CN115321960A - Alumina ceramic and preparation method and application thereof - Google Patents
Alumina ceramic and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses an alumina ceramic and a preparation method and application thereof, relating to the technical field of alumina ceramics. The invention provides a preparation method of alumina ceramic, which comprises the following steps: preparing an alumina ceramic biscuit; (2) Transferring the alumina ceramic biscuit obtained in the step (1) into a microwave hot isostatic pressing sintering furnace for sintering, and cooling to obtain the alumina ceramic; the sintering frequency of the microwave hot isostatic pressing sintering furnace is 2450 +/-50 MHz. The invention provides a preparation method of alumina ceramic, which prepares the alumina ceramic by using a microwave hot isostatic pressing sintering furnace. The invention utilizes the special wave band of the microwave to couple with the basic fine structure of the material to generate heat, the dielectric loss of the material in an electromagnetic field enables the whole material to be heated to the sintering temperature, certain external pressure is provided by inert gas in the sintering process to enable ceramic powder particles to move and fill pores, and therefore, the densification of the ceramic material is realized.
Description
Technical Field
The invention relates to the technical field of alumina ceramics, in particular to alumina ceramics and a preparation method and application thereof.
Background
The alumina ceramic has the excellent properties of small dielectric loss under high frequency, large specific volume resistance, high insulation resistance, high mechanical strength, high hardness, small thermal expansion coefficient, wear resistance, corrosion resistance, thermal shock resistance and the like. Meanwhile, the alumina has wide sources and low price, so the alumina has important application in the fields of machinery, chemical engineering, petroleum refining, pressure sensing, optics, vacuum electronics, biomedicine and the like.
The 99 alumina ceramic means that the content of alumina is 99%. The higher purity of 99 alumina results in a ceramic that is sintered for a long time at least 1750 c to achieve densification. However, the long-time sintering at high temperature can coarsen the crystal grains of the ceramic, generate defects among the crystal grains, and cause difficulty in controlling the porosity, thereby finally causing poor comprehensive performance of the ceramic and large energy consumption. Therefore, in order to lower the sintering temperature of 99 alumina ceramics, a Ca-Mg-Si sintering aid system is generally adopted, but impurity phases such as magnesia-alumina spinel and anorthite exist in the sintered ceramic materials. The difference between the thermal expansion coefficients of alumina and the impurity phases can cause cracking of the material when heated, thereby adversely affecting its strength.
Alumina is an electrically insulating material whose resistivity increases with increasing purity. Therefore, in order to obtain alumina ceramics with high insulation, high-purity alumina powder is required, and impurities introduced in the preparation process of the alumina ceramics are prevented and avoided. The dry pressing molding has the advantages of simple process and high product purity. However, only one side or the upper and lower sides can be pressed during press forming, so that the whole blank body cannot be uniformly pressed, the density of the alumina biscuit is low, and high density cannot be ensured. Therefore, in view of the problems of the prior art, it is important to develop a sintering process capable of preparing a high-purity, high-density 99 alumina ceramic by dry press molding.
Disclosure of Invention
Based on the above, the invention aims to overcome the defects of the prior art and provide the alumina ceramic and the preparation method and application thereof. The invention provides a preparation method of alumina ceramic, which prepares the alumina ceramic by using a microwave hot isostatic pressing sintering furnace. The microwave is coupled with the basic fine structure of the material to generate heat, the dielectric loss of the material in an electromagnetic field enables the material to be integrally heated to the sintering temperature, certain external pressure is provided by inert gas in the sintering process to promote ceramic powder particles to move and fill pores, and therefore densification of the ceramic material is achieved. The invention solves the technical problem of low strength caused by long-time heat preservation at higher temperature of the alumina of the Ca-Mg-Si sintering aid system by microwave isostatic pressing sintering.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of alumina ceramics comprises the following steps:
(1) Preparing an alumina ceramic biscuit;
(2) Transferring the alumina ceramic biscuit obtained in the step (1) into a microwave hot isostatic pressing sintering furnace for sintering, and cooling to obtain the alumina ceramic; wherein the sintering frequency of the microwave hot isostatic pressing sintering furnace is 2450 +/-50 MHz.
The invention provides a preparation method of alumina ceramic, which utilizes the special wave band of microwave to couple with the basic fine structure of the material to generate heat, the dielectric loss of the material in an electromagnetic field enables the whole material to be heated to the sintering temperature, certain external pressure is provided by inert gas in the sintering process to promote the movement of ceramic powder particles and fill pores, thereby realizing the densification of the ceramic material. The alumina ceramic biscuit can uniformly absorb microwave energy inside and outside in a microwave field to achieve the purpose of sintering, the microwave energy is absorbed by the material integrally, so that no temperature gradient exists in a sintered sample, uniform heating is realized, and thermal stress is not formed in the sample or the sample is not cracked.
Preferably, in the step (2), the sintering process of the microwave hot isostatic pressing sintering furnace comprises the following steps:
s1, heating rate K during sintering 1 Heating to T at a temperature of 10-15 deg.C/min 1 400-600 ℃ of heat preservation t 1 5-10min；
S2, heating rate K in sintering 2 Heating to T at 30-60 deg.C/min 2 1580-1650 deg.C, keeping the temperature t 1 10-30min。
Preferably, in S1, the pressure at the time of sinteringForce P 1 Is 0.1-5MPa; s2, pressure P at the time of sintering 2 Is 5-10MPa; in the microwave hot isostatic pressing sintering furnace, the hot isostatic pressing atmosphere is inert gas.
After the temperature of the aluminum oxide material is higher than the critical temperature, the loss factor is rapidly increased, so that the temperature is rapidly increased, the sintering temperature is reduced, the sintering speed is increased, and the sintering time is shortened. And hot isostatic pressing is applied in the sintering process to promote the further densification of the ceramic powder, the sintering temperature is lower than the normal pressure sintering temperature of 1750 ℃, the grain growth speed is slow, and the sintered ceramic material has relatively low porosity and small grain size. The sintering temperature is lower, the grain growth is inhibited to a certain extent, the densification degree of the obtained sintered body is improved, and the material has higher mechanical property.
Preferably, in S2, the temperature increase rate K during sintering 2 Is 40-50 deg.C/min.
After a great deal of experimental research, the inventor finds that the temperature rise rate K during sintering 2 The porosity of the prepared alumina ceramic is lower and the mechanical property is higher when the temperature is 40-50 ℃/min. When K is 2 When the temperature rise rate is too high, the reaction does not completely occur in the alumina, and the sintering process is finished, so that pores are formed in the alumina material; and K 2 When the heating rate is too slow, the sintering time of the blank is prolonged, more sufficient energy is available among particles to fully carry out the reaction, the prepared material is very compact, the porosity is low, but more energy is consumed when the heating rate is too slow.
Preferably, in the step (1), the preparation of the alumina ceramic biscuit comprises the following steps:
(a) Uniformly mixing the polyvinyl alcohol solution and the alumina powder to obtain mixed slurry;
(b) And (b) carrying out ball milling, granulation, compression molding and drying on the mixed slurry obtained in the step (a) to obtain the alumina ceramic biscuit.
Preferably, in the step (a), the mass ratio of the polyvinyl alcohol solution to the alumina powder is polyvinyl alcohol solution: alumina powder =1: (3-5); the polyvinyl alcohol solution is prepared from polyvinyl alcohol and deionized water, and the mass ratio of the polyvinyl alcohol to the deionized water is polyvinyl alcohol: deionized water =95:5.
preferably, in the step (b), the ball milling time is 1-4h, the ball milling rotation speed is 200-400r/min, the ball milling inner lining material and the ball milling outer lining material are polyethylene, and the material of the milling ball is alumina.
Preferably, in the step (b), the granulation is performed by a spray granulation method, the particle size D50 obtained by granulation is 200-300 μm, the pressure of compression molding is 90-200MPa, the drying temperature is 85-110 ℃, and the drying time is 8-12h.
In addition, the invention provides the alumina ceramic prepared by the preparation method of the alumina ceramic.
Further, the invention provides application of the alumina ceramic in substrates, ceramic bearings, ceramic sealing elements and the like.
Compared with the prior art, the invention has the beneficial effects that: (1) The invention provides a preparation method of alumina ceramic, which utilizes the special wave band of microwave to couple with the basic fine structure of material to generate heat, the dielectric loss of the material in an electromagnetic field enables the material to be integrally heated to a sintering temperature, certain external pressure is provided by inert gas in the sintering process to promote the movement of ceramic powder particles and fill pores, thereby realizing the densification of the ceramic material. (2) The alumina sintered sample can uniformly absorb microwave energy inside and outside in a microwave field to achieve the purpose of sintering, and the material can uniformly absorb the microwave energy so that no temperature gradient exists in the sintered sample and uniform heating is achieved without forming thermal stress in the sample or causing the sample to crack. (3) After the temperature of the aluminum oxide material is higher than the critical temperature, the loss factor is rapidly increased, so that the temperature is rapidly increased, the sintering temperature is reduced, the sintering speed is increased, and the sintering time is shortened. (4) And hot isostatic pressing is applied in the sintering process to promote the further densification of the ceramic powder, the sintering temperature is lower than the normal pressure sintering temperature of 1750 ℃, the grain growth speed is slow, and the sintered ceramic material has relatively low porosity and small grain size. (5) The sintering temperature is lower, the grain growth is inhibited to a certain extent, the densification degree of the obtained sintered body is improved, and the material has higher mechanical property.
Detailed Description
To better illustrate the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to specific examples. In the examples, the experimental methods used were all conventional methods unless otherwise specified, and the materials, reagents and the like used were commercially available without otherwise specified.
Examples 1 to 11 and comparative examples 1 to 10
The specific parameters of the preparation processes of the alumina ceramics in the examples and the comparative examples are shown in table 1: a preparation method of alumina ceramics comprises the following steps:
(1) Preparing an alumina ceramic biscuit; uniformly mixing the polyvinyl alcohol solution and the alumina powder to obtain mixed slurry; ball-milling, granulating, press-forming and drying the mixed slurry to obtain the alumina ceramic biscuit; the ball milling time is 2 hours, the ball milling rotating speed is 300r/min, the ball milling inner lining material and the ball milling outer lining material are polyethylene, and the material of the grinding balls is alumina; granulating by spray granulation method, wherein the particle diameter D50 of the granulated particles is 200 μm, the pressure of compression molding is 150MPa, the drying temperature is 100 deg.C, and the drying time is 10h;
(2) Transferring the alumina ceramic biscuit obtained in the step (1) into a microwave hot isostatic pressing sintering furnace for sintering, and cooling to obtain the alumina ceramic; wherein, the sintering frequency of the microwave hot isostatic pressing sintering furnace is 2450 +/-50 MHz, and the sintering process of the microwave hot isostatic pressing sintering furnace comprises the following steps:
s1, heating rate K during sintering 1 Heating to T at a temperature of 10-15 deg.C/min 1 400-600 ℃ of heat preservation t 1 5-10min, pressure P during sintering 1 Is 0.1-5MPa;
s2, heating rate K in sintering 2 Heating to T at 30-60 deg.C/min 2 1580-1650 deg.C, keeping the temperature t 1 10-30min, pressure P during sintering 2 Is 5-10MPa.
Comparative example 8 sintering was carried out in a microwave sintering furnace at normal pressure without isostatic pressing; comparative example 9 was sintered in a microwave hot isostatic pressing sintering furnace using a microwave frequency of 915MHz, and comparative example 10 was sintered in a conventional sintering furnace using isostatic pressing without microwave heating.
TABLE 1
Performance testing
And (4) testing standard:
(1) The test methods for density and porosity were performed according to GB/T25995-2010.
(2) The bending strength adopts a three-point bending test method, and the specific mode is as follows: at ambient temperature, a 24 × 40mm size sample was pressed against the specimen on a 30mm span loading device at a constant loading rate of 1mm/min until the specimen broke.
(3) Grain size: the sample micro-topography was photographed using SEM and the grain size was measured using Nano Measurer software.
And (3) testing results: the results of the performance tests are shown in table 2.
TABLE 2
From the comparison between example 1 and comparative example 9, it is understood that the higher the frequency, the shorter the wavelength, since the microwave frequency is inversely proportional to the wavelength. In comparative example 9, the microwave frequency of 915MHz was used, and the microwave frequency of 915MHz was lower than the frequency of 2450MHz, and the wavelength was relatively long, so that the field intensity of the microwave field was relatively uneven, and some regions of the sample had temperature differences, thereby generating thermal stress. The presence of thermal stress causes microcracking of the sample, which in turn significantly reduces strength.
As can be seen from the comparison of the examples 1, 5-6 and 4-5, when the microwave temperature is higher than 1650 ℃, the interior of the blank is continuously dense, the porosity is reduced, but the crystal grains are synchronously increased, so the abnormal growth of the crystal grains obviously reduces the strength of the material; when the microwave temperature is lower than 1580 ℃, the blank does not reach densification, the number of air holes is large, simultaneously the crystal grain growth is incomplete, and the strength of the aluminum oxide material is also obviously reduced.
As is clear from comparison of examples 1 to 4 and comparative examples 1 to 2, K is 2 The temperature rise rate of (2) is too fast, the reaction does not completely occur in the alumina, and the sintering process is finished, so that the alumina material has air holes inside; and K 2 The heating rate is too slow, the sintering time of the blank is prolonged, more sufficient energy is provided among particles to fully carry out the reaction, the prepared material is very compact, the porosity is low, but more energy is consumed by too slow heating rate.
As is clear from comparison of examples 1, 7 to 8 and 6 to 7, the holding time t of the S2 at the high temperature stage 2 Determining the degree of complete densification of the blank. The heat preservation time is too short, and the internal temperature and the external temperature of the material are different, so that the crystal grains are completely compact, and air holes are remained in the body; if the holding time is too long, the porosity will decrease, but the grain growth will be too large, resulting in a decrease in strength.
The invention mainly controls the sintering of the alumina ceramic at the temperature of 600-1650 ℃, the heat preservation temperature and the heat preservation time influence the mechanical property of the alumina ceramic by influencing the grain size and the porosity of the alumina ceramic, and the strength of the alumina ceramic is changed within the range of 419.39-450.1MPa under the proper temperature rise rate, heat preservation temperature and heat preservation time.
As can be seen from comparison between example 1 and comparative example 8, when sintering was carried out at atmospheric pressure in a microwave sintering furnace without using isostatic pressing, the energy supplied at 1595 ℃ was insufficient to sinter the alumina ceramic, and thus there were substantially no crystal grains, and the porosity was high and the strength was low; as is clear from comparison between example 1 and comparative example 10, when sintering was performed by isostatic pressing without microwave heating, the contact area between solid particles was reduced after the binder decomposition was completed, so that the porosity was high after sintering was completed, and the strength was adversely affected.
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, and 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 to 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 alumina ceramic is characterized by comprising the following steps:
(1) Preparing an alumina ceramic biscuit;
(2) Transferring the alumina ceramic biscuit obtained in the step (1) into a microwave hot isostatic pressing sintering furnace for sintering, and cooling to obtain the alumina ceramic; wherein the sintering frequency of the microwave hot isostatic pressing sintering furnace is 2450 +/-50 MHz.
2. The method for preparing the alumina ceramic according to claim 1, wherein in the step (2), the sintering process of the microwave hot isostatic pressing sintering furnace comprises the following steps:
s1, heating rate K during sintering 1 Heating to T at a temperature of 10-15 deg.C/min 1 Keeping the temperature at 400-600 DEG C 1 5-10min；
S2, heating rate K in sintering 2 Heating to T at 30-60 deg.C/min 2 1580-1650 deg.C, keeping the temperature t 1 10-30min。
3. The method for producing an alumina ceramic according to claim 2, wherein the pressure P at the time of sintering in S1 is 1 Is 0.1-5MPa; s2, pressure P at the time of sintering 2 Is 5-10MPa.
4. The method according to claim 2, wherein in S2, the temperature increase rate K during sintering is set to 2 Is 40-50 deg.C/min.
5. The method for preparing alumina ceramics according to claim 1, wherein in the step (1), the alumina ceramics biscuit is prepared, and the method comprises the following steps:
(a) Uniformly mixing the polyvinyl alcohol solution and the alumina powder to obtain mixed slurry;
(b) And (b) carrying out ball milling, granulation, compression molding and drying on the mixed slurry obtained in the step (a) to obtain the alumina ceramic biscuit.
6. The method for preparing alumina ceramic according to claim 1, wherein in the step (a), the mass ratio of the polyvinyl alcohol solution to the alumina powder is polyvinyl alcohol solution: alumina powder =1: (3-5).
7. The method for preparing the alumina ceramic according to claim 1, wherein in the step (b), the ball milling time is 1-4h, the rotation speed of the ball milling is 200-400r/min, the ball milling lining material is polyethylene, and the material of the milling ball is alumina.
8. The method of preparing alumina ceramic according to claim 1, wherein in the step (b), the granulation is performed by a spray granulation method, the particle size D50 of the granules obtained by the granulation is 200 to 300 μm, the pressure of the press molding is 90 to 200MPa, the temperature of the drying is 85 to 110 ℃, and the time of the drying is 8 to 12 hours.
9. An alumina ceramic produced by the method for producing an alumina ceramic according to any one of claims 1 to 8.
10. Use of the alumina ceramic of claim 9 in substrates, ceramic bearings and ceramic seals.
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| CN116332630A (en) * | 2023-05-24 | 2023-06-27 | 无锡卓瓷科技有限公司 | Preparation method of alumina ceramic for semiconductor equipment |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116332630A (en) * | 2023-05-24 | 2023-06-27 | 无锡卓瓷科技有限公司 | Preparation method of alumina ceramic for semiconductor equipment |
| CN116332630B (en) * | 2023-05-24 | 2023-08-11 | 无锡卓瓷科技有限公司 | Preparation method of alumina ceramic for semiconductor equipment |
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