CN114368964A - Preparation method, product and application of nano aluminum oxide material - Google Patents
Preparation method, product and application of nano aluminum oxide material Download PDFInfo
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Abstract
The invention discloses a preparation method of a nano aluminum oxide material, which comprises the following steps: step 1, preparing a metal stabilizer solution and an organic aluminum salt solution; step 2, mixing the metal stabilizer solution with the organic aluminum salt solution to obtain an organic aluminum salt reaction solution; step 3, adding deionized water to supplement the volume of the solution to the original volume after concentration, simultaneously dropwise adding a nitric acid solution, and then performing reflux aging treatment to obtain alumina sol; step 4, adding the niobium silicide nitride nano microspheres, and drying under reduced pressure to obtain aluminum oxide/niobium silicide nitride nano microspheres; and 5, placing the aluminum oxide material in a reaction furnace, and carrying out heat preservation treatment at the temperature of 1125-1200 ℃ for 2-4 h to obtain the nano aluminum oxide material. The nano aluminum oxide material prepared by the method has high strength, good oxidation resistance, corrosion resistance and wear resistance, can have long-term service effect, and is suitable for preparing materials of mechanical equipment or conveying pipelines in the metallurgical power industry.
Description
Technical Field
The invention relates to the field of nano materials, in particular to a preparation method, a product and application of a nano aluminum oxide material.
Background
The nanoscale aluminum oxide material has the characteristics of high hardness, high strength, heat resistance, corrosion resistance and the like, and is widely applied to the fields of machinery, metallurgy, petroleum, chemical engineering, ceramics, aerospace and the like. The rapid development of industrial technology makes the service conditions of engineering equipment and components increasingly strict, and thus the requirements for material properties are also increasingly strict. For example, the material must have one or more of high temperature resistance, wear resistance, corrosion resistance, thermal shock resistance, fatigue resistance and the like. In the metallurgical power industry, the service conditions of mechanical equipment and pipelines are worse, particularly, the pipelines in a power plant are worn extremely severely under the high-temperature and wear service conditions, and the phenomenon of pipe explosion can be caused seriously. However, the performance of a single material, such as an aluminum oxide material, in the aspects of high-temperature oxidation resistance, corrosion resistance, wear resistance, friction reduction and the like cannot completely meet the requirements of service conditions, so that the service life of engineering equipment is shortened, and the service environment is limited. Therefore, the invention aims at the aluminum oxide material to carry out composite modification treatment so as to obtain a material with more excellent performance.
Disclosure of Invention
Aiming at the problem that the performance of the aluminum oxide material in the aspects of high-temperature oxidation resistance, corrosion resistance, wear resistance and the like in the prior art can not completely meet the requirement of service conditions, the invention aims to provide a preparation method, a product and application of a nano aluminum oxide material.
The purpose of the invention is realized by adopting the following technical scheme:
in a first aspect, the present invention provides a method for preparing a nano aluminum oxide material, comprising the following steps:
step 1, weighing a metal stabilizer, mixing the metal stabilizer into deionized water, and fully and uniformly mixing to obtain a metal stabilizer solution; weighing organic aluminum salt, mixing with an organic solvent, and fully and uniformly mixing to obtain an organic aluminum salt solution;
step 2, slowly dripping an organic aluminum salt solution into the metal stabilizer solution while stirring, and continuing the reaction treatment after completely dripping to obtain an organic aluminum salt reaction solution;
step 3, concentrating the organic aluminum salt reaction solution to half of the volume of the original reaction solution, adding deionized water to supplement the volume of the original reaction solution again, simultaneously dropwise adding a nitric acid solution, and then performing reflux aging treatment to obtain alumina sol;
step 4, adding the niobium silicide nitride nano microspheres into the alumina sol, fully and uniformly mixing, and then drying under reduced pressure to obtain alumina/niobium silicide nitride nano microspheres;
and 5, placing the aluminum oxide/niobium silicide nitride nano microspheres in a reaction furnace, heating to 1125-1200 ℃ under the action of inert gas, carrying out heat preservation treatment for 2-4 h, and cooling to room temperature to obtain the nano aluminum oxide material.
Preferably, in the step 1, the metal stabilizer is ethylenediamine tetraacetic acid, and the mass ratio of the metal stabilizer to the deionized water is 1: 20-50.
Preferably, in step 1, the organic aluminum salt includes one or more of aluminum isopropoxide, aluminum n-butoxide and aluminum sec-butoxide, the organic solvent is one or more of isopropanol, n-butanol and sec-butoxide, and the mass ratio of the organic aluminum salt to the organic solvent is 1: 6-12.
Preferably, in the step 2, the reaction temperature is 80-85 ℃, the dropping speed is 20-30 drops/min, and the reaction time is 1-2 h after complete dropping.
Preferably, in the step 2, the mass ratio of the metal stabilizer solution to the organic aluminum salt solution is 1: 0.8-1.
Preferably, in step 3, the concentration process is as follows: continuously stirring and evaporating at the temperature of 90-95 ℃.
Preferably, in the step 3, the nitric acid solution is dropwise added until the pH value of the reaction system reaches 3.5-4.0, and the time of the reflux aging treatment is 12-18 h.
Preferably, in step 4, the preparation method of the niobium silicide nitride nanosphere comprises:
s1, weighing nanoscale niobium silicide powder, dispersing the nanoscale niobium silicide powder into deionized water, adding a silane coupling agent, stirring at room temperature for 2-5 hours, filtering, and drying to obtain surface-activated niobium silicide powder; wherein the mass ratio of the niobium silicide powder to the silane coupling agent to the deionized water is 1: 0.05-0.1: 6-10;
s2, dispersing the surface-activated niobium silicide powder into ammonia water with the mass fraction of 10%, adding resorcinol, carrying out ultrasonic homogenization, dropwise adding a formaldehyde aqueous solution with the mass fraction of 35%, carrying out continuous stirring treatment for 18-24 h at room temperature, filtering, collecting precipitate, and drying to obtain resorcinol formaldehyde polymer/niobium silicide nano-microspheres; wherein the mass ratio of the surface-activated niobium silicide powder to the aqueous solution of ammonia water to formaldehyde is 0.26-0.52: 3-4: 1, and the mass ratio of resorcinol to the aqueous solution of formaldehyde is 0.5-0.8: 1;
s3, placing the resorcinol formaldehyde polymer/niobium silicide nano-microspheres into a reaction furnace, heating to 400-500 ℃, and treating for 2-4 hours under the air condition to obtain porous carbon-coated niobium silicide composite microspheres;
s4, cooling the reaction furnace to 120-180 ℃, carrying out heat preservation treatment for 1-2 hours, introducing nitrogen to replace air, pressurizing to 10-15 MPa, heating to 280-330 ℃, carrying out heat preservation treatment for 2-4 hours, cooling to normal pressure and normal temperature, and crushing to obtain the niobium silicide nitride nano-microspheres.
Preferably, in the step 4, the mass ratio of the alumina sol to the niobium silicide nitride nanospheres is 1: 0.1-0.4.
Preferably, the particle size of the nano aluminum oxide material is 200-500 nm.
In a second aspect, the invention provides a nano aluminum oxide material product, which is prepared by adopting the preparation method of the nano aluminum oxide material.
In a third aspect, the invention provides an application of the nano aluminum oxide material, wherein the product prepared by the preparation method of the nano aluminum oxide material is applied to the manufacturing of mechanical equipment or transportation pipelines.
The invention has the beneficial effects that:
the nano aluminum oxide material prepared by the invention has the advantages of simple and convenient preparation process, compact process flow and strong operability, and is suitable for industrial large-scale production.
The nano aluminum oxide material prepared by the method has high strength, good oxidation resistance, corrosion resistance and wear resistance, can have long-term service effect, and is suitable for preparing materials of mechanical equipment or conveying pipelines in the metallurgical power industry.
The nano aluminum oxide material prepared by the invention is prepared into aluminum oxide sol by using organic aluminum salt, then the niobium silicide nitride nano microspheres are added to modify the aluminum oxide sol so that the aluminum oxide is adsorbed on the surfaces of the nano microspheres, and then the aluminum oxide is more firmly combined with the nano microspheres through high-temperature sintering treatment, so that the nano aluminum oxide material with more excellent performance is finally obtained.
Detailed Description
For the purpose of more clearly illustrating the present invention and more clearly understanding the technical features, objects and advantages of the present invention, the technical solutions of the present invention will now be described in detail below, but are not to be construed as limiting the implementable scope of the present invention.
The preparation process of the niobium silicide nitride nano microsphere comprises the following steps: firstly, carrying out surface activation treatment on niobium silicide powder by using a silane coupling agent, then preparing the niobium silicide composite microsphere coated with the resorcinol formaldehyde polymer by using the reaction of resorcinol and formaldehyde, then placing the niobium silicide composite microsphere in a reaction furnace to carry out carbonization treatment on the polymer, and finally carrying out nitridation treatment on the obtained microsphere. Compared with the composite with silicon nitride and niobium nitride added separately, the addition of the niobium silicide nitride nanospheres shows better performance, and the suspected reason is that the unique preparation process of the invention causes part of niobium silicide to be not reacted, and the prepared niobium silicide nitride composite microspheres also have better binding property with aluminum oxide.
The carbonization temperature of the resorcinol-formaldehyde resin is 400-500 ℃, the surface of the niobium silicide powder is partially oxidized in the process, but the niobium silicide powder is reduced by carbon generated at the same time due to the overhigh temperature, so that the niobium silicide powder is subjected to heat treatment again at a lower temperature (120-180 ℃) to oxidize the surface of the niobium silicide powder again, and a nitride cushion is generated better in the follow-up process.
The invention is further described below with reference to the following examples.
Example 1
A preparation method of a nano aluminum oxide material comprises the following steps:
step 1, weighing ethylenediamine tetraacetic acid, mixing the ethylenediamine tetraacetic acid with deionized water, and fully and uniformly mixing to obtain a metal stabilizer solution; weighing and mixing aluminum isopropoxide and isopropanol, and fully and uniformly mixing to obtain an organic aluminum salt solution; wherein the mass ratio of the ethylene diamine tetraacetic acid to the deionized water is 1: 35; the mass ratio of the aluminum isopropoxide to the isopropanol is 1: 10;
step 2, dropwise adding an organic aluminum salt solution into the metal stabilizer solution at the speed of 20-30 drops/min while stirring, and continuously reacting for 2 hours at the temperature of 80 ℃ after completely dropwise adding to obtain an organic aluminum salt reaction solution; wherein the mass ratio of the metal stabilizer solution to the organic aluminum salt solution is 1: 0.8;
step 3, continuously stirring and evaporating the organic aluminum salt reaction solution at the temperature of 90 ℃ until the volume of the original reaction solution is half, adding deionized water to supplement the volume of the original reaction solution again, simultaneously dropwise adding a nitric acid solution until the pH value of the reaction system reaches 3.5-4.0, and performing reflux aging for 18 hours to obtain alumina sol;
step 4, adding the niobium silicide nitride nano microspheres into the alumina sol, fully and uniformly mixing, and then drying under reduced pressure to obtain alumina/niobium silicide nitride nano microspheres; wherein the mass ratio of the alumina sol to the niobium silicide nitride nano-microspheres is 1: 0.3;
and 5, placing the aluminum oxide/niobium silicide nitride nano microspheres in a reaction furnace, heating to 1150 ℃ under the action of inert gas, carrying out heat preservation treatment for 3 hours, and cooling to room temperature to obtain the nano aluminum oxide material.
The preparation method of the niobium silicide nitride nano-microsphere comprises the following steps:
s1, weighing nanoscale niobium silicide powder, dispersing the nanoscale niobium silicide powder into deionized water, adding a silane coupling agent, stirring at room temperature for 3 hours, filtering, and drying to obtain surface-activated niobium silicide powder; wherein the mass ratio of the niobium silicide powder to the silane coupling agent to the deionized water is 1:0.06: 8;
s2, dispersing the surface-activated niobium silicide powder into ammonia water with the mass fraction of 10%, adding resorcinol, carrying out ultrasonic homogenization, dropwise adding a formaldehyde aqueous solution with the mass fraction of 35%, continuously stirring at room temperature for 18h, filtering, collecting precipitate, and drying to obtain resorcinol formaldehyde polymer/niobium silicide nano-microspheres; wherein the mass ratio of the surface-activated niobium silicide powder, ammonia water and an aqueous solution of formaldehyde is 0.35:3:1, and the mass ratio of resorcinol and an aqueous solution of formaldehyde is 0.6: 1;
s3, placing the resorcinol formaldehyde polymer/niobium silicide nano-microspheres into a reaction furnace, heating to 450 ℃, and treating for 3 hours under the air condition to obtain porous carbon coated niobium silicide composite microspheres;
s4, cooling the reaction furnace to 150 ℃, carrying out heat preservation treatment for 2 hours, introducing nitrogen to replace air, pressurizing to 10MPa, heating to 300 ℃, carrying out heat preservation treatment for 3 hours, cooling to normal pressure and normal temperature, and crushing to obtain the nano-particles to obtain the niobium silicide nitride nano-microspheres.
Example 2
A preparation method of a nano aluminum oxide material comprises the following steps:
step 1, weighing ethylenediamine tetraacetic acid, mixing the ethylenediamine tetraacetic acid with deionized water, and fully and uniformly mixing to obtain a metal stabilizer solution; weighing n-butanol aluminum and mixing with n-butanol, and fully and uniformly mixing to obtain an organic aluminum salt solution; wherein the mass ratio of the ethylene diamine tetraacetic acid to the deionized water is 1: 20; the mass ratio of the n-butyl aluminum alkoxide to the n-butyl alcohol is 1: 6;
step 2, dropwise adding an organic aluminum salt solution into the metal stabilizer solution at the speed of 20-30 drops/min while stirring, and continuously reacting for 1h at the temperature of 80 ℃ after complete dropwise addition to obtain an organic aluminum salt reaction solution; wherein the mass ratio of the metal stabilizer solution to the organic aluminum salt solution is 1: 0.8;
step 3, continuously stirring and evaporating the organic aluminum salt reaction solution at the temperature of 90 ℃ until the volume of the original reaction solution is half, adding deionized water to supplement the volume of the original reaction solution again, simultaneously dropwise adding a nitric acid solution until the pH value of the reaction system reaches 3.5-4.0, and performing reflux aging for 12 hours to obtain alumina sol;
step 4, adding the niobium silicide nitride nano microspheres into the alumina sol, fully and uniformly mixing, and then drying under reduced pressure to obtain alumina/niobium silicide nitride nano microspheres; wherein the mass ratio of the alumina sol to the niobium silicide nitride nano-microspheres is 1: 0.1;
and 5, placing the aluminum oxide/niobium silicide nitride nano microspheres in a reaction furnace, heating to 1125 ℃ under the action of inert gas, carrying out heat preservation treatment for 2 hours, and cooling to room temperature to obtain the nano aluminum oxide material.
The preparation method of the niobium silicide nitride nano-microsphere comprises the following steps:
s1, weighing nanoscale niobium silicide powder, dispersing the nanoscale niobium silicide powder into deionized water, adding a silane coupling agent, stirring at room temperature for 2 hours, filtering, and drying to obtain surface-activated niobium silicide powder; wherein the mass ratio of the niobium silicide powder to the silane coupling agent to the deionized water is 1:0.05: 6;
s2, dispersing the surface-activated niobium silicide powder into ammonia water with the mass fraction of 10%, adding resorcinol, carrying out ultrasonic homogenization, dropwise adding a formaldehyde aqueous solution with the mass fraction of 35%, continuously stirring at room temperature for 18h, filtering, collecting precipitate, and drying to obtain resorcinol formaldehyde polymer/niobium silicide nano-microspheres; wherein the mass ratio of the surface-activated niobium silicide powder, ammonia water and an aqueous solution of formaldehyde is 0.26:3:1, and the mass ratio of resorcinol and an aqueous solution of formaldehyde is 0.5: 1;
s3, placing the resorcinol formaldehyde polymer/niobium silicide nano-microspheres into a reaction furnace, heating to 400 ℃, and treating for 2 hours under the air condition to obtain porous carbon coated niobium silicide composite microspheres;
s4, cooling the reaction furnace to 120 ℃, carrying out heat preservation treatment for 1 hour, introducing nitrogen to replace air, pressurizing to 10MPa, heating to 280 ℃, carrying out heat preservation treatment for 2 hours, cooling to normal pressure and normal temperature, and crushing to obtain the niobium silicide nitride nano-microspheres.
Example 3
A preparation method of a nano aluminum oxide material comprises the following steps:
step 1, weighing ethylenediamine tetraacetic acid, mixing the ethylenediamine tetraacetic acid with deionized water, and fully and uniformly mixing to obtain a metal stabilizer solution; weighing and mixing aluminum sec-butoxide and sec-butanol, and fully and uniformly mixing to obtain an organic aluminum salt solution; wherein the mass ratio of the ethylene diamine tetraacetic acid to the deionized water is 1: 50; the mass ratio of the aluminum sec-butoxide to the sec-butanol is 1: 12;
step 2, dropwise adding an organic aluminum salt solution into the metal stabilizer solution at the speed of 20-30 drops/min while stirring, and continuously reacting for 2 hours at 85 ℃ after completely dropwise adding to obtain an organic aluminum salt reaction solution; wherein the mass ratio of the metal stabilizer solution to the organic aluminum salt solution is 1: 1;
step 3, continuously stirring and evaporating the organic aluminum salt reaction solution at the temperature of 95 ℃ until the volume of the original reaction solution is half, adding deionized water to supplement the volume of the original reaction solution again, simultaneously dropwise adding a nitric acid solution until the pH value of the reaction system reaches 3.5-4.0, and performing reflux aging for 18 hours to obtain alumina sol;
step 4, adding the niobium silicide nitride nano microspheres into the alumina sol, fully and uniformly mixing, and then drying under reduced pressure to obtain alumina/niobium silicide nitride nano microspheres; wherein the mass ratio of the alumina sol to the niobium silicide nitride nano-microspheres is 1: 0.4;
and 5, placing the aluminum oxide/niobium silicide nitride nano microspheres in a reaction furnace, heating to 1200 ℃ under the action of inert gas, carrying out heat preservation treatment for 4 hours, and cooling to room temperature to obtain the nano aluminum oxide material.
The preparation method of the niobium silicide nitride nano-microsphere comprises the following steps:
s1, weighing nanoscale niobium silicide powder, dispersing the nanoscale niobium silicide powder into deionized water, adding a silane coupling agent, stirring at room temperature for 5 hours, filtering, and drying to obtain surface-activated niobium silicide powder; wherein the mass ratio of the niobium silicide powder to the silane coupling agent to the deionized water is 1:0.1: 10;
s2, dispersing the surface-activated niobium silicide powder into ammonia water with the mass fraction of 10%, adding resorcinol, carrying out ultrasonic homogenization, dropwise adding a formaldehyde aqueous solution with the mass fraction of 35%, continuously stirring at room temperature for 24 hours, filtering, collecting precipitate, and drying to obtain resorcinol formaldehyde polymer/niobium silicide nano-microspheres; wherein the mass ratio of the surface-activated niobium silicide powder, ammonia water and an aqueous solution of formaldehyde is 0.52:4:1, and the mass ratio of resorcinol and an aqueous solution of formaldehyde is 0.8: 1;
s3, placing the resorcinol formaldehyde polymer/niobium silicide nano-microspheres into a reaction furnace, heating to 500 ℃, and treating for 4 hours under the air condition to obtain porous carbon coated niobium silicide composite microspheres;
s4, cooling the reaction furnace to 180 ℃, carrying out heat preservation treatment for 2 hours, introducing nitrogen to replace air, pressurizing to 15MPa, heating to 330 ℃, carrying out heat preservation treatment for 4 hours, cooling to normal pressure and normal temperature, and crushing to obtain the niobium silicide nitride nano-microspheres.
Comparative example 1
(difference from comparative example 1 in that the niobium silicide nitride nanospheres were replaced with niobium silicide powder)
A preparation method of a nano aluminum oxide material comprises the following steps:
step 1, weighing ethylenediamine tetraacetic acid, mixing the ethylenediamine tetraacetic acid with deionized water, and fully and uniformly mixing to obtain a metal stabilizer solution; weighing and mixing aluminum isopropoxide and isopropanol, and fully and uniformly mixing to obtain an organic aluminum salt solution; wherein the mass ratio of the ethylene diamine tetraacetic acid to the deionized water is 1: 35; the mass ratio of the aluminum isopropoxide to the isopropanol is 1: 10;
step 2, dropwise adding an organic aluminum salt solution into the metal stabilizer solution at the speed of 20-30 drops/min while stirring, and continuously reacting for 2 hours at the temperature of 80 ℃ after completely dropwise adding to obtain an organic aluminum salt reaction solution; wherein the mass ratio of the metal stabilizer solution to the organic aluminum salt solution is 1: 0.8;
step 3, continuously stirring and evaporating the organic aluminum salt reaction solution at the temperature of 90 ℃ until the volume of the original reaction solution is half, adding deionized water to supplement the volume of the original reaction solution again, simultaneously dropwise adding a nitric acid solution until the pH value of the reaction system reaches 3.5-4.0, and performing reflux aging for 18 hours to obtain alumina sol;
step 4, adding niobium silicide powder into the alumina sol, fully and uniformly mixing, and then drying under reduced pressure to obtain alumina/niobium silicide composite powder; wherein the mass ratio of the alumina sol to the niobium silicide powder is 1: 0.3;
and 5, placing the aluminum oxide/niobium silicide composite powder in a reaction furnace, heating to 1150 ℃ under the action of inert gas, carrying out heat preservation treatment for 3h, and cooling to room temperature to obtain the nano aluminum oxide material.
Comparative example 2
(different from comparative example 1 in that no niobium silicide nitride nanosphere was added)
A preparation method of a nano aluminum oxide material comprises the following steps:
step 1, weighing ethylenediamine tetraacetic acid, mixing the ethylenediamine tetraacetic acid with deionized water, and fully and uniformly mixing to obtain a metal stabilizer solution; weighing and mixing aluminum isopropoxide and isopropanol, and fully and uniformly mixing to obtain an organic aluminum salt solution; wherein the mass ratio of the ethylene diamine tetraacetic acid to the deionized water is 1: 35; the mass ratio of the aluminum isopropoxide to the isopropanol is 1: 10;
step 2, dropwise adding an organic aluminum salt solution into the metal stabilizer solution at the speed of 20-30 drops/min while stirring, and continuously reacting for 2 hours at the temperature of 80 ℃ after completely dropwise adding to obtain an organic aluminum salt reaction solution; wherein the mass ratio of the metal stabilizer solution to the organic aluminum salt solution is 1: 0.8;
step 3, continuously stirring and evaporating the organic aluminum salt reaction solution at the temperature of 90 ℃ until the volume of the original reaction solution is half, adding deionized water to supplement the volume of the original reaction solution again, simultaneously dropwise adding a nitric acid solution until the pH value of the reaction system reaches 3.5-4.0, and performing reflux aging for 18 hours to obtain alumina sol;
step 4, drying the alumina sol under reduced pressure to obtain alumina powder;
and 5, placing the alumina powder in a reaction furnace, heating to 1150 ℃ under the action of inert gas, carrying out heat preservation treatment for 3 hours, and cooling to room temperature to obtain the nano alumina material.
In order to more clearly illustrate the present invention, the nano-alumina materials prepared in examples 1 to 3 and comparative examples 1 to 2 were compared for performance tests. The specific surface is detected using a surface analyzer; the high-temperature oxidation resistance is that 5.000g of nano aluminum oxide material is used for carrying out ten times of repeated sintering (1150 ℃) treatment, the mass change quantity is detected in each time of sintering, the mass average loss quantity after the ten times of sintering is comprehensively calculated, and the mass average loss quantity in each time of sintering is equal to the sum of the mass loss quantities of the ten times of sintering/10; the corrosion resistance detection is to place the nano aluminum oxide material under the condition of acid solution (1mol/L sulfuric acid solution) or alkali solution (1mol/L sodium hydroxide solution) for treatment for 72 hours to detect corrosion; abrasion resistance the abrasion was measured according to standard JCT848.1-2010 with the results shown in table 1:
TABLE 1 comparison of Properties of different Nano-alumina materials
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The preparation method of the nano aluminum oxide material is characterized by comprising the following steps of:
step 1, weighing a metal stabilizer, mixing the metal stabilizer into deionized water, and fully and uniformly mixing to obtain a metal stabilizer solution; weighing organic aluminum salt, mixing with an organic solvent, and fully and uniformly mixing to obtain an organic aluminum salt solution;
step 2, slowly dripping an organic aluminum salt solution into the metal stabilizer solution while stirring, and continuing the reaction treatment after completely dripping to obtain an organic aluminum salt reaction solution;
step 3, concentrating the organic aluminum salt reaction solution to half of the volume of the original reaction solution, adding deionized water to supplement the volume of the original reaction solution again, simultaneously dropwise adding a nitric acid solution, and then performing reflux aging treatment to obtain alumina sol;
step 4, adding the niobium silicide nitride nano microspheres into the alumina sol, fully and uniformly mixing, and then drying under reduced pressure to obtain alumina/niobium silicide nitride nano microspheres;
and 5, placing the aluminum oxide/niobium silicide nitride nano microspheres in a reaction furnace, heating to 1125-1200 ℃ under the action of inert gas, carrying out heat preservation treatment for 2-4 h, and cooling to room temperature to obtain the nano aluminum oxide material.
2. The method for preparing the nano aluminum oxide material as claimed in claim 1, wherein in the step 1, the metal stabilizer is ethylenediamine tetraacetic acid, and the mass ratio of the metal stabilizer to the deionized water is 1: 20-50.
3. The method for preparing the nano aluminum oxide material as claimed in claim 1, wherein in step 1, the organic aluminum salt comprises one or more of aluminum isopropoxide, aluminum n-butoxide and aluminum sec-butoxide, the organic solvent is one or more of isopropanol, n-butoxide and sec-butoxide, and the mass ratio of the organic aluminum salt to the organic solvent is 1: 6-12.
4. The method for preparing the nano aluminum oxide material as claimed in claim 1, wherein in the step 2, the reaction temperature is 80-85 ℃, the dropping speed is 20-30 drops/min, and the reaction time is 1-2 h after complete dropping.
5. The method for preparing the nano aluminum oxide material as claimed in claim 1, wherein in the step 2, the mass ratio of the metal stabilizer solution to the organic aluminum salt solution is 1: 0.8-1.
6. The method for preparing nano aluminum oxide material as claimed in claim 1, wherein in step 3, the concentration process is as follows: continuously stirring and evaporating at the temperature of 90-95 ℃.
7. The method for preparing nano aluminum oxide material as claimed in claim 1, wherein in step 3, the nitric acid solution is added dropwise until the pH of the reaction system reaches 3.5-4.0, and the time of the reflux aging treatment is 12-18 h.
8. The method for preparing nano aluminum oxide material as claimed in claim 1, wherein in step 4, the method for preparing the niobium silicide nitride nano microspheres comprises:
s1, weighing nanoscale niobium silicide powder, dispersing the nanoscale niobium silicide powder into deionized water, adding a silane coupling agent, stirring at room temperature for 2-5 hours, filtering, and drying to obtain surface-activated niobium silicide powder;
s2, dispersing the surface-activated niobium silicide powder into ammonia water with the mass fraction of 10%, adding resorcinol, carrying out ultrasonic homogenization, dropwise adding a formaldehyde aqueous solution with the mass fraction of 35%, carrying out continuous stirring treatment for 18-24 h at room temperature, filtering, collecting precipitate, and drying to obtain resorcinol formaldehyde polymer/niobium silicide nano-microspheres;
s3, placing the resorcinol formaldehyde polymer/niobium silicide nano-microspheres into a reaction furnace, heating to 400-500 ℃, and treating for 2-4 hours under the air condition to obtain porous carbon-coated niobium silicide composite microspheres;
s4, cooling the reaction furnace to 120-180 ℃, carrying out heat preservation treatment for 1-2 hours, introducing nitrogen to replace air, pressurizing to 10-15 MPa, heating to 280-330 ℃, carrying out heat preservation treatment for 2-4 hours, cooling to normal pressure and normal temperature, and crushing to obtain the niobium silicide nitride nano-microspheres.
9. A product of nano aluminum oxide material, which is characterized in that the product is prepared by the preparation method of nano aluminum oxide material as claimed in claim 1.
10. The application of the nano aluminum oxide material is characterized in that the product prepared by the preparation method of the nano aluminum oxide material in claim 1 is applied to the manufacture of mechanical equipment or transportation pipelines.
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| CN116120895A (en) * | 2022-12-28 | 2023-05-16 | 河南创研新材料科技有限公司 | Preparation method of alumina-diamond composite microsphere powder |
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