CN111732421A - Preparation method of alumina ceramic composite powder - Google Patents
Preparation method of alumina ceramic composite powder Download PDFInfo
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- CN111732421A CN111732421A CN202010452235.XA CN202010452235A CN111732421A CN 111732421 A CN111732421 A CN 111732421A CN 202010452235 A CN202010452235 A CN 202010452235A CN 111732421 A CN111732421 A CN 111732421A
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Abstract
The invention discloses a preparation method of alumina ceramic composite powder, which comprises the following steps of 1), alumina slurry preparation: 100-200 parts of alumina powder, 5-20 parts of additive powder, 3-13 parts of dispersant and 150-300 parts of ultrapure water; step 2), coarse grinding: grinding the prepared alumina slurry by using a coarse grinding machine to obtain coarse ground slurry; step 3), fine grinding: sieving the coarse ground slurry, and grinding the coarse ground slurry in a fine grinding machine to obtain fine ground slurry; step 4), spray granulation: carrying out spray granulation on the fine grinding slurry by using a spray drying tower to obtain aluminum oxide composite powder; step 5), compression molding: pressing and forming the alumina composite powder by a flat plate tablet press to obtain an alumina ceramic prefabricated part; step 6), cold isostatic pressing: carrying out cold isostatic pressing on the alumina ceramic prefabricated part to obtain an alumina ceramic blank; step 7), sintering: sintering the alumina ceramic blank in a resistance furnace to obtain the alumina ceramic finished product. The alumina ceramic composite powder obtained by the invention is uniformly mixed, the process is simple, and the sintered ceramic has good mechanical properties.
Description
Technical Field
The invention relates to the field of ceramic powder, in particular to a preparation method of alumina ceramic composite powder.
Background
The alumina ceramic has the advantages of high hardness, high temperature resistance, wear resistance, electric insulation, oxidation resistance, rich raw material, low price and the like, and is the most widely applied fine ceramic at the earliest. The single alumina powder has high sintering temperature, and grains are easy to grow abnormally in the middle and later sintering periods, so that the structure is not uniform, even the inside is wrapped with closed air holes, the bonding strength of a crystal boundary is reduced, and the performance of the material is deteriorated. Therefore, it is necessary to introduce other powders as additives to form liquid phase or solid solution with alumina to overcome the above disadvantages.
The traditional alumina composite powder is prepared by adding different additives into treated alumina powder with better particle size distribution and mixing by adopting dry-method or wet-method ball milling. The particle size and particle size distribution of alumina are ground to appropriate size, and as disclosed in patent application No. 201710951141.5, a method for preparing superfine alumina powder includes the following steps: (1) coarsely grinding the alumina slurry in the presence of a first dispersant; (2) filtering the coarsely ground alumina slurry; (3) finely grinding the filtered alumina slurry in the presence of a second dispersant; (4) drying and crushing the finely ground alumina slurry, wherein the first dispersing agent is ammonium polyacrylate, and the second dispersing agent is a mixture of polyacrylic acid and ammonium polyacrylate, the mass ratio of the polyacrylic acid to the ammonium polyacrylate is 2: 1-1: 2, and in the step (1), the alumina slurry is coarsely ground by zirconia beads with the diameter of 4.0-7.0 mm for 2-4 hours; in the step (3), the alumina slurry is finely ground with zirconia beads having a diameter of 0.8mm to 2mm for 1 to 3 hours. Finally, the obtained powder is dried and crushed.
The required composite powder is prepared by mixing the treated alumina powder with additives and carrying out secondary grinding and mixing, but because the particle sizes of different powders are different greatly, the dispersing capacities are also different greatly, the powder obtained by the mixing mode has poor uniformity, and particularly for larger agglomerated particles, local stress is caused by the states of local eutectic melting and the like during ceramic sintering, so that the defects of the ceramic are generated, the mechanical properties and the like are reduced, and the yield is low. Therefore, a better preparation method of the alumina ceramic composite powder is urgently needed.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide an improved preparation method of alumina ceramic composite powder, which is characterized in that different additives are mixed while the granularity of alumina powder is optimized, so that the prepared alumina ceramic composite powder has uniform particle size distribution and simple process, no additional mixing step is needed, and the sintered ceramic has good mechanical property.
The technical scheme adopted by the invention for solving the technical problem is as follows: a preparation method of alumina ceramic composite powder comprises the following steps:
step 1), preparing alumina slurry: mixing the following components in parts by weight together to prepare alumina slurry, wherein the alumina slurry comprises 100-200 parts of alumina powder, 5-20 parts of additive powder, 3-13 parts of dispersing agent and 150-300 parts of ultrapure water;
step 2), coarse grinding: grinding the prepared alumina slurry by using a coarse grinding machine to obtain coarse ground slurry;
step 3), fine grinding: sieving the coarse ground slurry, and grinding the coarse ground slurry in a fine grinding machine to obtain fine ground slurry;
step 4), spray granulation: carrying out spray granulation on the fine grinding slurry by using a spray drying tower to obtain aluminum oxide composite powder;
step 5), compression molding: pressing and forming the alumina composite powder by a flat plate tablet press to obtain an alumina ceramic prefabricated part;
step 6), cold isostatic pressing: carrying out cold isostatic pressing on the alumina ceramic prefabricated part to obtain an alumina ceramic blank;
step 7), sintering: sintering the alumina ceramic blank in a resistance furnace to obtain the alumina ceramic finished product.
Further, in the step 1), the purity of the alumina powder is 99-99.99%.
Further, in the step 1), the additive powder is SiO2、MgO、CaO、SrO、BaO、Fe2O3、TiO2And MnO or a combination of more than one of them.
Further, in the step 1), the dispersing agent is any one or a combination of several of sodium hexametaphosphate, polyacrylic acid, ammonium polyacrylate, citric acid, polyvinyl alcohol and sodium polyacrylate.
Further, in the step 2), the rough grinding speed is 120-180r/min, and the rough grinding time is 1-5 h.
Further, in the step 3), the fine grinding speed is 500-1000r/min, and the fine grinding time is 0.5-3 h.
Further, in the step 5), the pressure in the compression molding process is 20-30MPa, and the time is 6-10 min.
Further, in the step 6), the pressure of the cold isostatic pressing is 100-200MPa, and the time is 0.1-2 h.
Further, in the step 7), the temperature in the sintering process is 1400-1650 ℃, and the sintering time is 3-8 h.
The invention has the beneficial effects that: compared with the traditional preparation method of the alumina ceramic composite powder, the preparation method of the alumina ceramic composite powder provided by the invention has the advantages that the particle size of the alumina powder is optimized, and different additives are mixed at the same time, so that the prepared alumina ceramic composite powder has uniform particle size distribution, the process is simple, no additional mixing step is required, and the sintered ceramic has good mechanical property.
Drawings
FIG. 1: comparative example 1 scanning electron micrographs of the alumina pellets obtained by spray granulation.
FIG. 2: comparative example 2 scanning electron micrograph of the alumina composite powder obtained by spray granulation.
FIG. 3: example 1 scanning electron micrographs of the alumina composite powder obtained by spray granulation.
Detailed Description
The invention is further illustrated by the following specific examples. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention.
Comparative example 1:
preparing alumina slurry: alumina powder: 100 parts, adding MgO powder: 0 part, dispersant: 3 parts of ultrapure water: 160 parts.
Coarse grinding: and grinding the prepared alumina slurry by using a coarse grinding machine to obtain coarse ground slurry. The rough grinding speed is 120r/min, and the rough grinding time is 1 h.
Fine grinding: and sieving the coarse ground slurry, and grinding the coarse ground slurry in a fine grinding machine to obtain fine ground slurry. The fine grinding speed is 1000r/min, and the fine grinding time is 2 h.
Spray granulation: and carrying out spray granulation on the fine ground slurry by using a spray drying tower to obtain the alumina granules. The scanning electron microscope image of the obtained alumina granules is shown in figure 1, and the granules are relatively uniform and have no obvious large granules.
And (3) pressing and forming: and pressing and forming the alumina granules by a flat plate tablet press to obtain the alumina ceramic prefabricated part. The pressing pressure is 20MPa, and the time is 6 min.
Cold isostatic pressing: and (3) carrying out cold isostatic pressing on the alumina ceramic prefabricated member to obtain an alumina ceramic blank. The pressure of the cold isostatic pressing is 100MPa, and the time is 1 h.
And (3) sintering: sintering the alumina ceramic blank in a resistance furnace to obtain the alumina ceramic finished product. The temperature of the sintering process is 1600 ℃, and the sintering time is 5 h.
The ceramic product obtained was tested and the data are shown in table 1.
Comparative example 2:
preparing alumina slurry: comparative example 1 spray granulation of the obtained alumina pellets: 100 parts, adding MgO powder: 3 parts, dispersant: 3 parts of ultrapure water: 160 parts.
Fine grinding: and (3) putting the prepared alumina slurry into a fine grinding machine to be ground to obtain fine ground slurry. The fine grinding speed is 1000r/min, and the fine grinding time is 2 h.
Spray granulation: and (4) carrying out spray granulation on the fine ground slurry by using a spray drying tower to obtain the aluminum oxide composite powder. The scanning electron micrograph of the obtained alumina composite powder is shown in fig. 2, and the particles are not uniformly mixed and have obvious large particles.
And (3) pressing and forming: and pressing and forming the alumina composite powder by a flat plate tablet press to obtain the alumina ceramic prefabricated part. The pressing pressure is 20MPa, and the time is 6 min.
Cold isostatic pressing: and (3) carrying out cold isostatic pressing on the alumina ceramic prefabricated member to obtain an alumina ceramic blank. The pressure of the cold isostatic pressing is 100MPa, and the time is 1 h.
And (3) sintering: sintering the alumina ceramic blank in a resistance furnace to obtain the alumina ceramic finished product. The temperature of the sintering process is 1600 ℃, and the sintering time is 5 h.
The ceramic product obtained was tested and the data are shown in table 1.
Comparative example 3:
coarse grinding: the alumina pellets obtained in comparative example 1 were spray granulated: 100 parts, adding MgO powder: 3 parts, dispersant: 0 part of ultrapure water: 0 portion, adding into a coarse grinding machine for grinding. The rough grinding speed is 120r/min, and the rough grinding time is 3 h.
And (3) pressing and forming: and pressing and forming the aluminum oxide composite powder obtained by coarse grinding by a flat-plate tablet press to obtain the aluminum oxide ceramic prefabricated part. The pressing pressure is 20MPa, and the time is 6 min.
Cold isostatic pressing: and (3) carrying out cold isostatic pressing on the alumina ceramic prefabricated member to obtain an alumina ceramic blank. The pressure of the cold isostatic pressing is 100MPa, and the time is 1 h.
And (3) sintering: sintering the alumina ceramic blank in a resistance furnace to obtain the alumina ceramic finished product. The temperature of the sintering process is 1600 ℃, and the sintering time is 5 h.
The ceramic product obtained was tested and the data are shown in table 1.
Example 1:
preparing alumina slurry: alumina powder: 100 parts, adding MgO powder: 3 parts, dispersant: 3 parts of ultrapure water: 160 parts.
Coarse grinding: and grinding the prepared alumina slurry by using a coarse grinding machine to obtain coarse ground slurry. The rough grinding speed is 120r/min, and the rough grinding time is 1 h.
Fine grinding: and sieving the coarse ground slurry, and grinding the coarse ground slurry in a fine grinding machine to obtain fine ground slurry. The fine grinding speed is 1000r/min, and the fine grinding time is 2 h.
Spray granulation: and (4) carrying out spray granulation on the fine ground slurry by using a spray drying tower to obtain the aluminum oxide composite powder. The scanning electron microscope image of the obtained aluminum oxide composite powder is shown in fig. 3, the particles are uniformly mixed, no obvious large particles exist, and the appearance of the particles is similar to that of the particles shown in fig. 1.
And (3) pressing and forming: and pressing and forming the alumina composite powder by a flat plate tablet press to obtain the alumina ceramic prefabricated part. The pressing pressure is 20MPa, and the time is 6 min.
Cold isostatic pressing: and (3) carrying out cold isostatic pressing on the alumina ceramic prefabricated member to obtain an alumina ceramic blank. The pressure of the cold isostatic pressing is 100MPa, and the time is 1 h.
And (3) sintering: sintering the alumina ceramic blank in a resistance furnace to obtain the alumina ceramic finished product. The temperature of the sintering process is 1600 ℃, and the sintering time is 5 h.
The ceramic product obtained was tested and the data are shown in table 1.
Example 2:
preparing alumina slurry: alumina powder: 100 parts, adding MgO powder: 5 parts, dispersant: 3 parts of ultrapure water: 160 parts.
Coarse grinding: and grinding the prepared alumina slurry by using a coarse grinding machine to obtain coarse ground slurry. The rough grinding speed is 120r/min, and the rough grinding time is 1 h.
Fine grinding: and sieving the coarse ground slurry, and grinding the coarse ground slurry in a fine grinding machine to obtain fine ground slurry. The fine grinding speed is 1000r/min, and the fine grinding time is 2 h.
Spray granulation: and (4) carrying out spray granulation on the fine ground slurry by using a spray drying tower to obtain the aluminum oxide composite powder.
And (3) pressing and forming: and pressing and forming the alumina composite powder by a flat plate tablet press to obtain the alumina ceramic prefabricated part. The pressing pressure is 20MPa, and the time is 6 min.
Cold isostatic pressing: and (3) carrying out cold isostatic pressing on the alumina ceramic prefabricated member to obtain an alumina ceramic blank. The pressure of the cold isostatic pressing is 100MPa, and the time is 1 h.
And (3) sintering: sintering the alumina ceramic blank in a resistance furnace to obtain the alumina ceramic finished product. The temperature of the sintering process is 1600 ℃, and the sintering time is 5 h.
The ceramic product obtained was tested and the data are shown in table 1.
Example 3:
preparing alumina slurry: alumina powder: 100 parts, adding MgO powder: 7 parts, dispersant: 3 parts of ultrapure water: 160 parts.
Coarse grinding: and grinding the prepared alumina slurry by using a coarse grinding machine to obtain coarse ground slurry. The rough grinding speed is 120r/min, and the rough grinding time is 1 h.
Fine grinding: and sieving the coarse ground slurry, and grinding the coarse ground slurry in a fine grinding machine to obtain fine ground slurry. The fine grinding speed is 1000r/min, and the fine grinding time is 2 h.
Spray granulation: and (4) carrying out spray granulation on the fine ground slurry by using a spray drying tower to obtain the aluminum oxide composite powder.
And (3) pressing and forming: and pressing and forming the alumina composite powder by a flat plate tablet press to obtain the alumina ceramic prefabricated part. The pressing pressure is 20MPa, and the time is 6 min.
Cold isostatic pressing: and (3) carrying out cold isostatic pressing on the alumina ceramic prefabricated member to obtain an alumina ceramic blank. The pressure of the cold isostatic pressing is 100MPa, and the time is 1 h.
And (3) sintering: sintering the alumina ceramic blank in a resistance furnace to obtain the alumina ceramic finished product. The temperature of the sintering process is 1600 ℃, and the sintering time is 5 h.
The ceramic product obtained was tested and the data are shown in table 1.
The results of the tests on the finished ceramic products of the above comparative and examples are given in table 1 below:
as can be seen from the above table 1 and the following figures 1, 2 and 3, the alumina ceramic composite powder prepared by the invention has the advantages of uniform mixing, simple process and better mechanical property of sintered ceramic.
The above embodiments are only for illustrating the invention and are not to be construed as limiting the invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention, therefore, all equivalent technical solutions also belong to the scope of the invention, and the scope of the invention is defined by the claims.
Claims (9)
1. A preparation method of alumina ceramic composite powder is characterized by comprising the following steps: the preparation method comprises the following steps:
step 1), preparing alumina slurry: mixing the following components in parts by weight together to prepare alumina slurry, wherein the alumina slurry comprises 100-200 parts of alumina powder, 5-20 parts of additive powder, 3-13 parts of dispersing agent and 150-300 parts of ultrapure water;
step 2), coarse grinding: grinding the prepared alumina slurry by using a coarse grinding machine to obtain coarse ground slurry;
step 3), fine grinding: sieving the coarse ground slurry, and grinding the coarse ground slurry in a fine grinding machine to obtain fine ground slurry;
step 4), spray granulation: carrying out spray granulation on the fine grinding slurry by using a spray drying tower to obtain aluminum oxide composite powder;
step 5), compression molding: pressing and forming the alumina composite powder by a flat plate tablet press to obtain an alumina ceramic prefabricated part;
step 6), cold isostatic pressing: carrying out cold isostatic pressing on the alumina ceramic prefabricated part to obtain an alumina ceramic blank;
step 7), sintering: sintering the alumina ceramic blank in a resistance furnace to obtain the alumina ceramic finished product.
2. The method for preparing the alumina ceramic composite powder according to claim 1, wherein the method comprises the following steps: in the step 1), the purity of the alumina powder is 99-99.99%.
3. The method for preparing the alumina ceramic composite powder according to claim 1, wherein the method comprises the following steps: in the step 1), the additive powder is SiO2、MgO、CaO、SrO、BaO、Fe2O3、TiO2And MnO or a combination of more than one of them.
4. The method for preparing the alumina ceramic composite powder according to claim 1, wherein the method comprises the following steps: in the step 1), the dispersing agent is any one or a combination of several of sodium hexametaphosphate, polyacrylic acid, ammonium polyacrylate, citric acid, polyvinyl alcohol and sodium polyacrylate.
5. The method for preparing the alumina ceramic composite powder according to claim 1, wherein the method comprises the following steps: in the step 2), the coarse grinding speed is 120-180r/min, and the coarse grinding time is 1-5 h.
6. The method for preparing the alumina ceramic composite powder according to claim 1, wherein the method comprises the following steps: in the step 3), the fine grinding speed is 500-1000r/min, and the fine grinding time is 0.5-3 h.
7. The method for preparing the alumina ceramic composite powder according to claim 1, wherein the method comprises the following steps: in the step 5), the pressure in the compression molding process is 20-30MPa, and the time is 6-10 min.
8. The method for preparing the alumina ceramic composite powder according to claim 1, wherein the method comprises the following steps: in the step 6), the pressure of the cold isostatic pressing is 100-200MPa, and the time is 0.1-2 h.
9. The method for preparing the alumina ceramic composite powder according to claim 1, wherein the method comprises the following steps: in the step 7), the temperature in the sintering process is 1400-1650 ℃, and the sintering time is 3-8 h.
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| CN114702307A (en) * | 2022-01-14 | 2022-07-05 | 洛阳索莱特材料科技有限公司 | Preparation method of compact alumina ceramic product |
| CN115159965A (en) * | 2022-08-03 | 2022-10-11 | 陕西宝光陶瓷科技有限公司 | Method for improving strength of cold isostatic pressing blank |
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