CN115872776A - Surface gradient hardening method for nano heat-insulating material - Google Patents
Surface gradient hardening method for nano heat-insulating material Download PDFInfo
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- CN115872776A CN115872776A CN202211386371.9A CN202211386371A CN115872776A CN 115872776 A CN115872776 A CN 115872776A CN 202211386371 A CN202211386371 A CN 202211386371A CN 115872776 A CN115872776 A CN 115872776A
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- 239000011810 insulating material Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 59
- 239000000203 mixture Substances 0.000 claims abstract description 52
- 239000000919 ceramic Substances 0.000 claims abstract description 48
- 239000002245 particle Substances 0.000 claims abstract description 35
- 229910052810 boron oxide Inorganic materials 0.000 claims abstract description 34
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000002904 solvent Substances 0.000 claims abstract description 28
- 239000012774 insulation material Substances 0.000 claims abstract description 25
- 229920000642 polymer Polymers 0.000 claims abstract description 22
- 238000000498 ball milling Methods 0.000 claims abstract description 19
- 229910052580 B4C Inorganic materials 0.000 claims abstract description 17
- 229910052582 BN Inorganic materials 0.000 claims abstract description 17
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 17
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- MOWNZPNSYMGTMD-UHFFFAOYSA-N oxidoboron Chemical class O=[B] MOWNZPNSYMGTMD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000011248 coating agent Substances 0.000 claims abstract description 9
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000007789 sealing Methods 0.000 claims abstract description 6
- 239000003921 oil Substances 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 238000003776 cleavage reaction Methods 0.000 claims 1
- 230000007017 scission Effects 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 230000006835 compression Effects 0.000 description 4
- 238000007906 compression Methods 0.000 description 4
- 239000005388 borosilicate glass Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000779 depleting effect Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229930195734 saturated hydrocarbon Natural products 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a surface gradient hardening method of a nano heat-insulating material, belonging to the technical field of preparation of nano heat-insulating materials. Under a dry environment, carrying out ball milling on the boron oxide powder and white oil to obtain modified boron oxide powder; uniformly mixing the modified boron oxide powder with boron nitride powder, boron carbide powder and polymer particles to obtain a composition A; adding the composition A into a solvent B, and stirring until the polymer particles are completely dissolved to obtain a composition B; uniformly coating the composition B on the inner surface of the ceramic box, and uniformly attaching the composition A on the inner surface of the ceramic box after the solvent B is volatilized; and placing the nano heat insulation material component in a ceramic box, sealing the ceramic box, placing the ceramic box in a muffle furnace, performing heat treatment, cooling and taking out to obtain the nano heat insulation material block with the gradient hardened surface. The invention can solve the problems of loose surface structure and easy powder falling of the nanometer heat-insulating material component.
Description
Technical Field
The invention belongs to the technical field of preparation of nano heat-insulating materials, and particularly relates to a surface gradient hardening method of a nano heat-insulating material.
Background
The nanometer heat insulating material is a novel high-performance heat insulating material, is prepared by taking nanometer powder as a main raw material through mould pressing, has the advantages of low density, good heat insulating property, good temperature resistance, low cost and the like, and has obvious application prospects in the fields of aerospace, metallurgy, building and the like. However, since the nano heat insulation material is formed by molding nano powder, the powder particles are not connected with each other under chemical action, and the nano heat insulation material has the obvious defects of low surface strength and easy powder falling, thereby severely limiting the application of the nano heat insulation material. In the prior art, the problem of powder falling can be solved to a certain extent by preparing the coating on the surface, the heat insulation performance of the coating is improved, but the overall strength and the surface hardness of the nano heat insulation material cannot be obviously improved. Therefore, it is necessary to invent a surface gradient hardening method of nano heat insulation material to optimize the strength and hardness of the nano heat insulation material.
Disclosure of Invention
The invention aims to solve the problems of loose surface structure and easy powder falling of a nanometer heat insulation material member, and provides a method for optimizing the strength and hardness of a nanometer heat insulation material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a surface gradient hardening method of a nanometer heat insulation material comprises the following steps:
1) Under a dry environment, adding boron oxide powder into a ball milling tank, adding white oil which is 1-5% of the boron oxide by mass into the ball milling tank, and carrying out ball milling for 3-10 hours at a speed of 100-400r/min to obtain modified boron oxide powder;
2) Uniformly mixing the modified boron oxide powder, boron nitride powder, boron carbide powder and polymer particles according to the mass ratio of (10-20) to (1-2) to obtain a composition A;
3) Adding the composition A into a solvent B, and stirring until the polymer particles are completely dissolved to obtain a composition B;
4) Uniformly coating the composition B on the inner surface of the ceramic box, and uniformly attaching the composition A on the inner surface of the ceramic box after the solvent B is volatilized;
5) And (3) placing the nano heat insulation material component in a ceramic box to ensure that the nano heat insulation material component does not directly contact with the composition A, then sealing the ceramic box, placing the ceramic box in a muffle furnace, performing heat treatment according to a temperature rise program, cooling to room temperature, and taking out to obtain the surface gradient hardened nano heat insulation material block.
Preferably, the particle size of the boron oxide powder is less than 100 μm.
Preferably, the amount m of the composition A is determined according to the surface area S of the nano heat insulating material member, and the calculation formula is m = Sx (0.1-0.4) g/cm 2 。
Preferably, the particle sizes of the boron nitride powder and the boron carbide powder are both less than 100 μm.
Preferably, the cracking temperature of the polymer particles is lower than 350 ℃, and polyethylene glycol, polyvinyl alcohol and the like are preferred.
Preferably, the solvent B is a good solvent for the polymer particles.
Preferably, the amount of the solvent B is at least 1 time, preferably 1 to 2 times, that of the composition a.
Preferably, the ceramic box is one of a silicon carbide box, an alumina box and a zirconia box.
Preferably, the ceramic cartridge has an opening and closing function, and is sealed in a closed state.
Preferably, the temperature-raising program is: the muffle furnace is heated to 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃ and 1000 ℃ in turn at the speed of 5-10 ℃/min, and the temperature is kept for 1 hour at each temperature point.
The beneficial effects obtained by the invention are as follows:
1) The boron oxide in the composition A attached to the inner surface of the ceramic box is heated and melted, and the generated boron oxide steam can react with silicon dioxide in the nano heat-insulating material to generate a borosilicate glass phase, so that the nano heat-insulating material is hardened. The boron oxide steam has diffusivity and can be diffused from the surface to the interior of the nano heat-insulating material in a gradient manner, so that the effect of gradient hardening of the surface of the nano heat-insulating material is realized. The white oil is white mineral oil which is industrially extracted and mainly contains liquid saturated hydrocarbon, and the surface of the white oil is subjected to hydrophobic modification to prevent the boron oxide from deteriorating after absorbing water to generate boric acid. The boron oxide is coated and subjected to hydrophobic treatment through the white oil, so that the boron oxide is effectively prevented from losing moisture in the air.
2) Boron carbide can be oxidized at temperatures above 500 ℃ to form boron oxide, and boron nitride can be oxidized at temperatures above 700 ℃ to form boron oxide. As the boron oxide in the composition A is firstly heated and melted, the boron carbide and the boron nitride are wrapped by the boron oxide and cannot contact with oxygen, and only the boron oxide in the composition A generates steam to perform gradient hardening on the nano heat-insulating material; and (3) adopting a step-type temperature rise program, gradually evaporating and depleting boron oxide along with the rise of temperature and the time, exposing boron carbide and boron nitride, contacting and oxidizing the boron carbide and the boron nitride with air to generate and release new boron oxide steam, reacting the steam with silicon dioxide in the nano heat-insulating material after the steam is diffused to the surface of the nano heat-insulating material to generate a borosilicate glass phase, and continuously carrying out gradient hardening on the nano heat-insulating material. By adopting the technical means, the boron oxide slow release caused by the release of boron oxide at one time with high concentration is avoided, the controllable concentration of boron oxide steam is ensured, and the surface gradient hardening of the nano heat-insulating material achieves the best effect.
3) Boron oxide steam is utilized, and boron oxide is not directly doped into the nano heat-insulating material, so that the phenomena of uneven hardening and uncontrollable caused by uneven doping of boron oxide are avoided.
Drawings
FIG. 1 is a flow chart of the surface gradient hardening process of a nano-insulation material according to the present invention.
Detailed Description
In order to make the aforementioned and other features and advantages of the invention more comprehensible, embodiments accompanied with figures are described in detail below.
Example 1
1) Under a dry environment, adding boron oxide powder with the particle size of less than 100 microns into a ball milling tank, adding white oil with the mass of 1% of boron oxide into the ball milling tank, and carrying out ball milling for 10 hours at the speed of 400r/min to obtain modified boron oxide powder;
2) Uniformly mixing the modified boron oxide powder, boron nitride powder, boron carbide powder and polymer particles according to a mass ratio of 10;
wherein the dosage m of the composition A is determined according to the surface area S of the nano heat insulation material member, and the calculation formula is m = S multiplied by 0.1g/cm 2 。
Wherein the particle diameters of the boron nitride powder and the boron carbide powder are both less than 100 mu m.
Wherein the polymer particles are polyvinyl alcohol.
3) Adding the composition A into a solvent B, and stirring until the polymer particles are completely dissolved to obtain a composition B;
wherein the solvent B is water.
Wherein the dosage of the solvent B is 1 time of that of the composition A.
4) Uniformly coating the composition B on the inner surface of the ceramic box, and uniformly attaching the composition A on the inner surface of the ceramic box after the solvent B is volatilized;
wherein, the ceramic casket is the carborundum casket.
Wherein the ceramic box has an opening and closing function, and is sealed in a closed state.
5) And (2) placing the nano heat-insulating material component in a ceramic box to ensure that the nano heat-insulating material component is not in direct contact with the composition A, then sealing the ceramic box, placing the ceramic box in a muffle furnace, performing heat treatment according to a temperature rise program, cooling to room temperature, and taking out to obtain the nano heat-insulating material block with the gradient hardened surface.
Wherein the temperature-raising program is: the muffle furnace was sequentially heated at a rate of 5 ℃/min to 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃ and 1000 ℃, and the temperature was maintained at each of the above temperature points for 1 hour.
Tests show that the nano heat-insulating material block subjected to surface gradient hardening has no powder falling on the surface, the total thickness of a surface hardening layer is 1.3mm, and the density of a hardening area is 1.52g/cm 3 The compactness is good; the compression strength of the nanometer heat insulation material block is improved to 3.5MPa from 2.3MPa before hardening.
Example 2
1) Under a dry environment, adding boron oxide powder with the particle size of less than 100 mu m into a ball milling tank, adding white oil with the mass of 5 percent of boron oxide into the ball milling tank, and carrying out ball milling for 3 hours at the speed of 100r/min to obtain modified boron oxide powder;
2) Uniformly mixing the modified boron oxide powder, boron nitride powder, boron carbide powder and polymer particles according to a mass ratio of 20;
wherein the amount m of the composition A is determined according to the surface area S of the nano heat insulating material member, and the calculation formula is m = S × 0.4g/cm 2 。
Wherein the particle diameters of the boron nitride powder and the boron carbide powder are both less than 100 mu m.
Wherein the polymer particles are polyvinyl alcohol.
3) Adding the composition A into a solvent B, and stirring until the polymer particles are completely dissolved to obtain a composition B;
wherein the solvent B is water.
Wherein the dosage of the solvent B is 2 times of that of the composition A.
4) Uniformly coating the composition B on the inner surface of the ceramic box, and uniformly attaching the composition A on the inner surface of the ceramic box after the solvent B is volatilized;
wherein, the ceramic box is an alumina box.
Wherein the ceramic box has an opening and closing function, and is sealed in a closed state.
5) And (2) placing the nano heat-insulating material component in a ceramic box to ensure that the nano heat-insulating material component is not in direct contact with the composition A, then sealing the ceramic box, placing the ceramic box in a muffle furnace, performing heat treatment according to a temperature rise program, cooling to room temperature, and taking out to obtain the nano heat-insulating material block with the gradient hardened surface.
Wherein the temperature-raising program is: the muffle furnace was sequentially heated at a rate of 10 ℃/min to 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃, 1000 ℃ and held at each of the above temperature points for 1 hour.
Tests show that the nano heat-insulating material block after surface gradient hardening has no powder falling on the surface, the total thickness of the surface hardening layer is 1.83mm, and the density of the hardening area is 1.62g/cm 3 The compactness is good; the compression strength of the nanometer heat insulation material block is improved to 3.8MPa from 2.3MPa before hardening.
Example 3
1) Under a dry environment, adding boron oxide powder with the particle size of less than 100 mu m into a ball milling tank, adding white oil with the mass of 3 percent of boron oxide into the ball milling tank, and carrying out ball milling for 6 hours at the speed of 300r/min to obtain modified boron oxide powder;
2) Uniformly mixing the modified boron oxide powder, the boron nitride powder, the boron carbide powder and the polymer particles according to a mass ratio of 15;
wherein the dosage m of the composition A is determined according to the surface area S of the nano heat insulation material member, and the calculation formula is m = S multiplied by 0.3g/cm 2 。
Wherein the particle diameters of the boron nitride powder and the boron carbide powder are both less than 100 mu m.
Wherein, the polymer particles are polyethylene glycol.
3) Adding the composition A into a solvent B, and stirring until the polymer particles are completely dissolved to obtain a composition B;
wherein the solvent B is water.
Wherein the dosage of the solvent B is 1.5 times of that of the composition A.
4) Uniformly coating the composition B on the inner surface of the ceramic box, and uniformly attaching the composition A on the inner surface of the ceramic box after the solvent B is volatilized;
wherein, the ceramic box is an alumina box.
Wherein the ceramic box has an opening and closing function, and is sealed in a closed state.
5) And (3) placing the nano heat insulation material component in a ceramic box to ensure that the nano heat insulation material component does not directly contact with the composition A, then sealing the ceramic box, placing the ceramic box in a muffle furnace, performing heat treatment according to a temperature rise program, cooling to room temperature, and taking out to obtain the surface gradient hardened nano heat insulation material block.
Wherein the temperature-raising program is: the muffle furnace was sequentially heated at a rate of 8 ℃/min to 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃, 1000 ℃ and held at each of the above temperature points for 1 hour.
Tests show that the nano heat-insulating material block after surface gradient hardening has no powder falling on the surface, the total thickness of the surface hardening layer is 1.62mm, and the density of the hardening area is 1.56g/cm 3 The compactness is good; the compression strength of the nanometer heat insulation material block is improved to 3.8MPa from 2.3MPa before hardening.
Comparative example
A comparison was made with example 3:
1) Under a dry environment, adding boron oxide powder with the particle size of less than 100 mu m into a ball milling tank, adding white oil with the mass of 3 percent of boron oxide into the ball milling tank, and carrying out ball milling for 6 hours at the speed of 300r/min to obtain modified boron oxide powder;
2) Uniformly mixing the modified boron oxide powder, boron nitride powder, boron carbide powder and polymer particles according to a mass ratio of 15;
wherein the amount m of the composition A is determined according to the surface area S of the nano heat insulating material member, and the calculation formula is m = S × 0.3g/cm 2 。
Wherein the particle diameters of the boron nitride powder and the boron carbide powder are both less than 100 mu m.
Wherein, the polymer particles are polyethylene glycol.
3) Adding the composition A into a solvent B, and stirring until the polymer particles are completely dissolved to obtain a composition B;
wherein the solvent B is water.
Wherein the dosage of the solvent B is 1.5 times of that of the composition A.
4) Uniformly coating the composition B on the inner surface of the ceramic box, and uniformly attaching the composition A on the inner surface of the ceramic box after the solvent B is volatilized;
wherein, the ceramic box is an alumina box.
Wherein the ceramic box has an opening and closing function, and is sealed in a closed state.
5) And (2) placing the nano heat-insulating material component in a ceramic box to ensure that the nano heat-insulating material component is not in direct contact with the composition A, then keeping the ceramic box in an open state, placing the ceramic box in a muffle furnace, performing heat treatment according to a temperature rise program, cooling to room temperature, and taking out to obtain the nano heat-insulating material block with the gradient hardened surface.
Wherein the temperature-raising program is: the muffle furnace is sequentially heated to 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃ and 1000 ℃ at the speed of 8 ℃/min, and heat preservation is not carried out at each temperature point.
Tests show that the nano heat-insulating material block subjected to surface gradient hardening has no obvious hardened layer on the surface, the total thickness of the hardened layer is less than 0.3mm, and the density of the hardened area is 0.83g/cm 3 The compactness is poor, and the surface still has powder falling; the compression strength of the nanometer heat insulation material block body is not obviously changed.
Although the present invention has been described with reference to the above embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A surface gradient hardening method of a nanometer heat insulation material is characterized by comprising the following steps:
1) Under a dry environment, adding boron oxide powder into a ball milling tank, adding white oil which is 1-5% of the boron oxide by mass into the ball milling tank, and carrying out ball milling for 3-10 hours at the speed of 100-400r/min to obtain modified boron oxide powder;
2) Uniformly mixing the modified boron oxide powder, the boron nitride powder, the boron carbide powder and the polymer particles according to the mass ratio of (10-20) to (1-2) to obtain a composition A;
3) Adding the composition A into a solvent B, and stirring until the polymer particles are completely dissolved to obtain a composition B;
4) Uniformly coating the composition B on the inner surface of the ceramic box, and uniformly attaching the composition A on the inner surface of the ceramic box after the solvent B is volatilized;
5) And (2) placing the nano heat-insulating material component in a ceramic box to ensure that the nano heat-insulating material component is not in direct contact with the composition A, then sealing the ceramic box, placing the ceramic box in a muffle furnace, performing heat treatment according to a temperature rise program, cooling to room temperature, and taking out to obtain the nano heat-insulating material block with the gradient hardened surface.
2. The method of claim 1, wherein the boron oxide powder has a particle size of less than 100 μ ι η.
3. The method of claim 1, wherein the amount m of the composition a is determined according to the surface area S of the nano heat insulating material member, calculated as m = sx (0.1-0.4) g/cm 2 。
4. The method of claim 1, wherein the boron nitride powder and the boron carbide powder each have a particle size of less than 100 μm.
5. The method of claim 1, wherein the polymer particles have a cleavage temperature of less than 350 ℃ and are selected from the group consisting of polyethylene glycol and polyvinyl alcohol.
6. The method according to claim 1, wherein the solvent B is a good solvent for polymer particles.
7. The method of claim 1, wherein the amount of solvent B is at least 1 times that of composition a.
8. The method of claim 1, wherein the ceramic cassette is one of a silicon carbide cassette, an alumina cassette, and a zirconia cassette.
9. The method of claim 1, wherein the ceramic container has an opening and closing function, and is sealed in a closed state.
10. The method of claim 1, wherein the temperature ramp program is: the muffle furnace is heated to 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃ and 1000 ℃ in turn at the speed of 5-10 ℃/min, and the temperature is kept for 1 hour at each temperature point.
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