CN115141025A - Production method of anti-sticking sagger for ternary cathode material production - Google Patents
Production method of anti-sticking sagger for ternary cathode material production Download PDFInfo
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- CN115141025A CN115141025A CN202210660065.3A CN202210660065A CN115141025A CN 115141025 A CN115141025 A CN 115141025A CN 202210660065 A CN202210660065 A CN 202210660065A CN 115141025 A CN115141025 A CN 115141025A
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 33
- 239000010406 cathode material Substances 0.000 title claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 45
- 229910052878 cordierite Inorganic materials 0.000 claims abstract 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 abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052582 BN Inorganic materials 0.000 claims abstract description 13
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 12
- 239000011230 binding agent Substances 0.000 claims abstract description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 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 9
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 9
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 8
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 8
- 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 8
- 239000000843 powder Substances 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 13
- 229910052710 silicon Inorganic materials 0.000 claims description 10
- 239000010703 silicon Substances 0.000 claims description 10
- 230000032683 aging Effects 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- 229920001353 Dextrin Polymers 0.000 claims description 5
- 239000004375 Dextrin Substances 0.000 claims description 5
- 235000019425 dextrin Nutrition 0.000 claims description 5
- 238000000748 compression moulding Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 3
- 238000010304 firing Methods 0.000 abstract description 5
- 239000002344 surface layer Substances 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract description 2
- 239000010410 layer Substances 0.000 abstract description 2
- 230000001050 lubricating effect Effects 0.000 abstract description 2
- 230000005012 migration Effects 0.000 abstract description 2
- 238000013508 migration Methods 0.000 abstract description 2
- 239000007774 positive electrode material Substances 0.000 abstract description 2
- 230000003746 surface roughness Effects 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000011863 silicon-based powder Substances 0.000 abstract 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 8
- 229910052744 lithium Inorganic materials 0.000 description 8
- 239000010405 anode material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 229910001437 manganese ion Inorganic materials 0.000 description 2
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 description 1
- SOXUFMZTHZXOGC-UHFFFAOYSA-N [Li].[Mn].[Co].[Ni] Chemical compound [Li].[Mn].[Co].[Ni] SOXUFMZTHZXOGC-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910001429 cobalt ion Inorganic materials 0.000 description 1
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C04B35/195—Alkaline earth aluminosilicates, e.g. cordierite or anorthite
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Abstract
The invention discloses a production method of an anti-sticking material sagger for producing a ternary cathode material, wherein the sagger formula comprises the following components in percentage by weight: 3-5wt% of boron nitride and alpha-Al 2 O 3 8-10wt%, 20-25wt% of large-particle-size cordierite, 10-15wt% of small-particle-size cordierite, 20-25wt% of mullite, 20-25wt% of kaolin, 3-5wt% of silicon powder and 4-6wt% of a binder are additionally added, the materials are mixed according to a sagger formula, stirred and mixed uniformly, aged for 48 hours, the water content is regulated to 3% -5%, and then the materials are fired and molded at a high temperature of 1350-1420 ℃ to obtain the anti-sticking sagger, when the materials are pressed, fine-particle-size particles spontaneously migrate to the surface layer to form a surface compact layer of 1-2mm, so that the corrosion of the surface layer by each material during the firing of the ternary positive electrode material is reduced, and the migration space of the materials is blocked,the problem of material sticking is improved; meanwhile, the formula provided by the invention contains a surface lubricating component, so that the surface roughness of a sagger firing part is improved, and the problem of material sticking of a product is further improved.
Description
Technical Field
The invention belongs to the field of lithium batteries, relates to a manufacturing technology of lithium battery generating equipment, and particularly relates to a production method of an anti-sticking sagger for producing a ternary cathode material.
Background
The application is a divisional application of a sagger formula and a production method (202110880352.0) for producing a ternary cathode material. The performance of a commercial lithium ion battery cathode material is an important factor determining the performance of a lithium ion battery. Currently, developed anode materials include lithium cobaltate, lithium iron phosphate, lithium manganate, ternary materials, and the like. Lithium nickel manganese cobalt is the most common cathode material of a ternary lithium battery. Nickel ion (Ni) 2+ ) The volume energy density of the anode material can be increased; manganese ion (Mn) 4+ ) The thermal stability of the material can be improved, and the safety performance of the material is further improved; cobalt ion (Co) 3+ ) Can make up the deficiency of manganese ions, maintain the stability of the layered structure of the material and further improve the cycle rate performance of the material. Therefore, the ternary lithium battery cathode material gradually becomes the mainstream cathode material of the lithium battery for the vehicle, and is widely applied to the field of new energy electric vehicles.
The ternary positive electrode material is prepared by placing various precursors in a sagger and sintering at high temperature by adopting a high-temperature solid phase method (a pushed slab kiln or a roller kiln). The sagger material for firing is mainly cordierite, mullite and corundum. Sagger in the current market is applied to production of ternary lithium battery anode materials, the ternary anode materials are adhered to the inner surface of the sagger after firing is completed, and more materials are remained and are difficult to remove when the sagger is inverted.
Aiming at the problem of sagger material sticking in the production of ternary cathode materials, few researches are carried out at present, the sagger pouring and cleaning mechanism is mainly improved, but the effect is not ideal.
Disclosure of Invention
The invention aims to provide a production method of a sagger for producing a ternary cathode material, which aims to solve the problems in the background technology.
In order to realize the purpose, the invention adopts the technical scheme as follows:
the production method of the anti-sticking sagger for producing the ternary cathode material is characterized by comprising the following steps of:
step one, weighing materials according to the weight percentage of a sagger formula, placing the materials in a stirrer to be stirred until the materials are uniformly mixed, ageing the materials for 48 hours to obtain powder, and measuring the water content of the powder after ageing to obtain the powder with the water content of 3-5%;
the sagger formula comprises the following components in percentage by weight: 3-5wt% of boron nitride and alpha-Al 2 O 3 8-10wt% of aluminum powder, 20-25wt% of large-particle-size cordierite, 10-15wt% of small-particle-size cordierite, 20-25wt% of mullite, 20-25wt% of kaolin, 3-5wt% of silicon micropowder and 4-6wt% of binder as the rest;
in the components of the sagger formula, the grain size range of the cordierite with large grain size is 0.5-1.5mm; the grain size of the small-grain cordierite is less than or equal to 0.075mm; the proportion of the large-particle-size cordierite to the small-particle-size cordierite is 2;
secondly, the materials enter a sagger die through a conveyor belt and an automatic feeding device for compression molding, and green bodies are manufactured;
step three, naturally airing the green body, transferring the green body to a drying room, and drying for 48 hours, wherein the baking temperature is controlled to be 90-100 ℃;
and step four, putting the sagger product dried in the step four into a high-temperature kiln for sintering, wherein the sintering temperature is 1350-1420 ℃, and the sintering time is 9-10 h, so that the anti-sticking sagger for producing the ternary cathode material is prepared.
Preferably, the boron nitride is in the form of particles having a particle size of 20 to 50 μm.
Further preferably, the density of the boron nitride is 2.27 to 2.30g/cm 3 。
Preferably, the granularity of the silicon micropowder is 800-1600 meshes.
More preferably, siO in the silicon micropowder 2 Content (wt.)>85%。
Preferably, the binder is a yellow dextrin solution.
Further preferably, the binder has a water content of 45 to 55%.
Preferably, the alpha-Al 2 O 3 Al in aluminum powder 2 O 3 The content is more than or equal to 98wt percent.
Further preferably, the alpha-Al 2 O 3 The grain diameter of the aluminum powder is less than or equal to 0.10mm.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the formula and the production method provided by the invention, coexisting bodies with various particle sizes are formed during burdening, and when green compact pressing is carried out, fine particle size particles spontaneously migrate to a surface layer along with the gradual increase of the pressure of a die after automatic feeding is finished, so that a surface compact layer with the diameter of 1-2mm is formed. Therefore, the corrosion of each material to the surface layer when the ternary cathode material is fired is reduced, the material migration space is blocked, and the problem of material adhesion is solved;
2. the formula provided by the invention contains boron nitride as an effective surface lubricating component, and can improve the surface roughness of a sagger firing part to a greater extent, so that the problem of material sticking of a product is solved.
Detailed Description
The invention provides a sagger formula for producing a ternary cathode material, which comprises the following components in percentage by weight: 3-5wt% of boron nitride and alpha-Al 2 O 3 8-10wt% of large-particle-size cordierite, 20-25wt% of small-particle-size cordierite, 20-25wt% of mullite, 20-25wt% of kaolin, 3-5wt% of silicon micropowder and 4-6wt% of binder as the rest.
Understandably, the boron nitride density: 2.27-2.30g/cm 3 The grain diameter is 20-50 mu m;
the alpha-Al 2 O 3 Al of aluminum powder 2 O 3 The content is more than or equal to 98wt%, and the grain diameter is less than or equal to 0.10mm;
the particle size range of the large-particle-size cordierite is 0.5-1.5mm;
the small-particle-size cordierite has the particle size of less than or equal to 0.075mm;
al of the mullite 2 O 3 The content is more than or equal to 65wt%, and the grain diameter is less than or equal to 1.0mm;
al of the kaolin 2 O 3 The content is more than or equal to 33wt%, and the grain diameter is less than or equal to 0.10mm;
SiO in the silicon micro powder 2 The content is more than 85 percent, and the granularity is 800-1600 meshes;
the binder is yellow dextrin solution with water content of 45-55%.
Wherein the proportion of the large-particle-size cordierite to the small-particle-size cordierite is 2.
The invention also provides a production method of the anti-sticking material sagger for producing the ternary cathode material, which comprises the following steps:
step one, weighing materials according to the weight percentage, placing the materials in a stirrer to be stirred until the materials are uniformly mixed, and ageing the materials for 48 hours to obtain powder, and measuring the water content of the powder after ageing, wherein the water content is between 3 and 5 percent;
secondly, the materials enter a sagger die through a conveyor belt and an automatic feeding device for compression molding, and green bodies are manufactured;
step three, naturally airing the green body, transferring the green body to a drying room, and drying for 48 hours, wherein the baking temperature is controlled to be 90-100 ℃;
and step four, putting the sagger product dried in the step four into a high-temperature kiln for sintering, wherein the sintering temperature is 1350-1420 ℃, and the sintering time is 9-10 h, so that the anti-sticking sagger for producing the ternary cathode material is prepared.
Example 1, a sagger formulation for ternary cathode material production comprises the following components in percentage by mass: boron nitride 3wt%, alpha-Al 2 O 3 10wt%, large-particle-size cordierite 25wt%, small-particle-size cordierite 12.5wt%, mullite 22.5wt%, kaolin 23wt%, fine silica powder 4wt%, and a 4wt% yellow dextrin solution (containing 50wt% of water) were added.
Material | Boron nitride | α-Al 2 O 3 | Large grain size cordierite | Small particle size cordierite | Mullite | Kaolin clay | Silicon micropowder |
Percentage of | 3wt% | 10wt% | 25wt% | 12.5wt% | 22.5wt% | 23wt% | 4wt% |
A production method of an anti-sticking sagger produced by a ternary cathode material comprises the following steps:
step one, boron nitride 3wt%, alpha-Al 2 O 3 10wt%, 25wt% of large-particle-size cordierite, 12.5wt% of small-particle-size cordierite, 22.5wt% of mullite, 23wt% of kaolin and 4wt% of silicon micropowder, and adding 4wt% of yellow dextrin solution (containing 50wt% of water) as a binder to mix, placing the mixture in a stirrer to stir until the mixture is uniformly mixed, and ageing for 48 hours to obtain the powder. Measuring the water content of the powder after the aging, wherein the water content range is 3-5%;
secondly, the materials enter a sagger die through a conveyor belt and an automatic feeding device for compression molding, and green bodies are manufactured;
step three, naturally airing the green body, transferring the green body to a drying room, and drying for 48 hours, wherein the baking temperature is controlled to be 90-100 ℃; and step four, putting the sagger product dried in the step four into a high-temperature kiln for sintering, wherein the sintering temperature is 1350-1420 ℃, and the sintering time is 9-10 h, so that the anti-sticking sagger for producing the ternary cathode material is prepared.
When the sagger prepared in the embodiment 1 is used for producing the ternary lithium battery cathode material, after the sagger is used for 25 times, the amount of the single sagger binder is 25g, which is far less than the conventional 50g binder.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. The production method of the anti-sticking sagger for producing the ternary cathode material is characterized by comprising the following steps of:
step one, weighing materials according to the weight percentage of a sagger formula, placing the materials in a stirrer to be stirred until the materials are uniformly mixed, ageing the materials for 48 hours to obtain powder, and measuring the water content of the powder after ageing to obtain the powder with the water content of 3-5%;
the sagger formula comprises the following components in percentage by weight: 3-5wt% of boron nitride and alpha-Al 2 O 3 8-10wt% of aluminum powder, 20-25wt% of large-particle-size cordierite, 10-15wt% of small-particle-size cordierite, 20-25wt% of mullite, 20-25wt% of kaolin, 3-5wt% of silicon micropowder and 4-6wt% of binder as the rest;
in the components of the sagger formula, the grain size range of the cordierite with large grain size is 0.5-1.5mm; the grain size of the small-grain cordierite is less than or equal to 0.075mm; the proportion of the large-particle-size cordierite to the small-particle-size cordierite is 2;
secondly, the materials enter a sagger die through a conveyor belt and an automatic feeding device for compression molding, and green bodies are manufactured;
step three, naturally airing the green body, transferring the green body to a drying room, and drying for 48 hours, wherein the baking temperature is controlled to be 90-100 ℃;
and step four, putting the sagger product dried in the step four into a high-temperature kiln for sintering, wherein the sintering temperature is 1350-1420 ℃, and the sintering time is 9-10 h, so that the anti-sticking sagger for producing the ternary cathode material is prepared.
2. The method for producing the anti-sticking material sagger for the production of the ternary cathode material as claimed in claim 1, wherein: the boron nitride is granular and has a particle size of 20-50 μm.
3. The method for producing the anti-sticking material sagger for the production of the ternary cathode material as claimed in claim 1, wherein: the density of the boron nitride is 2.27-2.30g/cm 3 。
4. The method for producing the anti-sticking material sagger for the production of the ternary cathode material as claimed in claim 1, wherein: the granularity of the silicon micro powder is 800-1600 meshes.
5. The method for producing the anti-sticking material sagger for the production of the ternary cathode material as claimed in claim 1, wherein: siO in the silicon micro powder 2 Content (wt.)>85%。
6. The method for producing the anti-sticking sagger for ternary cathode material production according to claim 1, wherein: the binder is yellow dextrin solution.
7. The method for producing the anti-sticking material sagger for the production of the ternary cathode material as claimed in claim 1, wherein: the water content of the binder is 45-55%.
8. The method for producing the anti-sticking material sagger for the production of the ternary cathode material as claimed in claim 1, wherein: the alpha-Al 2 O 3 Al in aluminum powder 2 O 3 The content is more than or equal to 98wt percent.
9. The method for producing the anti-sticking material sagger for the production of the ternary cathode material as claimed in claim 1, wherein: the alpha-Al 2 O 3 The grain diameter of the aluminum powder is less than or equal to 0.10mm.
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