased from dry mineral processing factory in Lingshou county; the kaolin is purchased from Guangzhou Changyue chemical Co., ltd; the mullite is purchased from a constant yang mineral product processing factory in Lingshou county; the alumina was purchased from a strength supplier of the fire-resistant material of heonangkei ltd.
Fine aggregate (the particle size is less than 4.75 mu m) and coarse aggregate (the particle size is more than or equal to 4.75 mu m) in the preparation raw materials of the matrix, wherein the weight ratio of the fine aggregate to the coarse aggregate in the matrix is 1:0.53.
the preparation method of the sagger comprises the following steps:
(1) Putting the preparation raw materials of the matrix and water into a stirrer for mixing, using a planetary edge runner mill, uniformly mixing and stirring, and then aging at 25 ℃ to obtain a matrix material;
(2) Pouring the mixed material into a die, and pressing and forming by using a bidirectional press to obtain a blank body;
(3) Drying the pressed green body in the shade at 25 ℃ for 24 hours, then putting the green body into a drying room for drying for 5 hours, and finally putting the green body into a drying kiln for drying at 110 ℃ for 4 hours;
(4) And roasting the dried green body to obtain the sagger.
The ratio of the water to the total mass of the matrix in the step 1 is 3:120.
the stirring speed of the step 1 is 16r/min, the stirring time is 20min, and the ageing time is 36h.
The pressing pressure of the step 2 is 30000MPa, and the pressing time is 30s.
The roasting temperature in the step 4 is 1300 ℃, and the roasting time is 6 hours.
Comparative example 3
A sagger comprises a substrate and a coating coated on the surface, wherein the coating comprises the following preparation raw materials in parts by weight: 15 parts of cordierite, 25 parts of mullite, 8 parts of corundum, 21 parts of kaolin, 5 parts of nitride, 4 parts of metal oxide and 5 parts of binder.
The preparation raw materials of the matrix comprise the following components in parts by weight: 20 parts of cordierite, 35 parts of mullite, 21 parts of kaolin, 4 parts of metal oxide and 5 parts of binder, and the other steps are the same as those in example 1.
Comparative example 4
A sagger comprises a base body and a coating coated on the surface, and the concrete steps are the same as example 1, but the difference is that the grain size of cordierite is 0.5-1.25 mu m, the grain size of kaolin is 0.3-3 mu m, the grain size of mullite is 8-12 mu m, the grain size of corundum is 6-10 mu m, the grain size of silicon nitride is 2.0-4 mu m, and the grain size of alumina is 5.2-6 mu m.
Performance testing
The sagger prepared in the examples 1-2 and the comparative examples 1-4 is used in the sintering process of 4.45V high-voltage lithium cobaltate, and the number of scrapped sagger, scrapped reason and scrapped percentage of the sagger under different groups of sintering times are tested. Average number of uses = (number of uses × scrap percentage)/n; n: the number of groups tested.
The test results of examples 1 to 2 are shown in Table 1, and the test results of comparative examples 1 to 4 are shown in tables 2,3,4,5.
TABLE 1
TABLE 2
TABLE 3
TABLE 4
TABLE 5
The average use times of the sagger examples prepared by the formula are 40 times and far higher than the average use times of the comparative examples, which shows that the protective effect of the coating on the matrix can be enhanced by adding corundum and nitride raw materials with specific dosage and particle size in the coating, and the service life of the sagger is further prolonged.
Claims (10)
1. The sagger is characterized by comprising a base body and a coating coated on the surface, wherein the coating comprises the following preparation raw materials in parts by weight: 40-60 parts of stone, 10-16 parts of corundum, 18-24 parts of kaolin, 7-10 parts of nitride, 2-6 parts of metal oxide and 2-6 parts of binder.
2. The sagger of claim 1, wherein the base is prepared from raw materials comprising, in parts by weight: 50-70 parts of stone, 20-30 parts of kaolin, 2-4 parts of metal oxide and 4-8 parts of binder.
3. Sagger according to claim 1 or 2, characterized in that said coating has a thickness of 1-5mm; the stone is selected from one or a combination of more of mullite, quartz and cordierite.
4. The sagger of claim 3, wherein the preparation raw materials of the substrate and the coating comprise fine aggregate and coarse aggregate, the particle size of the fine aggregate is less than 4.75 μm, the particle size of the coarse aggregate is more than or equal to 4.75 μm, and the weight ratio of the fine aggregate to the coarse aggregate is 1: (0.4-1).
5. A process for the preparation of a sagger according to any one of claims 1 to 4, characterized by comprising the following steps:
(1) Putting the preparation raw materials of the matrix and water into a stirrer for mixing, uniformly mixing and stirring, and then aging at room temperature to obtain a matrix material;
(2) Mixing the coating preparation raw materials and water in a stirrer, uniformly mixing and stirring, and ageing at room temperature to obtain a coating material;
(3) Laying a layer of coating material at the bottom of the die, adding a base material, laying a layer of coating material above the base material, and performing compression molding to obtain a blank;
(4) Drying and baking the pressed green body;
(5) And roasting the dried green body to obtain the sagger.
6. The method of producing a sagger as claimed in claim 5, wherein the ratio of the water to the total mass of the raw materials for preparing the base in step 1 is 3: (90-110); the ratio of the water to the total mass of the raw materials for preparing the coating in the step 2 is 3: (90-110).
7. The sagger preparation method according to claim 5, wherein the stirring speed of step 1,2 is 13-18r/min, the stirring time is 15-30min, and the aging time is 30-40h.
8. The process for producing sagger as claimed in claim 5, wherein said pressing pressure of step 3 is 25000-35000MPa, and pressing time is 20-40s.
9. The sagger manufacturing method according to claim 5, wherein the roasting temperature in step 5 is 1200-1400 ℃, and the roasting time is 5-7 hours.
10. Use of a sagger according to any one of claims 1-4 in the preparation of a positive electrode material, wherein said sagger is used primarily in the sintering process of high voltage lithium cobaltate above 4.45V.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115340392A (en) * | 2022-08-31 | 2022-11-15 | 泰安蔚蓝金属陶瓷材料有限公司 | Sagger for long-life lithium battery positive electrode material and preparation method of sagger |
| CN115340409A (en) * | 2022-08-31 | 2022-11-15 | 泰安蔚蓝金属陶瓷材料有限公司 | Sagger coating for lithium battery positive electrode material and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115340392A (en) * | 2022-08-31 | 2022-11-15 | 泰安蔚蓝金属陶瓷材料有限公司 | Sagger for long-life lithium battery positive electrode material and preparation method of sagger |
| CN115340409A (en) * | 2022-08-31 | 2022-11-15 | 泰安蔚蓝金属陶瓷材料有限公司 | Sagger coating for lithium battery positive electrode material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 李楠等编著: "《等离子束表面冶金强化硬面材料设计、制备及性能》", vol. 2, 冶金工业出版社, pages: 424 - 425 * |
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