CN115872776B - Surface gradient hardening method of nano heat insulation material - Google Patents
Surface gradient hardening method of nano heat insulation material Download PDFInfo
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Abstract
The invention discloses a surface gradient hardening method of a nano heat insulation material, and belongs to the technical field of preparation of nano heat insulation materials. Ball milling boron oxide powder and white oil in a dry environment to obtain modified boron oxide powder; uniformly mixing modified boron oxide powder with boron nitride powder, boron carbide powder and polymer particles to obtain a composition A; adding the composition A into the 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 (3) placing the nano heat-insulating material component in a ceramic box, sealing the ceramic box, placing the ceramic box in a muffle furnace, and cooling and taking out the ceramic box after heat treatment to obtain the nano heat-insulating material block with the surface hardened gradient. The invention can solve the problems of loose surface structure and easy powder falling of the nano heat insulation material component.
Description
Technical Field
The invention belongs to the technical field of preparation of nanometer heat insulation materials, and particularly relates to a surface gradient hardening method of a nanometer heat insulation material.
Background
The nano heat insulating material is a novel high-performance heat insulating material, is prepared by taking nano powder as a main raw material through mould pressing, has the advantages of low density, good heat insulating performance, good temperature resistance, low cost and the like, and has remarkable application prospect in the fields of aerospace, metallurgy, construction and the like. However, since the nano heat-insulating material is formed by molding nano powder, the powder particles are not connected by chemical action, and the obvious defects of low surface strength and easy powder falling exist, so that the application of the nano heat-insulating material is severely limited. Under the prior art, the powder falling problem can be solved to a certain extent by preparing the coating on the surface, and the heat insulation performance of the nano heat insulation material is improved, but the overall strength and the surface hardness of the nano heat insulation material cannot be obviously increased. Therefore, it is necessary to invent a surface gradient hardening method of the nano heat insulation material, and the strength and hardness of the nano heat insulation material are optimized.
Disclosure of Invention
The invention aims to solve the problem that the surface structure of a nano heat insulation material member is loose and powder is easy to fall, and provides a method for optimizing the strength and hardness of the nano heat insulation material.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a surface gradient hardening method of a nano heat insulation material, comprising the following steps:
1) Adding boron oxide powder into a ball milling tank in a dry environment, adding white oil accounting for 1-5% of the mass of boron oxide into the ball milling tank, and ball milling for 3-10 hours at a speed of 100-400r/min to obtain modified boron oxide powder;
2) Uniformly mixing modified boron oxide powder, boron nitride powder, boron carbide powder and polymer particles according to the mass ratio of (10-20): (1-2) to obtain a composition A;
3) Adding the composition A into the 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-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, sealing the ceramic box, placing the ceramic box in a muffle furnace, performing heat treatment according to a heating program, cooling to room temperature, and taking out to obtain the nano heat-insulating material block with the surface hardened gradient.
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 calculated formula is m=sx (0.1 to 0.4) g/cm 2 。
Preferably, the particle size of the boron nitride powder and the boron carbide powder is less than 100 mu m.
Preferably, the polymer particles have a cleavage temperature of less than 350 ℃, preferably polyethylene glycol, polyvinyl alcohol, and the like.
Preferably, the solvent B is a good solvent for the polymer particles.
Preferably, the solvent B is used in an amount of at least 1, 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 container has an opening and closing function, and is sealed in a closed state.
Preferably, the temperature increase program is: the muffle furnace is heated to 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃, 1000 ℃ at a speed of 5-10 ℃/min in sequence, 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 insulation material to generate borosilicate glass phase, so that the nano heat insulation material is hardened. The boron oxide vapor has diffusivity, so that the boron oxide vapor can be diffused from the surface to the inside of the nano heat insulation material in a gradient way, and the effect of the gradient hardening of the surface of the nano heat insulation material is realized. The white oil is white mineral oil which is refined in industry and mainly contains liquid saturated hydrocarbon, and the surface of the boron oxide is subjected to hydrophobic modification, so that the boron oxide is prevented from going bad after boric acid is generated due to water absorption. The white oil is used for coating and hydrophobic treatment of the boron oxide, so that the moisture absorption failure of the boron oxide in the air is effectively avoided.
2) Boron carbide can be oxidized to form boron oxide at more than 500 ℃, and boron nitride can be oxidized to form boron oxide at more than 700 ℃. As the boron oxide in the composition A is heated and melted first, the boron carbide and the boron nitride are wrapped by the boron oxide and cannot contact oxygen, and only the boron oxide in the composition A generates steam to carry out gradient hardening on the nano heat insulation material; the temperature rising program is adopted, boron oxide is gradually evaporated and exhausted along with the time of temperature rising, boron carbide and boron nitride are exposed and are in contact with air for oxidation, new boron oxide steam is generated and released, after the steam is diffused to the surface of the nano heat insulation material, the steam reacts with silicon dioxide in the nano heat insulation material to generate borosilicate glass phase, and gradient hardening is continuously carried out on the nano heat insulation material. By adopting the technical means, the slow release of the boron oxide caused by the once high-concentration release of the boron oxide is avoided, the concentration of the boron oxide steam is controllable, and the gradient hardening of the surface of the nano heat-insulating material achieves the optimal effect.
3) Boron oxide vapor is utilized instead of directly doping boron oxide into the nano heat insulation material, so that the phenomenon of uneven hardening and uncontrollable hardening caused by uneven boron oxide doping is avoided.
Drawings
Fig. 1 is a surface gradient hardening flow chart of a nano heat insulation material according to the present invention.
Detailed Description
In order to make the above features and advantages of the present invention more comprehensible, embodiments accompanied with figures are described in detail below.
Example 1
1) Adding boron oxide powder with the particle size smaller than 100 mu m into a ball milling tank in a dry environment, adding white oil with the mass of 1% of that of boron oxide into the ball milling tank, and performing ball milling at the speed of 400r/min for 10 hours to obtain modified boron oxide powder;
2) Uniformly mixing modified boron oxide powder with boron nitride powder, boron carbide powder and polymer particles according to the mass ratio of 10:10:10:1 to obtain a composition A;
wherein the amount m of the composition A is determined according to the surface area S of the nano heat insulating material memberThe calculation formula is m=S×0.1g/cm 2 。
Wherein the particle sizes of the boron nitride powder and the boron carbide powder are smaller than 100 mu m.
Wherein the polymer particles are polyvinyl alcohol.
3) Adding the composition A into the solvent B, and stirring until the polymer particles are completely dissolved to obtain a composition B;
wherein the solvent B is water.
Wherein the amount of the solvent B is 1 time 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 a silicon carbide box.
Wherein, the ceramic box has opening and closing functions, and is sealed in a closing state.
5) And (3) 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, sealing the ceramic box, placing the ceramic box in a muffle furnace, performing heat treatment according to a heating program, cooling to room temperature, and taking out to obtain the nano heat-insulating material block with the surface hardened gradient.
Wherein, the temperature rise program is: the muffle furnace was heated to 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃, 1000 ℃ in sequence at a rate of 5 ℃/min, and the temperature was kept for 1 hour at each temperature point.
Through testing, the nano heat insulation 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 compressive strength of the nano heat insulation material block is improved from 2.3MPa to 3.5MPa before hardening.
Example 2
1) Adding boron oxide powder with the particle size smaller than 100 mu m into a ball milling tank in a dry environment, adding white oil with the mass of 5% of that of boron oxide into the ball milling tank, and performing ball milling at the speed of 100r/min for 3 hours to obtain modified boron oxide powder;
2) Uniformly mixing modified boron oxide powder with boron nitride powder, boron carbide powder and polymer particles according to the mass ratio of 20:15:20:2 to obtain a composition A;
wherein the amount m of the composition A is determined according to the surface area S of the nano heat insulation material component, and the calculated formula is m=S×0.4g/cm 2 。
Wherein the particle sizes of the boron nitride powder and the boron carbide powder are smaller than 100 mu m.
Wherein the polymer particles are polyvinyl alcohol.
3) Adding the composition A into the solvent B, and stirring until the polymer particles are completely dissolved to obtain a composition B;
wherein the solvent B is water.
Wherein the amount of the solvent B is 2 times 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 opening and closing functions, and is sealed in a closing state.
5) And (3) 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, sealing the ceramic box, placing the ceramic box in a muffle furnace, performing heat treatment according to a heating program, cooling to room temperature, and taking out to obtain the nano heat-insulating material block with the surface hardened gradient.
Wherein, the temperature rise program is: the muffle furnace was heated to 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃, 1000 ℃ in sequence at a rate of 10 ℃/min, and the temperature was kept for 1 hour at each temperature point.
Through testing, the nano heat insulation material block subjected to surface gradient hardening has no powder falling on the surface, the total thickness of a surface hardening layer is 1.83mm, and the density of a hardening area is 1.62g/cm 3 The compactness is good; the compressive strength of the nano heat insulation material block is improved from 2.3MPa to 3.8MPa before hardening.
Example 3
1) Adding boron oxide powder with the particle size smaller than 100 mu m into a ball milling tank in a dry environment, adding white oil with the mass of 3% of that of boron oxide into the ball milling tank, and performing ball milling at the speed of 300r/min for 6 hours to obtain modified boron oxide powder;
2) Uniformly mixing modified boron oxide powder with boron nitride powder, boron carbide powder and polymer particles according to the mass ratio of 15:20:15:2 to obtain a composition A;
wherein the amount m of the composition A is determined according to the surface area S of the nano heat insulation material component, and the calculated formula is m=S×0.3g/cm 2 。
Wherein the particle sizes of the boron nitride powder and the boron carbide powder are smaller than 100 mu m.
Wherein the polymer particles are polyethylene glycol.
3) Adding the composition A into the solvent B, and stirring until the polymer particles are completely dissolved to obtain a composition B;
wherein the solvent B is water.
Wherein the amount of the solvent B is 1.5 times 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 opening and closing functions, and is sealed in a closing state.
5) And (3) 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, sealing the ceramic box, placing the ceramic box in a muffle furnace, performing heat treatment according to a heating program, cooling to room temperature, and taking out to obtain the nano heat-insulating material block with the surface hardened gradient.
Wherein, the temperature rise program is: the muffle furnace was heated to 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃, 1000 ℃ in sequence at a rate of 8 ℃/min, and the temperature was kept for 1 hour at each temperature point.
Through testing, the nano heat insulation material block subjected to surface gradient hardening has no powder falling on the surface, the total thickness of a surface hardening layer is 1.62mm, and the density of a hardening area is 1.56g/cm 3 The compactness is good; the compressive strength of the nano heat insulation material block is improved from 2.3MPa to 3.8MPa before hardening.
Comparative example
Comparison is made with example 3:
1) Adding boron oxide powder with the particle size smaller than 100 mu m into a ball milling tank in a dry environment, adding white oil with the mass of 3% of that of boron oxide into the ball milling tank, and performing ball milling at the speed of 300r/min for 6 hours to obtain modified boron oxide powder;
2) Uniformly mixing modified boron oxide powder, boron nitride powder, boron carbide powder and polymer particles according to the mass ratio of 15:20:10:2 to obtain a composition A;
wherein the amount m of the composition A is determined according to the surface area S of the nano heat insulation material component, and the calculated formula is m=S×0.3g/cm 2 。
Wherein the particle sizes of the boron nitride powder and the boron carbide powder are smaller than 100 mu m.
Wherein the polymer particles are polyethylene glycol.
3) Adding the composition A into the solvent B, and stirring until the polymer particles are completely dissolved to obtain a composition B;
wherein the solvent B is water.
Wherein the amount of the solvent B is 1.5 times 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 opening and closing functions, and is sealed in a closing state.
5) And 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 heating program, cooling to room temperature, and taking out to obtain the nano heat-insulating material block with the surface gradient hardened.
Wherein, the temperature rise program is: the muffle furnace was heated to 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃, 1000 ℃ in sequence at a rate of 8 ℃/min, and no heat preservation was performed at each temperature point.
Through tests, the nano heat-insulating material block subjected to surface gradient hardening has no obvious hardening layer on the surface, the total thickness of the hardening layer is less than 0.3mm, and the density of a hardening area is 0.83g/cm 3 The compactness is poor, and powder still exists on the surface; the compressive strength of the nano heat insulation material block is not obviously changed.
Although the present invention has been described with reference to the above embodiments, it should be understood that the invention is not limited thereto, and that modifications and equivalents may be made thereto by those skilled in the art, which modifications and equivalents are intended to be included within the scope of the present invention as defined by the appended claims.
Claims (8)
1. A surface gradient hardening method of a nano heat insulation material, which is characterized by comprising the following steps:
1) Adding boron oxide powder into a ball milling tank in a dry environment, adding white oil accounting for 1% -5% of the mass of boron oxide into the ball milling tank, and performing ball milling at a speed of 100-400r/min for 3-10 hours to obtain modified boron oxide powder;
2) Uniformly mixing modified boron oxide powder, boron nitride powder, boron carbide powder and polymer particles according to the mass ratio of (10-20): (1-2) to obtain a composition A; the cracking temperature of the polymer particles is lower than 350 ℃, and the polymer particles are selected from one of polyethylene glycol and polyvinyl alcohol;
3) Adding the composition A into the 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) Placing the nano heat-insulating material component inside a ceramic box, ensuring that the nano heat-insulating material component is not in direct contact with the composition A, sealing the ceramic box, placing the ceramic box in a muffle furnace, and performing heat treatment according to a heating program, wherein the heating program is as follows: sequentially heating the muffle furnace to 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃, 1000 ℃ at a speed of 5-10 ℃/min, and preserving heat at each temperature point for 1 hour; cooling to room temperature and taking out to obtain a nano heat insulation material block with the surface hardened in a gradient manner; boron oxide in the composition A attached to the inner surface of the ceramic box is heated and melted, and generated boron oxide steam reacts with silicon dioxide in the nano heat insulation material to generate borosilicate glass phase, so that the nano heat insulation material is hardened.
2. The method of claim 1, wherein the boron oxide powder has a particle size of less than 100 μm.
3. The method according to 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, and the calculated formula is m=sx (0.1 to 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 solvent B is a good solvent for the polymeric particles.
6. The method of claim 1, wherein the solvent B is used in an amount of at least 1-fold that of composition a.
7. The method of claim 1, wherein the ceramic box is one of a silicon carbide box, an aluminum oxide box, and a zirconium oxide box.
8. The method of claim 1, wherein the ceramic box has an opening and closing function, and is sealed in a closed state.
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