CN111848194A - High-strength light spinel hollow ball brick for kiln for producing lithium ion battery anode material and preparation method thereof - Google Patents
High-strength light spinel hollow ball brick for kiln for producing lithium ion battery anode material and preparation method thereof Download PDFInfo
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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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Abstract
A high-strength light spinel hollow ball brick for a lithium battery anode material production kiln is characterized in that a brick body is made of, by weight, 56-65 parts of magnesium aluminate spinel hollow balls, 35-44 parts of matrix powder and 2-6 parts of sintering aids; al in magnesium aluminate spinel hollow sphere2O3More than or equal to 68 percent, MgO more than or equal to 29 percent and grain diameter of 0.2-5 mm; the matrix powder is 325 meshes of rho-Al2O3The powder and 200-mesh light-burned magnesia powder are composed of 1.85:1 by weight, the sintering aid is lanthanum cerium carbonate, and the volume density of the designed magnesium aluminum light spinel hollow ball brick is 0.9-1.65g/cm3(ii) a The prepared lightweight magnesia-alumina spinel brick has excellent erosion resistance and improves the strength of products. The brick body is used for building a kiln, so that the corrosion of the lithium ion anode material can be effectively resisted, the service life of the brick body is prolonged, meanwhile, the brick body is prevented from being peeled off, the quality of the anode material is improved, and the use cost is reduced.
Description
Technical Field
The invention belongs to the technical field of refractory materials, and particularly relates to a high-strength light spinel hollow ball brick for a kiln for producing a lithium ion battery anode material and a preparation method thereof.
Background
The anode material of the lithium ion battery is commonly prepared by a high-temperature solid-phase synthesis method in actual production, and a kiln applied to high-temperature roasting of the lithium ion battery is often corroded and damaged due to the strong corrosion action of lithium oxide steam, so that the lithium ion battery has short service life and high maintenance cost.
The magnesia-alumina spinel ceramic has the advantages of high melting point (2135 ℃), high strength and good chemical erosion resistance, can well meet the requirements of kiln materials for high-temperature roasting of lithium ion battery anodes, and resists the erosion of lithium ion steam. However, the compact spinel refractory brick has the defects of high density, high heat conductivity coefficient, high cost and the like, and related applications cannot be promoted in time.
The material with the hollow sphere structure has the characteristics of small density and large gap, and the heat insulation material prepared by the hollow spheres has the advantages of uniform pore distribution, light weight and good heat insulation performance, and is commonly used for preparing high-performance heat insulation materials. The currently applied zirconia hollow sphere brick has the characteristics of high corrosion resistance, light weight and high strength, but the price and the storage capacity of raw materials limit the application of the zirconia hollow sphere brick, the current market needs a material which has rich raw materials, high cost performance, light weight, high strength and strong resistance to the corrosion of oxidation lithium steam, and a refractory brick body prepared from the spinel hollow sphere can well meet the requirements.
The spinel hollow sphere is a hollow microbead, and the main chemical components of the wall of the hollow microbead are magnesium oxide and aluminum oxide. The spinel hollow sphere has the characteristics of low density, high temperature resistance, good insulativity and the like. Compared with the common alumina hollow sphere, the spinel hollow sphere has better thermal shock resistance, and the existing experiments prove that the spinel hollow sphere has stronger corrosion resistance to the anode material of the lithium ion battery.
Chinese patent application CN102603329A discloses a double-layer light composite brick and a preparation method thereof, wherein a magnesium aluminate spinel hollow sphere layer is prepared by taking magnesium aluminate spinel hollow spheres as light aggregate, and the magnesium aluminate spinel hollow sphere layer has good alkaline material erosion resistance as a part of a brick body. The matrix powder in the application is one or a plurality of mixtures of alumina powder, corundum powder, magnesia powder, spinel powder, titanium oxide powder, chromium oxide powder, zirconium oxide powder, chromium corundum powder, zirconium corundum powder and aluminum titanate powder, when the matrix powder is a mixture, impurities which are easy to corrode are easy to introduce, if single alumina powder is adopted, the alumina powder is alpha-Al 2O3 and used as the matrix powder, and meanwhile, a yellow dextrin solution is used as a binding agent, experiments prove that the bending strength and the compressive strength of the prepared brick are not enough, and the brick is still not ideal when applied to a kiln in the production of the lithium ion battery anode material.
Disclosure of Invention
The invention provides a high-strength light spinel hollow ball brick for a kiln made of lithium ion battery anode material, and a preparation method thereof. The magnesium aluminate spinel hollow sphere is used as lightweight aggregate, rho-Al 2O3 in matrix powder is used as a bonding agent and lanthanum cerium carbonate is added as a sintering aid on the premise of not introducing impurity items, so that sintering of the magnesium aluminate spinel hollow sphere brick is effectively promoted, and the strength of the product is improved. The prepared lightweight magnesia-alumina spinel brick has excellent erosion resistance. The brick body is used for building a kiln, so that the corrosion of the lithium ion anode material can be effectively resisted, the service life of the brick body is prolonged, meanwhile, the brick body is prevented from being peeled off, the quality of the anode material is improved, and the use cost is reduced.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps: a high-strength light spinel hollow ball brick for a kiln for producing a lithium ion battery anode material is characterized in that a brick body is made of 56-65 parts by weight of magnesium aluminate spinel hollow balls, 35-44 parts by weight of matrix powder and 2-6 parts by weight of sintering aids;
al in the magnesium aluminate spinel hollow sphere2O3More than or equal to 68 percent, MgO more than or equal to 29 percent and grain diameter of 0.2-5 mm;
the matrix powder is rho-Al with 325 meshes2O3The powder and 200-mesh light-burned magnesia powder are mixed according to the weight ratio of 1.85: 1.
The sintering aid is lanthanum cerium carbonate;
the volume density of the designed magnesium-aluminum light spinel hollow ball brick is 0.9-1.65 g/cm3。
Furthermore, the magnesia-alumina spinel hollow spheres in the brick body are prepared according to the particle size grading, and are 8-39 parts of 0.2-1 mm, 10-26 parts of 1-2 mm, 4-22 parts of 2-3 mm and 0-16 parts of 3-5 mm.
Further, the rho-Al2O3Al in powder2O3More than or equal to 93 percent, and MgO in the light-burned magnesia powder is more than or equal to 90 percent.
Furthermore, the addition amount of the sintering aid lanthanum carbonate and cerium carbonate is preferably 4-6 parts.
Further, the volume density of the designed magnesium-aluminum light spinel hollow ball brick is 1.0-1.6 g/cm3。
The spinel hollow ball brick is prepared by introducing the magnesia-alumina spinel hollow ball as lightweight aggregate and light-burned magnesia powder and rho-alumina powder as matrix powder. Wherein rho-Al2O3And the magnesium-aluminum conjugate is also used as a binding agent, so that the matrix is purer, the influence of eutectic compounds on high-temperature performance is avoided, the normal-temperature compressive strength of a sample is improved, and the prepared magnesium-aluminum conjugate has good alkaline slag corrosion resistance and permeability. The artificial synthesized spinel is hard to sinter compactly, lanthanum and cerium carbonate is used as a sintering aid, the heat treatment temperature is raised, the carbonate is decomposed into rare earth oxide lanthanum and cerium oxide, and the rare earth oxide has the characteristics of high melting point, high chemical activity and strong erosion resistance. The lanthanum oxide cerium mainly forms a liquid phase in the sample to promote the discharge of pores at the grain boundary and accelerate the sintering densification of the magnesium aluminate spinel; while lanthanum ion La3+Cerium ion Ce4+When the spinel material is added, replacement and solid solution can occur, lattice defects are formed, lattices are activated, the crystallization degree of the spinel material is accelerated, and sintering is promoted finally. The prepared brick has the advantages of light weight, strong erosion resistance, good fireproof and heat-insulating properties and the like, and can well meet the requirements of kiln materials for high-temperature roasting of lithium ion battery anode materials.
The invention provides a preparation method of a high-strength light spinel hollow ball brick for a kiln for producing a lithium ion battery anode material, which comprises the following steps:
a, preparing materials: after the magnesium aluminate spinel hollow sphere aggregate is mixed, adding water to prepare slurry, adding the substrate powder and the sintering aid which are mixed in advance by a ball mill, mixing for 10-20 minutes, and uniformly mixing for later use;
b, forming: pouring the mixture into a mould according to the designed size after the material preparation is finished, and performing vibration and pressurization forming on a vibration table;
c, firing: and taking out the molded blank, naturally standing for 12-24 h, drying at 60-150 ℃, demolding, putting into a kiln, preserving heat at 1500-1780 ℃ for 4-10 h, and firing.
In the preparation method, the mechanical property is good when the firing temperature is 1700-1780 ℃.
The light spinel hollow ball brick has good mechanical property, low thermal conductivity and excellent thermal shock property on the premise of ensuring the light weight of the brick body. In addition, the overall composition is mainly spinel phase, which ensures good resistance to lithium ion attack. Meanwhile, the preparation process is simple, the cost is low, the preparation method can be popularized and used for building the kiln on a large scale, the weight of the kiln can be greatly reduced, a good heat preservation effect is achieved, the kiln chamber can be protected when the preparation method is applied to the lithium ion battery anode material furnace chamber, the corrosion can be effectively resisted, the service life of the furnace chamber is prolonged, meanwhile, the influence of slag falling on the performance of the anode material is prevented, the use cost is reduced, and the energy consumption is reduced.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below with reference to examples to facilitate understanding for those skilled in the art. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, belong to the scope of the present invention.
Examples 1 to 7:
preparing raw materials, namely aggregate of the magnesium aluminate spinel hollow sphere with four specifications of 0.2-1 mm, 1-2 mm, 2-3 mm and 3-5 mm, and adding Al in the magnesium aluminate spinel hollow sphere2O3More than or equal to 68 percent of MgO, more than or equal to 29 percent of MgO; 320 mesh rho-Al2O3Powder of Al2O3More than or equal to 93 percent; 200-mesh light-burned magnesia powder, wherein MgO is more than or equal to 90 percent; and designing the volume density of the magnesium-aluminum light spinel hollow ball brick.
The magnesium aluminate spinel hollow spheres are uniformly mixed in a stirrer, and then poured into a matrix powder material which is mixed in advance in a ball mill. Adding water, mixing for 10 minutes, and mixing uniformly for later use. And after the material preparation is finished, putting the slurry into a die according to the design size, and performing vibration and pressure molding on a vibration table. And taking out the molded blank, naturally standing for 12-24 h, drying at 60-150 ℃, demolding, putting into a kiln, preserving heat at 1500-1780 ℃ for 4-10 h, and firing.
The component contents and the performance parameters of the examples are shown in Table I.
Comparative examples 1 and 3
Raw materials: aggregate of the magnesium aluminate spinel hollow sphere with four specifications of 0.2-1 mm, 1-2 mm, 2-3 mm and 3-5 mm, and Al in the magnesium aluminate spinel hollow sphere2O3More than or equal to 68 percent of MgO, more than or equal to 29 percent of MgO; 320 mesh rho-Al2O3Powder of Al2O3More than or equal to 93 percent; 200 meshes of light-burned magnesia powder with MgO more than or equal to 90 percent, and the volume density of the designed magnalium light spinel hollow ball brick is 1.35g/cm3、1.0g/cm3
The preparation method is the same as above, and the component contents and performance parameters of each comparative example are shown in the table I
Comparative examples 2 and 4
Raw materials: aggregate of the magnesium aluminate spinel hollow sphere with four specifications of 0.2-1 mm, 1-2 mm, 2-3 mm and 3-5 mm, and Al in the magnesium aluminate spinel hollow sphere2O3More than or equal to 68 percent of MgO, more than or equal to 29 percent of MgO; 320 mesh alpha-Al2O3Powder of Al2O3More than or equal to 93 percent; 200-mesh light-burned magnesia powder, wherein MgO is more than or equal to 90 percent; yellow dextrin for designing the volume density of the light spinel hollow ball brick of magnesium aluminum to be 1.35g/cm3、1.2g/cm3
The preparation method is the same as above, and the component contents and performance parameters of each comparative example are shown in the table I
Watch 1
As can be seen from the data in Table one, the results are compared to the results obtained with alpha-Al2O3As matrix powder and yellow dextrin as binder, adopting rho-Al2O3And the spinel hollow ball brick body can be effectively promoted by adding lanthanum and cerium carbonateThe strength of the product is improved. Compared with similar products, the prepared brick has better performance, good lithium ion erosion resistance and no introduction of easily eroded impurities.
Claims (7)
1. A high-strength light spinel hollow ball brick for a lithium battery anode material production kiln is characterized in that a brick body is made of, by weight, 56-65 parts of magnesium aluminate spinel hollow balls, 35-44 parts of matrix powder and 2-6 parts of sintering aids;
al in the magnesium aluminate spinel hollow sphere2O3More than or equal to 68 percent, MgO more than or equal to 29 percent and grain diameter of 0.2-5 mm;
the matrix powder is rho-Al with 325 meshes2O3The powder and 200-mesh light-burned magnesia powder are mixed according to the weight ratio of 1.85: 1;
the sintering aid is lanthanum cerium carbonate;
the volume density of the designed magnesium-aluminum light spinel hollow ball brick is 0.9-1.65 g/cm3。
2. The high-strength light spinel hollow sphere brick for the lithium battery positive electrode material production kiln as claimed in claim 1, wherein the magnesium aluminate spinel hollow sphere in the brick body is prepared by 0.2-1 mm8-39 parts, 1-2 mm10-26 parts, 2-3 mm4-22 parts and 3-5 mm0-16 parts according to the grain size grading.
3. The high-strength light spinel hollow ball brick for lithium battery anode material production kiln as claimed in claim 1, wherein said rho-Al is selected from the group consisting of2O3Al in powder2O3More than or equal to 93 percent, and MgO in the light-burned magnesia powder is more than or equal to 90 percent.
4. The high-strength light spinel hollow ball brick for the kiln for producing the lithium battery anode material as claimed in claim 1, wherein the sintering aid lanthanum carbonate and cerium carbonate is added in an amount of 4-6 parts.
5. The high-strength light tip for the kiln for producing the lithium battery positive electrode material as claimed in claim 1The crystal stone hollow ball brick is characterized in that the volume density of the designed magnesium-aluminum light spinel hollow ball brick is 1.0-1.6 g/cm3。
6. A preparation method of a high-strength light spinel hollow ball brick for a kiln for producing lithium battery anode materials is characterized by comprising the following steps:
a, preparing materials: after the magnesium aluminate spinel hollow sphere aggregate is mixed, adding water to prepare slurry, adding the substrate powder and the sintering aid which are mixed in advance by a ball mill, mixing for 10-20 minutes, and uniformly mixing for later use;
b, forming: pouring the mixture into a mould according to the designed size after the material preparation is finished, and performing vibration and pressurization forming on a vibration table;
c, firing: and taking out the molded blank, naturally standing for 12-24 h, drying at 60-150 ℃, demolding, putting into a kiln, preserving heat at 1500-1780 ℃ for 4-10 h, and firing.
7. The method for preparing the high-strength light spinel hollow ball brick for the lithium battery anode material production kiln as claimed in claim 6, wherein the firing temperature is 1700-1780 ℃.
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| CN113701495A (en) * | 2021-08-26 | 2021-11-26 | 江苏润鸿高温窑具有限公司 | Design method of low-expansion strong-alkaline-corrosion-resistant material for inner cavity of gas flame-proof roller kiln |
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| US20140272168A1 (en) * | 2013-03-12 | 2014-09-18 | Rolls-Royce Corporation | Method for fabricating multilayer environmental barrier coatings |
| CN103496990A (en) * | 2013-09-13 | 2014-01-08 | 天津大学 | High-temperature thermal-shock-resistant magnesia alumina spinel-zirconia complex-phase material and preparation method thereof |
| CN108395262A (en) * | 2018-04-16 | 2018-08-14 | 河南工业大学 | A kind of olivine combination magnesium aluminate spinel hollow ball castable and preparation method |
| CN111041527A (en) * | 2020-01-15 | 2020-04-21 | 济宁碳素集团有限公司 | Preparation method of prebaked anode for rare earth additive modified aluminum |
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| CN113701495A (en) * | 2021-08-26 | 2021-11-26 | 江苏润鸿高温窑具有限公司 | Design method of low-expansion strong-alkaline-corrosion-resistant material for inner cavity of gas flame-proof roller kiln |
| CN113701495B (en) * | 2021-08-26 | 2024-02-23 | 江苏润鸿高温窑具有限公司 | Method for designing low-expansion strong alkaline corrosion resistant material for inner cavity of gas flame-proof roller kiln |
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