CN113416068A - Double-layer composite structure sagger for lithium battery positive electrode material and preparation method thereof - Google Patents

Double-layer composite structure sagger for lithium battery positive electrode material and preparation method thereof Download PDF

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Publication number
CN113416068A
CN113416068A CN202110775371.7A CN202110775371A CN113416068A CN 113416068 A CN113416068 A CN 113416068A CN 202110775371 A CN202110775371 A CN 202110775371A CN 113416068 A CN113416068 A CN 113416068A
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parts
sagger
lithium battery
green body
layer
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王泽宇薪
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Yangquan Yinyu New Material Co ltd
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Yangquan Yinyu New Material Co ltd
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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
    • C04B35/01—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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    • C04B35/01—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
    • C04B35/03—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
    • C04B35/04—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
    • C04B35/043—Refractories from grain sized mixtures
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    • 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
    • C04B35/195—Alkaline earth aluminosilicates, e.g. cordierite or anorthite
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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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    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • C04B2235/3222—Aluminates other than alumino-silicates, e.g. spinel (MgAl2O4)
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    • 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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    • C04B2235/349—Clays, e.g. bentonites, smectites such as montmorillonite, vermiculites or kaolines, e.g. illite, talc or sepiolite
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    • C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
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Abstract

The invention relates to the technical field of sagger kiln furniture preparation, and provides a sagger with a double-layer composite structure for a lithium battery positive electrode material and a preparation method thereof. The double-layer composite structure sagger for the lithium battery anode material comprises an inner layer and an outer layer. The preparation method of the sagger with the double-layer composite structure for the lithium battery anode material comprises the steps of preparing an outer-layer structure green body, preparing an inner-layer structure green body, processing and forming, drying, sintering at high temperature and the like. The sagger with the double-layer composite structure for the lithium battery positive electrode material, which is prepared by the method, has the advantages of good corrosion resistance, more recycling times, long service life, smaller thermal expansion coefficient, excellent thermal shock stability and certain bearing strength, and the sagger is easy to strip when the positive electrode material is in contact with the sagger, so that the sagger is not peeled, does not drop slag and is pollution-free in the using process, thereby being suitable for the sintering process of various lithium battery positive electrode materials, being beneficial to reducing the production cost and improving the economic benefit.

Description

Double-layer composite structure sagger for lithium battery positive electrode material and preparation method thereof
Technical Field
The invention relates to the technical field of sagger kiln furniture preparation, in particular to a sagger for a lithium battery positive electrode material and a preparation method thereof.
Background
Sagger is one of important kiln furniture for sintering lithium battery anode materials. The cathode materials of various lithium batteries are loaded into a sagger and then loaded into a high-temperature kiln for roasting. At present, the domestic sagger still has a larger difference with the similar products abroad in the aspects of cycle service life, erosion resistance, thermal shock stability, material bearing strength and the like, the cost for replacing the sagger every year is huge, and meanwhile, the environmental pollution is also caused.
The conventional sagger is generally of two structures, one structure is made of a composite material with a single structure, but the sagger can be corroded and permeated by a lithium battery anode material after being used, so that a small amount of anode material is remained on the surface of the sagger, the sagger cannot be repeatedly used, and the sagger becomes industrial waste; the other structure is a double-layer structure, namely, the surface of the substrate layer is sprayed, but after the structure is reused for a certain number of times, the physical and chemical properties of the sprayed layer on the surface of the sagger and the substrate are changed, the surface of the sagger begins to peel off, the product quality is influenced, and safety accidents are easily caused.
Therefore, in order to meet the demand of the lithium battery cathode material which is increasingly demanded, a novel sagger must be developed, so that the sagger has good erosion resistance, a small thermal expansion coefficient, excellent thermal shock stability and enough strength, the cathode material is easy to peel off when contacting with the sagger, the sagger does not peel off, the sagger does not drop slag, and the product is not easy to pollute. In view of the above problems, a sagger for a lithium battery positive electrode material is developed to have the excellent performance close to or as described above, and has important significance and industrial value.
Disclosure of Invention
The invention aims to provide a sagger with a double-layer composite structure for a lithium battery anode material, wherein the sagger has good corrosion resistance, smaller thermal expansion coefficient, excellent thermal shock stability and enough strength, the anode material is easy to strip when contacting with the sagger, the sagger does not peel, does not drop slag and is pollution-free in the using process, and most importantly, the service life is super-long, and the reusability is far beyond the same products in the market at present.
The invention also aims to provide a preparation method of the sagger with the double-layer composite structure for the lithium battery cathode material. The sagger with the double-layer composite structure prepared by the preparation method has excellent heat conductivity coefficient, the inner layer and the outer layer are tightly combined, the thermal expansion coefficient is similar, and the sagger can repeatedly performThe high-temperature sintering and cooling circulation of the alloy does not peel or drop slag, has excellent corrosion resistance, and can effectively resist Li in a high-temperature environment+And the like.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a sagger with a double-layer composite structure for a lithium battery anode material, which comprises an outer layer and an inner layer;
the outer layer comprises the following raw materials in parts by weight: 25-40 parts of cordierite, 20-40 parts of mullite, 5-20 parts of aluminum powder, 5-20 parts of clay and 5-10 parts of pulp waste liquid;
the inner layer comprises the following raw materials in parts by weight: 50-70 parts of tabular corundum, 10-20 parts of high-purity silicon nitride powder, 5-15 parts of zirconia, 5-15 parts of magnesia-alumina spinel, 5-15 parts of clay, 4-6 parts of carboxymethyl cellulose (CMC) and 5-10 parts of a binder.
A preparation method of a double-layer structure composite sagger for a lithium battery anode material comprises the following steps:
preparing an outer layer structure green body: uniformly mixing 25-40 parts of crushed cordierite, 20-40 parts of mullite and 5-10 parts of paper pulp waste liquid until the surfaces of dry particles are wetted, adding 5-20 parts of aluminum powder and 5-20 parts of clay into the mixed aggregate under an ultrasonic condition, mixing for 40-60min and ageing for 16-20h, and preparing an outer-layer structure green body by adopting a grouting forming method or an extrusion forming method;
preparing an inner layer structure green body: under the ultrasonic condition, uniformly mixing 50-70 parts of tabular corundum, 10-20 parts of high-purity silicon nitride powder, 5-15 parts of zirconia, 5-15 parts of magnesia alumina spinel, 5-15 parts of clay and 4-6 parts of carboxymethyl cellulose (CMC) for 20-40min for ageing, and then preparing an inner-layer structure green body by adopting a slip casting method or an extrusion molding method;
and (3) processing and forming: after the high-temperature-resistant inorganic adhesive is uniformly coated on the inner surface of the outer-layer structure green body, embedding the inner-layer structure green body into the outer-layer structure green body, and performing compression molding again through molding equipment to obtain a product green body;
drying and high-temperature sintering: and (3) placing the product green body in a drying room at 100 ℃ for drying for 12 hours, and sintering in a high-temperature furnace at 1250-1350 ℃ for 3-5 hours to obtain the sagger with the double-layer composite structure for the lithium battery cathode material.
The double-layer composite structure sagger for the lithium battery anode material and the preparation method thereof have the beneficial effects that: the sagger has the advantages of good corrosion resistance, small thermal expansion coefficient, excellent thermal shock stability and certain strength, and the anode material is easy to strip off when contacting with the sagger, the sagger does not peel off and slag in the using process, and is pollution-free, most importantly, the service life is super long, and the repeated use times of the sagger is far beyond the similar products on the market at present.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In recent ten years, with the improvement of environmental protection consciousness of countries in the world, people begin to search clean energy which is friendly to the environment, and the development of new energy is promoted. Lithium ion batteries are one such clean energy source. Lithium ion batteries are a type of battery using a nonaqueous electrolyte solution with lithium metal or a lithium alloy as a negative electrode material. Because the chemical properties of lithium metal are very active and the charge and discharge capacities are superior to those of traditional batteries, the lithium ion battery has become the mainstream of the battery manufacturing field along with the development of scientific technology. The sagger is one of important kiln furniture for firing the lithium battery anode material, and various lithium battery anode materials are loaded into the sagger and then loaded into a high-temperature kiln for roasting.
The sagger for roasting the anode material of the lithium ion battery is made of various raw materials, but the main raw materials are mullite, cordierite and magnesia-alumina spinel, and some plastic bonding materials such as dextrin, pulp waste liquid and the like.
Cordierite is a chemical compositionIs silicate mineral rich in iron, magnesium and aluminum, and has standard chemical formula of Mg2Al4Si5O18. Cordierite has good thermal shock stability, lower thermal conductivity, and excellent performances of low dielectric constant, small dielectric loss, high chemical stability and the like, but the material strength is low. In the sagger preparation process, the thermal shock stability of the sagger can be improved by adding cordierite.
Mullite with a standard chemical formula of 3Al2O3·2SiO2The material is orthorhombic, is columnar or acicular crystal, has melting temperature of about 1850 ℃, has good high-temperature strength and thermal shock stability, is widely applied to the industry as a refractory material with excellent performance, is one of main raw materials for preparing saggars, and provides enough high-temperature strength for the saggars.
The magnesia-alumina spinel belongs to a cubic crystal system, is doped with magnesia-alumina spinel and has higher corrosion resistance.
Si3N4The material has excellent physical and chemical properties, has the characteristics of high strength and high temperature resistance, has extremely excellent comprehensive mechanical properties in ceramic materials, has extremely excellent thermal shock resistance, wear resistance, oxidation resistance and acid-base corrosion resistance, can be rapidly cooled and then rapidly heated in a high-temperature environment of more than 1000 ℃, can not be cracked, and shows extremely strong cold and hot impact resistance.
The plate-like corundum is a pure sintered corundum which is completely sintered and shrunk without adding any additive such as MgO and the like, has coarse crystals and good development alpha-Al2O3Crystal structure of Al2O3The content of the high-temperature-resistant refractory material or castable is more than 99 percent, has a plate-shaped crystal structure, small air holes, more closed air holes, a porosity which is approximately equal to that of the fused corundum, high purity, good volume stability and extremely small re-sintering shrinkage, has good thermal shock stability and bending strength after being treated at high temperature, and has the characteristics of high refractoriness, high corrosion resistance, high scouring resistance, high thermal shock resistance, good strength and toughness and stable chemical performance.
The zirconia is an important high-temperature resistant material, has the excellent characteristics of high melting point, no oxidation and other high temperatures, has stable high-temperature chemical properties, corrosion resistance, oxidation resistance, thermal shock resistance, non-volatility and no pollution, and is a refractory material which is top internationally at present.
The adhesive is a high-temperature-resistant inorganic adhesive, has strong adhesive force and no corrosiveness, can keep good adhesive property and corrosion resistance at high temperature, has long service life, and has good effect on tight adhesion of the inner layer and the outer layer of the sagger. The XZ-T002 is widely applied to ceramic and metal products. The product is dried and formed at normal temperature when in use, and the hardness after drying and forming can reach more than 5H.
The following describes a method for preparing a sagger with a double-layer composite structure for a lithium battery cathode material according to an embodiment of the present invention.
A preparation method of a sagger with a double-layer composite structure for a lithium battery anode material comprises an outer layer and an inner layer;
the outer layer comprises the following raw materials in parts by weight: 25-40 parts of cordierite, 20-40 parts of mullite, 5-20 parts of aluminum powder, 5-20 parts of clay and 5-10 parts of pulp waste liquid;
furthermore, the particle size of cordierite particles is 0.3-2.5 mm; the granularity of mullite particles is 1-2.5mm, the granularity of aluminum powder is 325 meshes, and the aluminum content is more than or equal to 97 percent;
further, the clay is one of Guangxi white mud or Suzhou white mud;
the inner layer comprises the following raw materials in parts by weight: 50-70 parts of tabular corundum, 10-20 parts of high-purity silicon nitride powder, 5-15 parts of zirconia, 5-15 parts of magnesia-alumina spinel, 5-15 parts of clay, 4-6 parts of carboxymethyl cellulose (CMC) and 5-10 parts of a binder;
further, the granularity of the plate-shaped corundum is 0.5-2 mm; the grain diameter of the silicon nitride powder is 0.1-0.5mm, the grain diameter of the zirconia is 325 meshes, and the grain diameter of the magnesia-alumina spinel is 2 mm;
further, the adhesive is a high temperature resistant inorganic adhesive.
A preparation method of a sagger with a double-layer composite structure for a lithium battery positive electrode material comprises the following steps:
preparing an outer layer structure green body: uniformly mixing 25-40 parts of crushed cordierite, 20-40 parts of mullite and 5-10 parts of paper pulp waste liquid until the surfaces of dry particles are wetted, adding 5-20 parts of aluminum powder and 5-20 parts of clay into the mixed aggregate under an ultrasonic condition, mixing for 40-60min and ageing for 16-20h, and preparing an outer-layer structure green body by adopting a grouting forming method or an extrusion forming method;
furthermore, the particle size of cordierite particles is 0.3-2.5 mm; the particle size of mullite particles is 1-2.5mm, the particle size of aluminum powder is 325 meshes, the aluminum content is more than or equal to 97 percent, and the clay is one of Guangxi white mud or Suzhou white mud;
further, the ultrasonic treatment time is 50min, and the intensity is 0.5-1.2W/cm2The materials can be mixed more uniformly by ultrasonic treatment, the contact surface area between the materials is larger, the materials are easier to compact in the forming process, the outer layer structure of the manufactured sagger is more compact, and the thermal shock stability and the erosion resistance are stronger;
further, the mixing time was 50 min; the aging time is 18 h.
Preparing an inner layer structure green body: under the ultrasonic condition, uniformly mixing 50-70 parts of tabular corundum, 10-20 parts of high-purity silicon nitride powder, 5-15 parts of zirconia, 5-15 parts of magnesia alumina spinel, 5-15 parts of clay and 4-6 parts of carboxymethyl cellulose (CMC) for 20-40min for ageing, and then preparing an inner-layer structure green body by adopting a slip casting method or an extrusion molding method;
further, the granularity of the plate-shaped corundum is 0.5-2 mm; the grain diameter of the silicon nitride powder is 0.1-0.5mm, the grain diameter of the zirconia is 325 meshes, and the grain diameter of the magnesia-alumina spinel is 2 mm; si3N4The material has excellent physical and chemical properties, has the characteristics of high strength and high temperature resistance, has extremely excellent comprehensive mechanical properties in ceramic materials, has extremely excellent thermal shock resistance, wear resistance, oxidation resistance and acid-base corrosion resistance, can be rapidly cooled and then rapidly heated in a high-temperature environment of more than 1000 ℃, can not be cracked, and shows extremely strong cold and hot impact resistance;
further, the ultrasonic treatment time is 30min, and the intensity is 0.5-1.2W/cm2；
Further, the mixing time was 30 min; the staling time is 12 h.
And (3) processing and forming: after the high-temperature-resistant inorganic adhesive is uniformly coated on the inner surface of the outer-layer structure green body, embedding the inner-layer structure green body into the outer-layer structure green body, and performing compression molding again through molding equipment to obtain a product green body;
furthermore, the adhesive is a high-temperature-resistant inorganic adhesive, so that the adhesive is strong in bonding force and free of corrosion, can keep good bonding performance and corrosion resistance at high temperature, is long in service life, and has a good effect on tight bonding of the inner layer and the outer layer of the sagger;
further, the outer diameter of the green inner structure is equal to the inner diameter of the green outer structure.
Drying and high-temperature sintering: and (3) placing the product green body in a drying room at 100 ℃ for drying for 12 hours, and sintering in a high-temperature furnace at 1250-1350 ℃ for 3-5 hours to obtain the sagger with the double-layer composite structure for the lithium battery cathode material.
Further, the temperature of the high-temperature sintering is 1295 ℃ and the time is 4 hours.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The sagger with the double-layer composite structure for the lithium battery cathode material provided by the embodiment comprises an outer layer and an inner layer;
the outer layer raw material comprises the following components: 25kg of cordierite, 40kg of mullite, 5kg of aluminum powder, 20kg of clay and 5kg of pulp waste liquid;
wherein the particle size of cordierite particles is 0.3-2.5 mm; the particle size of mullite particles is 1-2.5mm, the particle size of aluminum powder is 325 meshes, the aluminum content is more than or equal to 97 percent, and the clay is one of Guangxi white mud or Suzhou white mud;
the inner layer raw material comprises the following components: 50kg of tabular corundum, 20kg of high-purity silicon nitride powder, 5kg of zirconia, 15kg of magnesia alumina spinel, 5kg of clay, 4kg of carboxymethyl cellulose (CMC), 10kg of a binder;
wherein, the granularity of the plate-shaped corundum is 0.5-2 mm; the grain diameter of the silicon nitride powder is 0.1-0.5mm, the grain diameter of the zirconia is 325 meshes, the grain diameter of the magnesia-alumina spinel is 2mm, and the adhesive is a high-temperature resistant inorganic adhesive XZ-T002;
the embodiment also provides a preparation method of the double-layer composite structure sagger for the lithium battery cathode material, which comprises the following steps:
preparing an outer layer structure green body: uniformly mixing 25kg of crushed cordierite with the particle size of 0.3-2.5mm, 40kg of mullite with the particle size of 1-2.5mm and 5kg of paper pulp waste liquid until the surfaces of dried particles are wetted to prepare mixed aggregate, adding 5kg of aluminum powder with the particle size of 325 meshes and the aluminum content of more than or equal to 97 percent and 20kg of clay into the mixed aggregate, and adding the mixture into the mixed aggregate at the strength of 0.5-1.2W/cm2Mixing for 50min under the action of ultrasonic waves, ageing the mixed material for 18h, and preparing an outer-layer structure green body by adopting a grouting forming method or an extrusion forming method;
preparing an inner layer structure green body: under the ultrasonic condition, 50kg of tabular corundum with the particle size of 0.5-2mm, 20kg of high-purity silicon nitride powder with the particle size of 0.1-0.5mm, 5kg of zirconia with the particle size of 0.5-2mm, 15kg of magnesia-alumina spinel with the particle size of 2mm, 5kg of clay and 4kg of carboxymethyl cellulose (CMC) are added under the condition that the strength is 0.5-1.2W/cm2Uniformly mixing for 30min under the action of ultrasonic waves, ageing the mixed material for 12h, and preparing an inner-layer structure green body by adopting a grouting forming method or an extrusion forming method, wherein the outer diameter of the inner-layer structure green body is equal to the inner diameter of the outer-layer structure green body;
and (3) processing and forming: uniformly coating 10kg of high-temperature-resistant inorganic adhesive on the inner surface of the outer-layer structure green body, embedding the inner-layer structure green body into the outer-layer structure green body, and performing compression molding again through molding equipment to obtain a product green body;
drying and high-temperature sintering: and (3) drying the product green body in a drying room at 100 ℃ for 12 hours, and sintering the product green body in a high-temperature furnace at 1295 ℃ for 4 hours to obtain the sagger with the double-layer composite structure for the lithium battery cathode material.
Example 2
The sagger with the double-layer composite structure for the lithium battery cathode material provided by the embodiment comprises an outer layer and an inner layer;
the outer layer raw material comprises the following components: 40kg of cordierite, 20kg of mullite, 20kg of aluminum powder, 5kg of clay and 10kg of pulp waste liquid;
wherein the particle size of cordierite particles is 0.3-2.5 mm; the particle size of mullite particles is 1-2.5mm, the particle size of aluminum powder is 325 meshes, the aluminum content is more than or equal to 97 percent, and the clay is one of Guangxi white mud or Suzhou white mud;
the inner layer raw material comprises the following components: 70kg of tabular corundum, 10kg of high-purity silicon nitride powder, 15kg of zirconia, 5kg of magnesia alumina spinel, 15kg of clay, 6kg of carboxymethylcellulose (CMC), 5kg of a binder;
wherein, the granularity of the plate-shaped corundum is 0.5-2 mm; the particle size of the silicon nitride powder is 0.1-0.5mm, the particle size of the zirconia is 325 meshes, the particle size of the magnesia-alumina spinel is 2mm, and the adhesive is a high-temperature resistant inorganic adhesive with the model of XZ-T002;
the embodiment also provides a preparation method of the double-layer composite structure sagger for the lithium battery cathode material, which comprises the following steps:
preparing an outer layer structure green body: uniformly mixing 40kg of crushed cordierite with the particle size of 0.3-2.5mm, 20kg of mullite with the particle size of 1-2.5mm and 10kg of paper pulp waste liquid until the surfaces of dried particles are wetted to prepare mixed aggregate, adding 20kg of aluminum powder with the particle size of 325 meshes and the aluminum content of more than or equal to 97 percent and 5kg of clay into the mixed aggregate, and adding the mixture into the mixed aggregate at the strength of 0.5-1.2W/cm2Mixing for 50min under the action of ultrasonic waves, ageing the mixed material for 18h, and preparing an outer-layer structure green body by adopting a grouting forming method or an extrusion forming method;
preparing an inner layer structure green body: under the ultrasonic condition, 70kg of tabular corundum with the particle size of 0.5-2mm, 10kg of high-purity silicon nitride powder with the particle size of 0.1-0.5mm, 15kg of zirconia with the particle size of 0.5-2mm, 5kg of magnesia-alumina spinel with the particle size of 2mm, 15kg of clay and 6kg of carboxymethyl cellulose (CMC) are subjected to ultrasonic treatment at the intensity of 0.5-1.2W/cm2Uniformly mixing for 30min under the action of ultrasonic waves, ageing the mixed material for 12h, and preparing an inner-layer structure green body by adopting a grouting forming method or an extrusion forming method, wherein the outer diameter of the inner-layer structure green body is equal to the inner diameter of the outer-layer structure green body;
and (3) processing and forming: uniformly coating 5kg of high-temperature-resistant inorganic adhesive on the inner surface of the outer-layer structure green body, embedding the inner-layer structure green body into the outer-layer structure green body, and performing compression molding again through molding equipment to obtain a product green body;
drying and high-temperature sintering: and (3) drying the product green body in a drying room at 100 ℃ for 12 hours, and sintering the product green body in a high-temperature furnace at 1295 ℃ for 4 hours to obtain the sagger with the double-layer composite structure for the lithium battery cathode material.
Example 3
The sagger with the double-layer composite structure for the lithium battery cathode material provided by the embodiment comprises an outer layer and an inner layer;
the outer layer raw material comprises the following components: 32kg of cordierite, 30kg of mullite, 12kg of aluminum powder, 12kg of clay and 8kg of pulp waste liquid;
wherein the particle size of cordierite particles is 0.3-2.5 mm; the particle size of mullite particles is 1-2.5mm, the particle size of aluminum powder is 325 meshes, the aluminum content is more than or equal to 97 percent, and the clay is one of Guangxi white mud or Suzhou white mud;
the inner layer raw material comprises the following components: 60kg of tabular corundum, 15kg of high-purity silicon nitride powder, 10kg of zirconia, 10kg of magnesia alumina spinel, 10kg of clay, 5kg of carboxymethyl cellulose (CMC), 8kg of a binder;
wherein, the granularity of the plate-shaped corundum is 0.5-2 mm; the grain diameter of the silicon nitride powder is 0.1-0.5mm, the grain diameter of the zirconia is 325 meshes, the grain diameter of the magnesia-alumina spinel is 2mm, and the adhesive is a high-temperature resistant inorganic adhesive XZ-T002;
the embodiment also provides a preparation method of the double-layer composite structure sagger for the lithium battery cathode material, which comprises the following steps:
preparing an outer layer structure green body: uniformly mixing 32kg of crushed cordierite with the particle size of 0.3-2.5mm, 30kg of mullite with the particle size of 1-2.5mm and 8kg of paper pulp waste liquid until the surfaces of dried particles are wetted to prepare mixed aggregate, adding 12kg of aluminum powder with the particle size of 325 meshes and the aluminum content of more than or equal to 97 percent and 12kg of clay into the mixed aggregate, and adding the mixture into the mixed aggregate at the strength of 0.5-1.2W/cm2Mixing for 50min under the action of ultrasonic waves, ageing the mixed material for 18h, and preparing an outer-layer structure green body by adopting a grouting forming method or an extrusion forming method;
preparing an inner layer structure green body: under the ultrasonic condition, 60kg of tabular corundum with the particle size of 0.5-2mm and the particle size of15kg of high-purity silicon nitride powder with the particle size of 0.1-0.5mm, 10kg of zirconia with the particle size of 0.5-2mm, 10kg of magnesia alumina spinel with the particle size of 2mm, 10kg of clay and 5kg of carboxymethyl cellulose (CMC) with the strength of 0.5-1.2W/cm2Uniformly mixing for 30min under the action of ultrasonic waves, ageing the mixed material for 12h, and preparing an inner-layer structure green body by adopting a grouting forming method or an extrusion forming method, wherein the outer diameter of the inner-layer structure green body is equal to the inner diameter of the outer-layer structure green body;
and (3) processing and forming: uniformly coating 8kg of high-temperature-resistant inorganic adhesive on the inner surface of the outer-layer structure green body, embedding the inner-layer structure green body into the outer-layer structure green body, and performing compression molding again through molding equipment to obtain a product green body;
drying and high-temperature sintering: and (3) drying the product green body in a drying room at 100 ℃ for 12 hours, and sintering the product green body in a high-temperature furnace at 1295 ℃ for 4 hours to obtain the sagger with the double-layer composite structure for the lithium battery cathode material.
Comparative example 1
Compared with example 3, the main differences are that: a single layer structure sagger without an inner layer;
the raw materials comprise the following components: 32kg of cordierite, 30kg of mullite, 12kg of aluminum powder, 12kg of clay and 8kg of pulp waste liquid;
wherein the particle size of cordierite particles is 0.3-2.5 mm; the particle size of mullite particles is 1-2.5mm, the particle size of aluminum powder is 325 meshes, the aluminum content is more than or equal to 97 percent, and the clay is one of Guangxi white mud or Suzhou white mud;
the comparative example also provides a preparation method of the sagger for the lithium battery positive electrode material, which comprises the following steps:
preparing a green body: uniformly mixing 32kg of crushed cordierite with the particle size of 0.3-2.5mm, 30kg of mullite with the particle size of 1-2.5mm and 8kg of paper pulp waste liquid until the surfaces of dried particles are wetted to prepare mixed aggregate, adding 12kg of aluminum powder with the particle size of 325 meshes and the aluminum content of more than or equal to 97 percent and 12kg of clay into the mixed aggregate, and adding the mixture into the mixed aggregate at the strength of 0.5-1.2W/cm2Mixing for 50min under the action of ultrasonic waves, ageing the mixed material for 18h, and preparing a sagger product green body by adopting a grouting forming method or an extrusion forming method;
drying and high-temperature sintering: and (3) drying the product green body in a drying room at 100 ℃ for 12 hours, and sintering the product green body in a high-temperature furnace at 1295 ℃ for 4 hours to obtain the sagger for the lithium battery positive electrode material.
Test examples
Service life performance tests were conducted on the saggars prepared in inventive examples 1 to 3 and comparative example 1, respectively, for calcination synthesis of a 333 (in order of nickel, cobalt, and manganese) type ternary material for a nickel-cobalt-manganese-lithium ion battery, the service life of each of the saggars was determined based on occurrence of fracture of the saggar to cause partial falling and breakage of the saggar, and the surface state of the saggars after 15 times of use was observed, and the test results are shown in table 1.
TABLE 1 results of performance test of sagger prepared in examples 1-3 and comparative example 1
Serial number Service life (times) Surface condition of saggar after 15 times of use
Example 1 45 No crack, no drop, no damage
Example 2 48 No crack, no drop, no damage
Example 3 55 No crack, no drop, no damage
Comparative example 1 15 No crack, no drop, no damage
After long-term use, the sagger prepared by the method has no problems of peeling, slag falling, pollution to fired materials and the like, has the service life of more than 45 times (ternary material 333), and is far more than the traditional mullite-cordierite sagger on the market.
The test results show that the used times of the saggars prepared by the raw materials and the method are obviously higher than the times of common use in the prior industry. The sagger has good high-temperature corrosion resistance in the using process, has no surface shedding phenomenon after repeated use, obviously improves the quality and stability of products, and is beneficial to the improvement of the production benefit of enterprises.
In summary, according to the sagger with the double-layer composite structure for the lithium battery cathode material and the preparation method thereof provided by the embodiment of the invention, the service life of the sagger is greatly prolonged as the sagger with the double-layer composite structure with different inner and outer layers is designed, and the sagger is formed by tightly combining a novel high-temperature-resistant inorganic adhesive and then punching and firing the mixture; due to the ultrasonic action added during the material mixing, the materials are mixed more uniformly, and the sagger has better structural strength and corrosion resistance; addition of Si to the inner layer composition3N4The high-temperature resistant material obviously enhances the erosion resistance of the inner layer of the sagger, thereby greatly prolonging the service life of the sagger, improving the quality and stability of products and being beneficial to the improvement of the production benefit of enterprises.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Claims (6)

1. A sagger with a double-layer composite structure for a lithium battery anode material is characterized by comprising an outer layer and an inner layer;
the outer layer comprises the following raw materials in parts by weight: 25-40 parts of cordierite, 20-40 parts of mullite, 5-20 parts of aluminum powder, 5-20 parts of clay and 5-10 parts of pulp waste liquid;
the inner layer comprises the following raw materials in parts by weight: 50-70 parts of tabular corundum, 10-20 parts of high-purity silicon nitride powder, 5-15 parts of zirconia, 5-15 parts of magnesia-alumina spinel, 5-15 parts of clay, 4-6 parts of carboxymethyl cellulose (CMC) and 5-10 parts of a binder.
2. The sagger with the double-layer composite structure for the positive electrode material of the lithium battery as claimed in claim 1, wherein the cordierite particle size is 0.3-2.5 mm; the granularity of the mullite particles is 1-2.5mm, the particle size of the aluminum powder is 325 meshes, and the aluminum content is more than or equal to 97 percent.
3. The sagger with the double-layer composite structure for the lithium battery positive electrode material as claimed in claim 1, wherein the plate-shaped corundum has a particle size of 0.5-2 mm; the particle size of the silicon nitride powder is 0.1-0.5mm, the particle size of the zirconia is 325 meshes, and the particle size of the magnesia-alumina spinel is 2 mm.
4. The sagger with the double-layer composite structure for the positive electrode material of the lithium battery as claimed in claim 1, wherein the clay is one of Guangxi white mud and Suzhou white mud.
5. The sagger with the double-layer composite structure for the positive electrode material of the lithium battery as claimed in claim 1, wherein the binder is a high-temperature-resistant inorganic binder.
6. A method for preparing a sagger with a double-layer composite structure for a positive electrode material of a lithium battery as defined in any one of claims 1 to 5, comprising:
preparing an outer layer structure green body: uniformly mixing 25-40 parts of crushed cordierite, 20-40 parts of mullite and 5-10 parts of paper pulp waste liquid until the surfaces of dry particles are wetted, adding 5-20 parts of aluminum powder and 5-20 parts of clay into the mixed aggregate under an ultrasonic condition, mixing for 40-60min and ageing for 16-20h, and then preparing an outer-layer structure green body by adopting a grouting forming method or an extrusion forming method;
preparing an inner layer structure green body: under the ultrasonic condition, uniformly mixing 50-70 parts of tabular corundum, 10-20 parts of high-purity silicon nitride powder, 5-15 parts of zirconia, 5-15 parts of magnesia alumina spinel, 5-15 parts of clay and 4-6 parts of carboxymethyl cellulose (CMC) for 20-40min for ageing, and then preparing an inner-layer structure green body by adopting a slip casting method or an extrusion molding method;
and (3) processing and forming: uniformly coating a high-temperature-resistant inorganic adhesive on the inner surface of the outer-layer structure green body, embedding the inner-layer structure green body into the outer-layer structure green body, and performing compression molding again through molding equipment to obtain a product green body;
drying and high-temperature sintering: and (3) drying the product green body in a drying room at 100 ℃ for 12 hours, and sintering in a high-temperature furnace at 1250-1350 ℃ for 3-5 hours to obtain the sagger with the double-layer composite structure for the lithium battery cathode material.
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