CN114349484B - Ceramic material for calcining electrode material of lithium battery and preparation method thereof - Google Patents
Ceramic material for calcining electrode material of lithium battery and preparation method thereof Download PDFInfo
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- CN114349484B CN114349484B CN202111628461.XA CN202111628461A CN114349484B CN 114349484 B CN114349484 B CN 114349484B CN 202111628461 A CN202111628461 A CN 202111628461A CN 114349484 B CN114349484 B CN 114349484B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention relates to a ceramic material, in particular to an electrode material for a lithium battery, which is prepared from the following raw materials in parts by weight: 0.5 to 5 parts of lithium carbonate; 1-7 parts of silicon micropowder; 0.5 to 3 portions of titanium dioxide; 5-10 parts of electric smelting monoclinic zirconium powder; the balance of 75-93 parts of alumina micropowder. The ceramic material for calcining the electrode material of the lithium battery has the advantages of excellent thermal shock property, high-temperature alkali corrosion resistance, small apparent porosity and long service life.
Description
Technical Field
The invention relates to a ceramic material, in particular to a ceramic material for calcining an electrode material of a lithium battery and a preparation method thereof.
Background
The lithium ion battery is a new generation secondary battery with highest energy density at present, is widely applied to the fields of mobile communication, new energy sources and the like, and has huge development space in the future. The positive electrode material is the core material of lithium ion battery, the output of lithium iron phosphate, lithium cobalt oxide and ternary positive electrode materials (LNCM, LNCA) in China are all the first world, wherein the ternary positive electrode material is the development direction of several years in the future, in particular to a high-nickel ternary positive electrode material (LiNi 1-x-y Co x Mn y O 2 Wherein Ni>0.8 Is developed rapidly.
The ceramic sagger is mainly calcined, the average service life of the current sagger is 10-15 times (the current life can reach about 36 times at most), slight peeling starts to appear after the current sagger is generally recycled for about 4 times, and then the current sagger is gradually increased until the current sagger is scrapped, and the erosion resistance of the current sagger can not meet the actual requirement of the development of the positive electrode material. In addition, the used sagger is adhered with metal compounds such as lithium, cobalt, manganese, nickel and the like, and the solid waste has great harm to the ecological environment. The materials are removed to realize the reutilization of the sagger, so that the cost is high, and the economic benefit is difficult to generate.
Disclosure of Invention
In order to solve the problems, the invention provides a ceramic material with good alkali erosion resistance and long service life for calcining an electrode material of a lithium battery, which comprises the following specific technical scheme:
the ceramic material for calcining the electrode material of the lithium battery is characterized by being prepared from the following raw materials in parts by weight: 0.5 to 5 parts of lithium carbonate; 1-7 parts of silicon micropowder; 0.5 to 3 portions of titanium dioxide; 5-10 parts of electric smelting monoclinic zirconium powder; the balance of 75-93 parts of alumina micropowder.
Preferably, the molar ratio of lithium carbonate to the silicon micropowder is 1:1.
Preferably, the mass of the titanium dioxide is 1-3% of that of the alumina powder.
Preferably, the electric smelting monoclinic zirconium powder is micron-sized electric smelting monoclinic zirconium powder.
A method for preparing a ceramic material for calcination of lithium battery electrode materials, comprising the following steps:
preparing a pre-synthesized material, dry-grinding and mixing lithium carbonate, silicon micropowder and alumina micropowder according to a molar ratio of 1:1:2, and calcining to obtain the pre-synthesized material;
and (3) batching: 5 to 15 parts of pre-synthesized material, 0.5 to 3 parts of titanium dioxide, 5 to 10 parts of micron-sized electric smelting monoclinic zirconium powder and 70 to 85 parts of alumina micro powder;
ball milling;
granulating by spraying;
isostatic compaction;
sintering, and preserving heat for 3-8 h at 1580-1620 ℃ to obtain the ceramic material.
Preferably, the calcination temperature is 650-750 ℃ when preparing the pre-synthesized material.
Preferably, during sintering, the temperature is firstly increased to 300 ℃ at a heating rate of 0.5 ℃/min, then is increased to 1580-1620 ℃ at a heating rate of 1 ℃/min, and is naturally cooled after heat preservation for 3-8 h.
Preferably, the ceramic material has a apparent porosity of less than 0.5%, a density of 3.4-3.6 g/cm < 3 >, and a micron-sized closed porosity of 6% -11%.
Preferably, after the ceramic material is subjected to air cooling circulation for 10-30 times at 1100 ℃ to room temperature, the flexural strength of the ceramic material is increased to more than 200 MPa.
Compared with the prior art, the invention has the following beneficial effects:
the ceramic material for calcining the electrode material of the lithium battery has the advantages of excellent thermal shock property, high-temperature alkali corrosion resistance, small apparent porosity and long service life.
Drawings
FIG. 1 is an electron microscopic image of the ceramic material of the present embodiment at a magnification of 100;
fig. 2 is an electron microscopic image of the ceramic material of the present embodiment at a magnification of 1000.
Detailed Description
The invention will now be further described with reference to the accompanying drawings.
The sagger which is widely used in China at present is made of cordierite-mullite, magnesia-alumina spinel-cordierite, silicon carbide and the like, and the service life of the sagger is short. According to research on exfoliation, when the lithium ion battery anode material is synthesized, the raw materials are decomposed to generate lithium oxide in the calcining synthesis process, and the lithium oxide has the characteristics of strong permeability and high reactivity, can accelerate corrosion to the sagger, and is mainly used for preparing the lithium oxide and cordierite (Mg 2 Al 4 Si 5 O 18 ) Mullite (Al) 6 Si 2 O 13 ) The reaction to generate LiAlSiO 4 、LiAlO 2 、Li 2 SiO 3 Substances such as Al and Si, which can react with the elements such as Al and Si continuously with the progress of the heat preservation time, and finally LiAlSiO is generated 4 、LiAlSi 2 O 6 And the like, the generation of these phases causes a phenomenon that the erosion layer and the refractory are peeled off due to a difference in thermal expansion coefficient.
The ceramic material for calcining the electrode material of the lithium battery is prepared from the following raw materials in parts by weight: 0.5 to 5 parts of lithium carbonate; 1-7 parts of silicon micropowder; 0.5 to 3 portions of titanium dioxide; 5-10 parts of electric smelting monoclinic zirconium powder; the balance of 75-93 parts of alumina micropowder.
The molar ratio of the lithium carbonate to the silicon micropowder is 1:1. The mass of the titanium dioxide is 1-3% of that of the alumina powder. The electric smelting monoclinic zirconium powder is micron-sized electric smelting monoclinic zirconium powder.
A method for preparing a ceramic material for calcination of lithium battery electrode materials, comprising the following steps:
(1) Firstly, carrying out dry grinding and mixing on lithium carbonate, silicon micropowder and alumina micropowder according to the mol ratio of 1:1:2, and carrying out calcination and presynthesis at 700 ℃;
(2) Adding 5-15 parts of pre-synthesized powder, 0.5-3 parts of titanium dioxide, 5-10 parts of electric smelting zirconia micro powder and 70-85 parts of alumina micro powder according to parts, adding water and a dispersing agent, and performing ball milling for 20 hours;
(3) Adding 1% PVA as an adhesive into the slurry, and performing spray granulation, isostatic compaction and sintering at 1580-1620 ℃ to obtain the required ceramic material.
Firstly, dry-grinding and mixing lithium carbonate and silicon micropowder and alumina micropowder according to the mol ratio of 1:1:2, and calcining and presynthesizing at 700 ℃; and mixing 15% of pre-synthesized powder, 2% of titanium dioxide, 10% of micron-sized fused zirconia micro powder and 73% of alumina micro powder according to the mass ratio, adding 60% of water and 0.2% of ammonium polyacrylate according to the mass ratio, ball-milling for 20 hours in a ball mill, and spray granulating. And (3) molding the prepared granulated powder under the pressure of 100MPa to prepare a test strip and a ceramic plate, placing the test strip and the ceramic plate in a resistance furnace, heating to 300 ℃ at the heating rate of 0.5 ℃/min, heating to 1600 ℃ at the heating rate of 1 ℃/min, preserving heat for 5 hours, and naturally cooling to obtain the ceramic material.
Examples
Firstly, dry-grinding and mixing lithium carbonate and silicon micropowder and alumina micropowder according to the mol ratio of 1:1:2, and calcining and presynthesizing at 700 ℃; and mixing 15% of pre-synthesized powder, 2% of titanium dioxide, 10% of micron-sized fused zirconia micro powder and 73% of alumina micro powder according to the mass ratio, adding 60% of water and 0.2% of ammonium polyacrylate according to the mass ratio, ball-milling for 20 hours in a ball mill, and spray granulating. The prepared granulated powder is molded under the pressure of 100MPa to prepare test strips and ceramic plates, the test strips and the ceramic plates are placed in a resistance furnace, the temperature is firstly increased to 300 ℃ at the heating rate of 0.5 ℃/min, then is increased to 1600 ℃ at the heating rate of 1 ℃/min, and is naturally cooled after being kept for 5 hours.
The sample prepared in this example had a bulk density of 3.590g/cm3 and a apparent porosity of zero. The normal temperature flexural strength is 141MPa, and after the material is subjected to air cooling circulation for 30 times at 1100 ℃ to room temperature, the flexural strength of the material is increased to 264MPa; in the erosion test of the ceramic plate, the temperature is kept at 850 ℃ for 20 hours, li 2 O only slightly reacts on the surface layer of the ceramic material, the thickness of the reaction layer is negligible, and the ceramic material has good high-temperature erosion resistance.
When the electrode material is calcined, a mode similar to a cement rotary kiln is adopted, so that the positive electrode material enters from one end and rolls in the kiln to finish the processes of heating, heat preservation and cooling. The calcining mode has the advantages that in the synthesizing process of the lithium battery material, the powder is gradually and uniformly stirred along with the rotation of the kiln, and compared with the traditional sagger-mounted calcining, the calcining mode has better synthetic material performance and relatively saves energy. The kiln body lining adopting the calcination mode needs to adopt a ceramic material with low porosity, and has good thermal shock resistance and good alkali corrosion resistance. Thereby ensuring the long-time stable operation of the kiln.
As shown in FIGS. 1 and 2, the sample prepared in this example had a bulk density of 3.590g/cm3 and a apparent porosity of zero. The normal temperature flexural strength is 141MPa, and after 30 times of air cooling circulation at 1100 ℃ to room temperature, the flexural strength of the material is increased to 264MPa; in the erosion test of the ceramic plate, the temperature is kept at 850 ℃ for 20 hours, li 2 O only slightly reacts on the surface layer of the ceramic material, the thickness of the reaction layer is negligible, and the ceramic material has good high-temperature erosion resistance and thermal shock resistance. Meanwhile, due to the nearly zero microscopic porosity and the special grain boundary phase, the alkali corrosion and permeation resistance of the alloy at high temperature is improved. Can be used as lining material of alkaline material calciner.
The refractory material formed by the coarse and fine grain composition of the traditional sagger material has higher apparent porosity and poorer bonding strength, has relatively loose structure and is extremely easy to be eroded to generate flaking in the use process. The furnace lining made of the material provided by the embodiment has the characteristics of low apparent porosity, small pore size, high bonding strength, good thermal shock resistance and the like, thereby having certain advantages in erosion resistance and spalling resistance.
The technical principle of the present invention is described above in connection with the specific embodiments. The description is made for the purpose of illustrating the general principles of the invention and should not be taken in any way as limiting the scope of the invention. Other embodiments of the invention will occur to those skilled in the art from consideration of the specification and practice of the invention without the need for inventive faculty, and are within the scope of the claims.
Claims (9)
1. The ceramic material for calcining the electrode material of the lithium battery is characterized by being prepared from the following raw materials in parts by weight:
0.5 to 5 parts of lithium carbonate;
1-7 parts of silicon micropowder;
0.5 to 3 portions of titanium dioxide;
5-10 parts of electric smelting monoclinic zirconium powder;
the balance of 75-93 parts of alumina micropowder.
2. The ceramic material for calcination of lithium battery electrode materials according to claim 1, wherein the molar ratio of lithium carbonate to silica fume is 1:1.
3. The ceramic material for calcination of lithium battery electrode materials according to claim 1, wherein the mass of the titanium pigment is 1-3% of that of the alumina powder.
4. The ceramic material for calcination of lithium battery electrode material according to claim 1, wherein the electrically fused monoclinic zirconium powder is a micron-sized electrically fused monoclinic zirconium powder.
5. A method for preparing a ceramic material for calcination of lithium battery electrode material according to claim 1, comprising the steps of:
preparing a pre-synthesized material, dry-grinding and mixing lithium carbonate, silicon micropowder and alumina micropowder according to a molar ratio of 1:1:2, and calcining to obtain the pre-synthesized material;
and (3) batching: 5 to 15 parts of pre-synthesized material, 0.5 to 3 parts of titanium dioxide, 5 to 10 parts of micron-sized electric smelting monoclinic zirconium powder and 70 to 85 parts of alumina micro powder;
ball milling;
granulating by spraying;
isostatic compaction;
sintering, and preserving heat for 3-8 h at 1580-1620 ℃ to obtain the ceramic material.
6. The method for preparing a ceramic material for calcination of lithium battery electrode material according to claim 5, wherein the calcination temperature is 650-750 ℃ when preparing the pre-synthesized material.
7. The method for preparing the ceramic material for calcining the electrode material of the lithium battery according to claim 5, wherein the sintering is carried out by heating to 300 ℃ at a heating rate of 0.5 ℃/min, heating to 1580-1620 ℃ at a heating rate of 1 ℃/min, and naturally cooling after heat preservation for 3-8 h.
8. The method for preparing the ceramic material for calcining the electrode material of the lithium battery according to claim 5, wherein the ceramic material has a porosity of less than 0.5%, a density of 3.4-3.6 g/cm < 3 >, and a micron-sized closed porosity of 6% -11%.
9. The method for preparing a ceramic material for calcination of lithium battery electrode material according to claim 5, wherein after the ceramic material is subjected to air cooling circulation for 10 to 30 times at 1100 ℃ to room temperature, the flexural strength of the ceramic material is increased to 200MPa or more.
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