CN114230322B - Preparation method of aluminum oxide composite ceramic powder - Google Patents
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Abstract
The invention discloses a preparation method of alumina composite ceramic powder, belonging to the technical field of ceramic materials and ceramic composite materials. Firstly, weighing 6.4-10% of sodium bentonite, 12.5-16.5% of calcined kaolin, 9.6-15% of talc, 5-7.5% of cordierite powder and the balance of composite alumina micropowder according to mass percentage; and then mixing and ball-milling the composite alumina micro powder, sodium bentonite, calcined kaolin, talc and water, and then adding cordierite powder, polyvinyl alcohol, silica sol and ammonium polyacrylate and ball-milling again to obtain the alumina composite ceramic powder. The invention keeps the advantages of wear resistance, high temperature resistance and the like of the alumina ceramic and overcomes the defects of thermal shock resistance and strength of the alumina ceramic. The alumina composite ceramic powder can effectively improve the thermal shock resistance and strength of the alumina composite ceramic, and has good application prospect.
Description
Technical Field
The invention belongs to the technical field of ceramic materials and ceramic composite materials, and particularly relates to a preparation method of aluminum oxide composite ceramic powder.
Background
The traditional ceramics are artificial materials creatively synthesized by human beings by comprehensively utilizing rocks, clay minerals and various natural resources and fire, the ceramics are invented by the human beings in the times of the new stoneware about 8000 years ago in the public yuan, the ceramic materials are mostly oxides, nitrides, borides, carbides and the like, and the invention and the progress of the ceramics have great influence on the human life and civilization.
Besides being used in daily life, the ceramic can also be widely applied to a plurality of fields such as scientific technology, industrial and agricultural production and the like as a structural and functional material. Due to the transition from the secondary material to the primary material, there are also more and higher demands on the properties of ceramics.
Alumina ceramics are ceramic materials which take alumina as a main body and contain a small amount of silicon dioxide, and because of good conductivity, wear resistance and high temperature resistance, the alumina ceramics are applied more and more widely in the current society. However, the alumina ceramics still have some disadvantages in practical application, such as poor thermal shock resistance, low strength, etc., thereby limiting the application range thereof.
The composite ceramic is made of two or more materials, different materials are mutually made up for deficiencies, and the composite ceramic can improve the performance limit of a single material, so that the high-performance requirement of a structural material is met. In view of the above, there is a need to develop a high-performance alumina composite ceramic.
Disclosure of Invention
Aiming at the problems of limitation of single material ceramic, poor thermal shock resistance and low strength of the alumina ceramic mentioned in the background technology, the invention aims to provide the preparation method of the alumina composite ceramic powder.
The invention is realized by the following technical scheme:
a preparation method of alumina composite ceramic powder comprises the following steps:
1) Weighing 6.4-10% of sodium bentonite, 12.5-16.5% of calcined kaolin, 9.6-15% of talc, 5-7.5% of cordierite powder and the balance of composite alumina micropowder according to the mass percentage; wherein, the alpha-alumina accounts for 92.5 to 95.5 percent of the total mass, the tungsten carbide accounts for 3.5 to 4.2 percent of the total mass, and the balance is other impurities in the composite alumina micro powder;
2) Mixing and ball-milling the composite alumina micro powder, the sodium bentonite, the calcined kaolin, the talc and water accounting for 80-95% of the total weight of the four for 3-5h, then adding cordierite powder, polyvinyl alcohol, silica sol and ammonium polyacrylate, continuing ball-milling for 6-8.5h under the pressure condition of 3.2-5.0MPa to obtain slurry, and spray-drying the slurry to obtain powder.
Further, the raw materials in the step 1) are respectively as follows by mass percent: 7.2 to 8.4 percent of sodium bentonite, 12.5 to 14.2 percent of calcined kaolin, 12 to 13.5 percent of talc, 6.6 to 7.5 percent of cordierite powder and the balance of composite alumina micro powder.
The ability of the ceramic material to withstand a sudden temperature change without being destroyed is the thermal shock resistance, and the level of the thermal shock resistance is representative of whether the ceramic material has excellent high-temperature performance. The thermal shock resistance of the ceramic material is a comprehensive expression of mechanical property and thermal property, and is also influenced by geometrical factors, environmental media and the like. The mechanical properties related to the thermal shock resistance of the material mainly comprise strength, fracture toughness and elastic modulus.
The alpha-alumina has excellent chemical stability and low specific surface area, and the ceramic diaphragm is not easy to absorb water. According to the invention, a small amount of tungsten carbide powder is compounded with the alpha-alumina micro powder, and the obtained composite micro powder can reduce the influence of thermal stress on the internal structure of the material, so that the thermal shock resistance temperature of the obtained alumina composite ceramic can be further improved.
Further, the particle size range of the composite alumina micro powder in the step 1) is 0.1-30 μm.
Furthermore, the particle size of the composite alumina micro powder is in the range of 0.1-2 μm and accounts for 45% of the total mass, and the particle size is in the range of 18-30 μm and accounts for 40% of the total mass.
Under the condition that the particle size range of the composite alumina micropowder is preferably 0.1-30 mu m, the inventor researches and discovers that when the proportion of micropowder particles at two ends of the particle size range is higher, the thermal shock resistance of the formed composite alumina micropowder to finally prepared alumina composite ceramic is obviously improved; by combining the dispersibility of the process system, the invention further adopts the composite alumina micro powder with the grain diameter of 0.1-2 microns accounting for 45 percent and the grain diameter of 18-30 microns accounting for 40 percent.
Further, in the composite alumina micro powder in the step 1), the alpha-alumina accounts for 92.5-94.0% of the total mass, the tungsten carbide accounts for 4.0-4.2% of the total mass, and the balance is other impurities.
Further, the mass ratio of the cordierite powder, the polyvinyl alcohol, the silica sol and the ammonium polyacrylate in the step 2) is 1 (0.15-0.45) to (0.8-1.6) to (0.03-0.3).
Further, the particle size of the cordierite powder in the step 2) is not more than 0.8 μm.
The method comprises the steps of mixing alumina micro powder and other base materials, carrying out ball milling, then adding cordierite powder, a dispersing agent, an emulsifying agent and a bonding agent under pressure, and carrying out ball milling again. The process method can effectively refine the grain size of the composite ceramic matrix, improve the strength of the alumina composite ceramic and improve the thermal shock resistance of the alumina composite ceramic.
Furthermore, the alumina composite ceramic powder prepared by the method can be prepared into the alumina composite ceramic with good thermal shock resistance and high strength through cold press molding and high-temperature sintering.
Compared with the prior art, the invention has the beneficial effects that:
the invention breaks the performance limitation of the existing single-material ceramic product, retains the advantages of wear resistance, high temperature resistance and the like of the alumina ceramic, and overcomes the defects of thermal shock resistance and strength of the alumina ceramic. The alumina composite ceramic powder prepared by the invention can be prepared into the alumina composite ceramic with good thermal shock resistance and high strength through cold press molding and high-temperature sintering.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are conventional products which are not indicated by manufacturers and are commercially available.
Example 1
1. Weighing 8.4% of sodium bentonite, 12.5% of calcined kaolin, 13.5% of talc, 7.5% of cordierite powder and the balance of composite alumina micro powder (wherein the alpha-alumina accounts for 94.0%, the tungsten carbide accounts for 4.0%, and the balance is other impurities);
2. mixing and ball-milling composite alumina micro powder, sodium bentonite, calcined kaolin and talc with water accounting for 88 percent of the total weight of the composite alumina micro powder, the sodium bentonite, the calcined kaolin and the talc for 4 hours, then adding cordierite powder, polyvinyl alcohol, silica sol and ammonium polyacrylate (the mass ratio is 1.25.
Example 2
1. Weighing 7.2% of sodium bentonite, 12.5% of calcined kaolin, 13.5% of talc, 7.5% of cordierite powder and the balance of composite alumina micro powder (wherein the alpha-alumina accounts for 94.0%, the tungsten carbide accounts for 4.2%, and the balance is other impurities);
2. mixing and ball-milling composite alumina micro powder, sodium bentonite, calcined kaolin and talc with water accounting for 90% of the total weight of the four materials for 4 hours, then adding cordierite powder, polyvinyl alcohol, silica sol and ammonium polyacrylate (mass ratio is 1.25.
Example 3
1. Weighing 6.4% of sodium bentonite, 14.2% of calcined kaolin, 15% of talc, 6.6% of cordierite powder and the balance of composite alumina micro powder (wherein the alpha-alumina accounts for 95.5%, the tungsten carbide accounts for 4.2% and the balance is other impurities);
2. mixing and ball-milling composite alumina micro powder, sodium bentonite, calcined kaolin and talc with water accounting for 88 percent of the total weight of the composite alumina micro powder, the sodium bentonite, the calcined kaolin and the talc for 4 hours, then adding cordierite powder, polyvinyl alcohol, silica sol and ammonium polyacrylate (the mass ratio is 1.25.
Example 4
1. Weighing 10% of sodium bentonite, 16.5% of calcined kaolin, 9.6% of talc, 5% of cordierite powder and the balance of composite alumina micro powder (wherein the alpha-alumina accounts for 92.5%, the tungsten carbide accounts for 4.2% and the balance is other impurities);
2. mixing and ball-milling composite alumina micro powder, sodium bentonite, calcined kaolin and talc with water accounting for 88 percent of the total weight of the composite alumina micro powder, the sodium bentonite, the calcined kaolin and the talc for 4 hours, then adding cordierite powder, polyvinyl alcohol, silica sol and ammonium polyacrylate (the mass ratio is 1.25.
And (3) respectively carrying out cold isostatic pressing on the alumina composite ceramic powder prepared in the embodiments 1-4 to obtain a blank, modifying the surface of the blank, and then transferring the blank into a kiln to sinter for 12 hours at 1650 ℃ to obtain the alumina composite ceramic. The thermal shock resistance, strength and insulation of the obtained alumina composite ceramic were measured, 6 samples were measured for each example, and the results are shown in table 1.
TABLE 1
Comparative example 1
1. Weighing 8.4% of sodium bentonite, 12.5% of calcined kaolin, 13.5% of talc, 7.5% of cordierite powder and the balance of composite alumina micro powder (wherein the alpha-alumina accounts for 94.0% and the balance is other impurities) according to the weight percentage;
2. mixing and ball-milling composite alumina micro powder, sodium bentonite, calcined kaolin and talc with water accounting for 88 percent of the total weight of the composite alumina micro powder, the sodium bentonite, the calcined kaolin and the talc for 4 hours, then adding cordierite powder, polyvinyl alcohol, silica sol and ammonium polyacrylate (the mass ratio is 1.25.
Comparative example 2
1. Weighing 8.4% of sodium bentonite, 12.5% of calcined kaolin, 13.5% of talc, 7.5% of cordierite powder and the balance of composite alumina micro powder (wherein the alpha-alumina accounts for 94.0%, the tungsten carbide accounts for 4.0%, and the balance is other impurities); wherein the particle size range of the composite alumina micro powder is 0.1-30 μm and is evenly distributed in the particle size range.
2. Mixing and ball-milling composite alumina micro powder, sodium bentonite, calcined kaolin and talc with water accounting for 88 percent of the total weight of the composite alumina micro powder, the sodium bentonite, the calcined kaolin and the talc for 4 hours, then adding cordierite powder, polyvinyl alcohol, silica sol and ammonium polyacrylate (the mass ratio is 1.25.
Comparative example 3
1. Weighing 8.4% of sodium bentonite, 12.5% of calcined kaolin, 13.5% of talc, 7.5% of cordierite powder and the balance of composite alumina micro powder (wherein the alpha-alumina accounts for 94.0%, the tungsten carbide accounts for 4.0%, and the balance is other impurities);
2. mixing the composite alumina micro powder, sodium bentonite, calcined kaolin and talc with water accounting for 88 percent of the total weight of the four materials, simultaneously adding cordierite powder, polyvinyl alcohol, silica sol and ammonium polyacrylate (the mass ratio is 1:0.25:1.35: 0.12), mixing and ball-milling for 11.8 hours to obtain slurry, and spray-drying the slurry to obtain powder.
And respectively carrying out cold isostatic pressing on the alumina composite ceramic powder prepared in the comparative examples 1-3 to obtain a blank, modifying the surface of the blank, and then transferring the blank into a kiln to sinter for 12 hours at 1650 ℃ to obtain the alumina composite ceramic. The thermal shock resistance, strength and insulation of the obtained alumina composite ceramic were measured, 6 samples were measured for each comparative example, and the results are shown in table 2.
TABLE 2
As shown in the table 1 and the table 2, the detection data of the comparative example sample show that the thermal shock resistance of the alumina composite ceramic can be well improved by the process method, and the prepared alumina composite ceramic also has good strength and insulativity.
The above-described embodiments are only preferred embodiments of the present invention and are not intended to limit the present invention. Various changes and modifications may be effected therein by one skilled in the art without departing from the spirit and scope of the invention, and any such changes, substitutions, improvements and the like are intended to be included within the scope of the invention.
Claims (5)
1. The preparation method of the alumina composite ceramic powder is characterized by comprising the following steps:
1) Weighing 6.4-10% of sodium bentonite, 12.5-16.5% of calcined kaolin, 9.6-15% of talc, 5-7.5% of cordierite powder and the balance of composite alumina micropowder according to the mass percentage; wherein, the alpha-alumina accounts for 92.5 to 95.5 percent of the total mass, the tungsten carbide accounts for 3.5 to 4.2 percent of the total mass, and the balance is other impurities in the composite alumina micro powder; the particle size range of the composite alumina micro powder is 0.1-30 mu m, the particle size range of 0.1-2 mu m accounts for 45% of the total mass, and the particle size range of 18-30 mu m accounts for 40% of the total mass;
2) Mixing and ball-milling composite alumina micro powder, sodium bentonite, calcined kaolin, talc and water accounting for 80-95% of the total weight of the four materials to obtain 3-5h, adding cordierite powder, polyvinyl alcohol, silica sol and ammonium polyacrylate, continuously ball-milling the mixture to obtain 6-8.5h under the pressure condition of 3.2-5.0MPa to obtain slurry, and carrying out spray drying on the slurry to obtain powder; wherein the mass ratio of the cordierite powder to the polyvinyl alcohol to the silica sol to the ammonium polyacrylate is 1 (0.15-0.45) to 0.8-1.6 to 0.03-0.3).
2. The method for preparing the alumina composite ceramic powder according to claim 1, wherein the raw materials in the step 1) are respectively as follows by mass percent: 7.2 to 8.4 percent of sodium bentonite, 12.5 to 14.2 percent of calcined kaolin, 12 to 13.5 percent of talc, 6.6 to 7.5 percent of cordierite powder and the balance of composite alumina micro powder.
3. The method for preparing the alumina composite ceramic powder according to claim 1, wherein the alpha-alumina in the composite alumina micropowder in the step 1) accounts for 92.5-94.0% of the total mass, the tungsten carbide accounts for 4.0-4.2% of the total mass, and the balance is other impurities.
4. The method for preparing alumina composite ceramic powder according to claim 1, wherein the particle size of the cordierite powder in step 2) is not more than 0.8 μm.
5. The alumina composite ceramic powder prepared by the method of any one of claims 1 to 4, which is subjected to cold press molding and high-temperature sintering to prepare the alumina composite ceramic with good thermal shock resistance and high strength.
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