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CN-121977357-A - Pollution-resistant sagger for sintering high-temperature materials and preparation method thereof

CN121977357ACN 121977357 ACN121977357 ACN 121977357ACN-121977357-A

Abstract

The application relates to the technical field of high-temperature sintering devices, in particular to an anti-pollution sagger for sintering high-temperature materials and a preparation method thereof, wherein the anti-pollution sagger comprises a sagger body made of mullite materials, a sapphire single crystal wafer is attached to the inner surface of the sagger body through a composite gradient structure bonding layer, the composite gradient structure bonding layer comprises a bottom transition bonding layer, a middle buffer reinforcing layer and a surface sapphire bonding layer which are arranged in a stacked manner, the bottom transition bonding layer is contacted with the inner surface of the sagger body, the middle buffer reinforcing layer is arranged between the bottom transition bonding layer and the surface sapphire bonding layer, and the surface sapphire bonding layer is contacted with the sapphire single crystal wafer; and the bottom layer to the surface layer sapphire bonding layer are laminated in a mode of continuously gradient change of chemical composition and thermal expansion coefficient. Through the arrangement, the application can realize effective isolation of materials, long-term stable combination of self interfaces and excellent thermal shock reliability in the long-term high-temperature sintering process.

Inventors

  • HAO WENJUAN
  • LU YARONG
  • KANG SEN
  • BAI XIAOXIA
  • YANG SHIYIN
  • LI LU
  • YANG BO

Assignees

  • 天通银厦新材料有限公司

Dates

Publication Date
20260505
Application Date
20260409

Claims (9)

  1. 1. The anti-pollution sagger for sintering high-temperature materials comprises a sagger body made of mullite materials, and is characterized in that a sapphire single crystal wafer is attached to the inner surface of the sagger body through a composite gradient structure bonding layer, the composite gradient structure bonding layer comprises a bottom transition bonding layer, a middle buffer reinforcing layer and a surface layer sapphire bonding layer which are arranged in a stacked mode, the bottom transition bonding layer is in contact with the inner surface of the sagger body, the middle buffer reinforcing layer is arranged between the bottom transition bonding layer and the surface layer sapphire bonding layer, the surface layer sapphire bonding layer is in contact with the sapphire single crystal wafer, and the bottom transition bonding layer, the middle buffer reinforcing layer and the surface layer sapphire bonding layer are arranged in a stacked mode in a mode that chemical components and thermal expansion coefficients continuously change in a gradient mode; the thickness of the sapphire single crystal wafer is 0.1-2 mm, and the total thickness of the composite gradient structure bonding layer is 1-2 mm.
  2. 2. The anti-pollution sagger for sintering high-temperature materials according to claim 1, wherein the composition raw materials of the bottom layer transition bonding layer comprise nano alumina powder, yttria-stabilized zirconia powder and nano silicon dioxide powder, the mass ratio of the nano alumina powder to the yttria-stabilized zirconia powder is (7:3) - (8:2), and the mass of the nano silicon dioxide powder is 1% -5% of the total mass of the raw materials of the bottom layer transition bonding layer.
  3. 3. The anti-pollution sagger for sintering high-temperature materials according to claim 2, wherein the intermediate buffer reinforcing layer comprises flaky alumina, alumina fibers and alumina-based bonding powder, the mass ratio of the flaky alumina to the alumina fibers to the alumina-based bonding powder is (1.5-2.5) (0.5-1.5) (6-8), the diameter of the alumina fibers is 3-10 mu m, and the length-diameter ratio of the alumina fibers is greater than or equal to 20.
  4. 4. The anti-pollution sagger for sintering high-temperature materials according to claim 3, wherein the surface sapphire bonding layer comprises rare earth doped aluminosilicate glass phase powder and active alumina micro powder, the mol ratio of alumina to silica in the aluminosilicate glass phase powder is (1:1) - (2:1), the aluminosilicate glass phase powder is doped with rare earth oxide, the mass of the rare earth oxide is 3% -8% of the total mass of the aluminosilicate glass phase powder, the rare earth oxide is at least one of yttrium oxide, lanthanum oxide and cerium oxide, the particle size of the active alumina micro powder is 0.5-3 μm, and the mass ratio of the active alumina micro powder to the glass phase powder is (3:7) - (4:6).
  5. 5. The anti-pollution sagger for sintering high-temperature materials according to claim 4, wherein the raw materials of the surface layer sapphire bonding layer further comprise yttria-stabilized zirconia nanowires, the mass of the yttria-stabilized zirconia nanowires is 0.5% -3% of the total mass of the raw materials of the surface layer sapphire bonding layer, the diameter of the yttria-stabilized zirconia nanowires is 30-100 nm, and the length of the yttria-stabilized zirconia nanowires is 5-20 μm.
  6. 6. The anti-pollution sagger for sintering high-temperature materials according to claim 1, wherein the bonding surface of the sapphire single crystal wafer is subjected to laser etching treatment to form a transition layer with a micropore structure, the pore diameter of the micropore structure in the transition layer is 0.1-2 μm, the depth of the micropore structure in the transition layer is 5-20 μm, and the surface roughness Ra of the bonding surface of the sapphire single crystal wafer after treatment is 0.5-1.4 μm.
  7. 7. A method for preparing an anti-contamination sagger for sintering a high temperature material, characterized in that it is applied to the anti-contamination sagger for sintering a high temperature material according to any one of claims 1 to 6, the method comprising: cleaning and roughening the inner surface of the sagger body, and performing laser etching treatment on the bonding surface of the sapphire single crystal wafer; Respectively preparing sizing agents for forming a bottom transition bonding layer, a middle buffer reinforcing layer and a surface sapphire bonding layer; Sequentially and electrostatically spraying the bottom layer transition bonding layer slurry, the middle buffer reinforcing layer slurry and the surface layer sapphire bonding layer slurry on the inner surface of the sagger body, and performing pre-curing treatment after spraying each layer of slurry so as to form a bonding layer blank in a layer-by-layer accumulation manner; The sapphire single crystal wafer is paved on the surface of the bonding layer green body to form a combination body composed of the sagger body, the bonding layer green body and the sapphire single crystal wafer, the combination body is applied with pressure of 0.5-2 MPa, the combination body is heated to an interface activation temperature at a rate of 3-8 ℃ per minute under a protective atmosphere, and the temperature and the pressure are kept for 10-60 min at the interface activation temperature, wherein the interface activation temperature is higher than the glass transition temperature of an aluminosilicate glass phase in the surface layer sapphire bonding layer, and the interface activation temperature is lower than the softening point of the aluminosilicate glass phase; Maintaining pressure and protective atmosphere, heating from the interface activation temperature to 600-800 ℃ at a rate of 2-5 ℃ per minute, preserving heat for 0.5-1 h, heating to 1000-1200 ℃ at a rate of 3-8 ℃ per minute, preserving heat for 10-30 min, and cooling to below 300 ℃ at a rate of 2-10 ℃ per minute in a program and then cooling with a furnace.
  8. 8. The method for preparing an anti-contamination sagger for sintering a high temperature material according to claim 7, wherein the interfacial activation temperature satisfies the following relationship of Tg+30℃≤Ta≤Tg+80℃, wherein Ta represents the interfacial activation temperature, tg represents the glass transition temperature of the aluminosilicate glass phase in the surface layer sapphire bonding layer, and the glass transition temperature is 480 ℃ to 580 ℃.
  9. 9. The method for preparing an anti-pollution sagger for sintering high-temperature materials according to claim 8, wherein the pressure applied to the combination body is in the range of 70% -100% of 0.5-2 mpa and periodically fluctuates at the frequency of 0.1-1 hz in the process of preserving heat and pressure for 10-60 min at the interface activation temperature.

Description

Pollution-resistant sagger for sintering high-temperature materials and preparation method thereof Technical Field The application relates to the technical field of high-temperature sintering devices, in particular to an anti-pollution sagger for sintering high-temperature materials and a preparation method thereof. Background In the industrial preparation of lithium ion battery anode materials (such as lithium cobaltate and ternary materials), the materials are required to be placed in a firing container (usually mullite materials, and the main components are as followsIn the process of sintering the anode material of the lithium battery, the common sagger taking mullite or composite ceramic thereof as a matrix is not specially anti-corrosion modified, and has the following core challenges that active components (such as lithium salt and transition metal oxide) in the anode material can chemically react with the surface of the mullite sagger at high temperature, the process not only corrodes the sagger, but also can cause elements such as aluminum, silicon and the like in the sagger to dissolve out and invade the anode material, introduce electrochemical impurities, and cause material capacity attenuation, cycle performance reduction and batch consistency to be poor. In order to solve the pollution problem, the prior art is mainly improved from two aspects, namely, the corrosion resistance of the sagger body is improved by adopting a raw material with higher purity or an optimized formula, but the method has high cost and limited effect, and the ceramic protective coating such as alumina is applied on the inner wall of the sagger to be physically isolated, but the thermal expansion coefficient between the protective layer and the mullite substrate is mismatched, so that the sagger body is easy to crack and peel due to stress in thermal circulation, and the service life is short. Therefore, the prior art is difficult to achieve a fundamental breakthrough between achieving long-term effective isolation and ensuring the stability of the protective layer bonding interface. Disclosure of Invention In order to solve the problems in the prior art, the application provides the anti-pollution sagger for sintering the high-temperature material and the preparation method thereof, which can realize effective isolation of materials, long-term stable combination of self interfaces and excellent thermal shock reliability in the long-term high-temperature sintering process. According to the anti-pollution sagger for sintering high-temperature materials, the anti-pollution sagger comprises a sagger body made of mullite materials, a sapphire single crystal wafer is attached to the inner surface of the sagger body through a composite gradient structure bonding layer, the composite gradient structure bonding layer comprises a bottom transition bonding layer, a middle buffer reinforcing layer and a surface layer sapphire bonding layer which are arranged in a stacked mode, the bottom transition bonding layer is in contact with the inner surface of the sagger body, the middle buffer reinforcing layer is arranged between the bottom transition bonding layer and the surface layer sapphire bonding layer, the surface layer sapphire bonding layer is in contact with the sapphire single crystal wafer, and the bottom transition bonding layer, the middle buffer reinforcing layer and the surface layer sapphire bonding layer are arranged in a stacked mode in a mode that chemical compositions and thermal expansion coefficients continuously change in a gradient mode. According to some embodiments of the first aspect of the application, the thickness of the sapphire single crystal wafer is 0.1 mm-2 mm, and the total thickness of the composite gradient structure bonding layer is 1 mm-2 mm. According to some embodiments of the first aspect of the present application, the composition raw materials of the bottom layer transition bonding layer include nano alumina powder, yttria-stabilized zirconia powder and nano silica powder, the mass ratio of the nano alumina powder to the yttria-stabilized zirconia powder is (7:3) - (8:2), and the mass of the nano silica powder is 1% -5% of the total mass of the bottom layer transition bonding layer raw materials. According to some embodiments of the first aspect of the present application, the intermediate buffer reinforcing layer comprises a sheet alumina, alumina fibers and alumina-based bonding powder, wherein the mass ratio of the sheet alumina, the alumina fibers and the alumina-based bonding powder is (1.5-2.5): (0.5-1.5): (6-8), the diameter of the alumina fibers is 3 μm-10 μm, and the length-diameter ratio of the alumina fibers is greater than or equal to 20. According to some embodiments of the first aspect of the present application, the raw materials for forming the surface sapphire bonding layer include rare earth doped aluminosilicate glass phase powder and activated alumina micro powder, wherein