CN115321960B - Alumina ceramic and preparation method and application thereof - Google Patents
Alumina ceramic and preparation method and application thereof Download PDFInfo
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- CN115321960B CN115321960B CN202211011355.1A CN202211011355A CN115321960B CN 115321960 B CN115321960 B CN 115321960B CN 202211011355 A CN202211011355 A CN 202211011355A CN 115321960 B CN115321960 B CN 115321960B
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Abstract
The invention discloses alumina ceramic, a preparation method and application thereof, and relates to the technical field of alumina ceramic. The invention provides a preparation method of alumina ceramic, which 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; 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 a microwave hot isostatic pressing sintering furnace to prepare the alumina ceramic. The invention utilizes the special wave band of the microwave to couple with the basic microstructure of the material to generate heat, the dielectric loss of the material in the electromagnetic field causes the material to be integrally heated to the sintering temperature, and the inert gas provides certain external pressure in the sintering process to cause the ceramic powder particles to move and fill the pores, thereby realizing the densification of the ceramic material.
Description
Technical Field
The invention relates to the technical field of alumina ceramics, in particular to an alumina ceramic, a preparation method and application thereof.
Background
The alumina ceramic has the advantages of small dielectric loss at high frequency, large specific volume resistance, high insulation resistance, high mechanical strength, large 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 that the alumina has important application in the fields of machinery, chemical industry, 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 densification of the ceramic by sintering at least at 1750 ℃ for a long period of time. However, sintering at high temperature for a long time causes coarsening of crystal grains of the ceramic, defects are generated among the crystal grains, the porosity is difficult to control, and finally the ceramic has poor comprehensive performance and high energy consumption. Therefore, in order to reduce the sintering temperature of 99 alumina ceramics, a common way is to introduce a Ca-Mg-Si sintering aid system, however, impurity phases such as magnesia-alumina spinel and anorthite exist in the sintered ceramic material. The difference between the coefficients of thermal expansion of the 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, it is necessary to use high purity alumina powder while preventing and avoiding the introduction of impurities during the preparation of alumina ceramics. The dry press molding has the advantages of simple process and high product purity. However, the pressing molding can only be carried out on one side or the upper side and the lower side, so that the whole blank body cannot be subjected to uniform pressure, the density of the alumina biscuit is low, and the high density cannot be ensured. Therefore, it is important to develop a sintering process capable of preparing high purity, high density 99 alumina ceramics by dry press forming, in view of the problems in the prior art.
Disclosure of Invention
Based on this, the present invention aims to overcome the above-mentioned shortcomings of the prior art and provide an alumina ceramic, and a preparation method and application thereof. The invention provides a preparation method of alumina ceramic, which utilizes a microwave hot isostatic pressing sintering furnace to prepare the alumina ceramic. The invention utilizes the special wave band of the microwave to couple with the basic microstructure of the material to generate heat, the dielectric loss of the material in the electromagnetic field causes the material to be integrally heated to the sintering temperature, and the inert gas provides certain external pressure to promote the movement of ceramic powder particles and fill the pores in the sintering process, thereby realizing the densification of the ceramic material. The invention solves the technical problem of lower strength caused by long-time heat preservation of the alumina of the Ca-Mg-Si sintering aid system at a higher temperature by microwave isostatic pressing sintering.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: a preparation method of alumina ceramic 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 basic microstructure of material to generate heat, the dielectric loss of material in electromagnetic field to heat the whole material to sintering temperature, and inert gas provides certain external pressure to promote the movement of ceramic powder particles and fill pores during sintering, thus realizing densification of ceramic material. The alumina ceramic biscuit can uniformly absorb microwave energy in the microwave field to achieve the purpose of sintering, and the material can uniformly heat the sintered sample without temperature gradient in the sample due to the fact that the material absorbs microwave energy, so that 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 10-15deg.C/min 1 Heat preservation t at 400-600 DEG C 1 5-10min；
S2, heating rate K during sintering 2 Heating to T at 30-60deg.C/min 2 1580-1650 ℃, insulating t 1 10-30min。
Preferably, in S1, the pressure P during sintering 1 0.1-5MPa; in S2, the pressure P during sintering 2 5-10MPa; the microwave hot isostatic pressing sintering furnace is characterized in that the hot isostatic pressing atmosphere is inert gas.
After the temperature of the alumina material is higher than the critical temperature, the loss factor is rapidly increased, so that the temperature rise is extremely rapid, the sintering temperature is reduced, the sintering rate is accelerated, and the sintering time is shortened. The ceramic powder is further densified by applying hot isostatic pressing in the sintering process, the sintering temperature is lower than the normal-pressure sintering temperature of 1750 ℃, the grain growth speed is low, and the ceramic material obtained after sintering 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 rise rate K during sintering 2 40-50 ℃/min.
The inventor has studied and found through a large number of experimentsAt present, the temperature rise rate K during sintering 2 At 40-50 ℃/min, the prepared alumina ceramic has lower porosity and higher mechanical property. When K is 2 When the temperature rising rate is too fast, the reaction does not completely occur in the alumina, and the sintering process is finished, so that the alumina material has pores in the alumina material; and K is 2 When the temperature rising rate is too slow, the sintering time of the green body is prolonged, the reaction is fully carried out by more sufficient energy among particles, the prepared material is very compact, the porosity is low, but the energy consumed by the too slow temperature rising rate can be more.
Preferably, in the step (1), the alumina ceramic biscuit is prepared and obtained, and the method comprises the following steps:
(a) Uniformly mixing a polyvinyl alcohol solution and alumina powder to obtain mixed slurry;
(b) And (c) ball milling, granulating, press forming and drying 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 that of the polyvinyl alcohol solution: alumina powder = 1: (3-5); the polyvinyl alcohol solution is prepared from polyvinyl alcohol and deionized water, wherein the mass ratio of the polyvinyl alcohol to the deionized water is as follows: deionized water = 95:5.
preferably, in the step (b), the ball milling time is 1-4h, the ball milling rotating speed is 200-400r/min, the ball milling inner lining material is polyethylene, and the ball milling ball material is alumina.
Preferably, 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 200-300 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 a substrate, a ceramic bearing, a ceramic sealing element 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 basic microstructure of material to generate heat, the dielectric loss of material in electromagnetic field to heat the whole material to sintering temperature, and inert gas provides certain external pressure to promote the movement of ceramic powder particles and fill pores during sintering, thus realizing densification of ceramic material. (2) The aluminum oxide sintered sample can uniformly and integrally absorb microwave energy inside and outside a microwave field to achieve the purpose of sintering, and the material integrally absorbs the microwave energy to ensure that the temperature gradient does not exist inside the sintered sample, so that the sintered sample is uniformly heated without forming thermal stress inside the sample or causing sample cracking. (3) After the temperature of the alumina material is higher than the critical temperature, the loss factor is rapidly increased, so that the temperature rise is extremely rapid, the sintering temperature is reduced, the sintering rate is accelerated, and the sintering time is shortened. (4) The ceramic powder is further densified by applying hot isostatic pressing in the sintering process, the sintering temperature is lower than the normal-pressure sintering temperature of 1750 ℃, the grain growth speed is low, and the ceramic material obtained after sintering 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
For a better description of the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the following specific examples. In the examples, the experimental methods used are conventional methods unless otherwise specified, and the materials, reagents, etc. used, unless otherwise specified, are commercially available.
Examples 1 to 11 and comparative examples 1 to 10
The specific parameters of the alumina ceramic preparation process in examples 1 to 11 and comparative examples 1 to 10 according to the present invention are shown in Table 1: a preparation method of alumina ceramic comprises the following steps:
(1) Preparing an alumina ceramic biscuit; uniformly mixing a polyvinyl alcohol solution and alumina powder to obtain mixed slurry; ball milling, granulating, compression molding 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 grinding ball material is alumina; granulation by a spray granulation method, the particle size D50 of the granules obtained by granulation is 200 mu m, the pressure of compression molding is 150MPa, the drying temperature is 100 ℃, and the drying time is 10 hours;
(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 10-15deg.C/min 1 Heat preservation t at 400-600 DEG C 1 5-10min, pressure P during sintering 1 0.1-5MPa;
s2, heating rate K during sintering 2 Heating to T at 30-60deg.C/min 2 1580-1650 ℃, insulating t 1 Pressure P during sintering for 10-30min 2 5-10MPa.
Comparative example 8 is a normal pressure sintering in a microwave sintering furnace without isostatic pressing; comparative example 9 was sintered in a microwave hot isostatic pressing sintering furnace with a microwave frequency of 915MHz, comparative example 10 was isostatically pressed, and sintered in a conventional sintering furnace without microwave heating.
TABLE 1
Performance testing
Test standard:
(1) The method for testing the density and the porosity is carried out according to GB/T25995-2010.
(2) The flexural strength adopts a three-point bending test method, and the specific mode is as follows: at normal temperature, a 24 x 40mm size sample was subjected to pressure on a 30mm span load cell at a constant loading rate of 1mm/min until the sample broke.
(3) Grain size: the sample microtopography was photographed using SEM and grain size was measured using Nano Measurer software.
Test results: the results of the performance test are shown in Table 2.
TABLE 2
As can be seen from the comparison of example 1 and comparative example 9, since the microwave frequency is inversely related to the wavelength, the higher the frequency, the shorter the wavelength. In comparative example 9, a microwave frequency of 915MHz was used, the microwave frequency of 915MHz was lower than that of 2450MHz, and the wavelength was relatively long, so that the field intensity of the microwave field was relatively uneven, and a temperature difference was present in some areas of the sample, thereby generating thermal stress. The presence of thermal stress causes microcracking of the sample, which in turn significantly reduces the strength.
As can be seen from the comparison of the examples 1, 5-6 and the comparative examples 4-5, when the microwave temperature is higher than 1650 ℃, the interior of the blank body is continuously compact, the porosity is reduced, but the crystal grains are synchronously increased, so that the strength of the material is obviously reduced due to the abnormal growth of the crystal grains; when the microwave temperature is lower than 1580 ℃, the blank body is not densified, more air holes are formed, meanwhile, the grain growth is incomplete, and the strength of the alumina material is also obviously reduced.
As can be seen from the comparison of examples 1 to 4 and comparative examples 1 to 2, K 2 The temperature rising rate is too fast, the reaction does not completely occur in the alumina, and the sintering process is finished, so that the alumina material has pores in the alumina material; and K is 2 The temperature rising rate is too slow, and the sintering time of the green body is prolongedThe reaction is fully carried out by long particles with more sufficient energy, the prepared material is very compact and has low porosity, but the energy consumed by the too slow temperature rising rate can be more.
As can be seen from the comparison of examples 1, examples 7 to 8 and comparative examples 6 to 7, the heat-retaining time t of the S2 high temperature stage 2 Determining the full densification degree of the blank. The heat preservation time is too short, and the internal and external temperatures of the materials are different, so that the crystal grains are completely compact, and air holes remain in the body; the heat preservation time is too long, the porosity is reduced, but the grain growth is too large, and the strength is reduced.
The temperature rise and heat preservation at 600-1650 ℃ are mainly controlled by the sintering of the alumina ceramic, the heat preservation temperature and 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 a comparison of example 1 and comparative example 8, when normal pressure sintering is performed in a microwave sintering furnace without isostatic pressing, the energy provided at 1595 ℃ is insufficient to sinter the alumina ceramic, so that there are substantially no grains, and the porosity is higher and the strength is lower; as is clear from the comparison between example 1 and comparative example 10, when the sintering is performed without microwave heating by isostatic pressing, the contact area between the solid particles is reduced after the decomposition of the binder is completed, resulting in higher porosity after the completion of the sintering, and thus adversely affecting the strength.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (8)
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, 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 10-15deg.C/min 1 Heat preservation t at 400-600 DEG C 1 5-10min, pressure P during sintering 1 0.1-5MPa;
s2, heating rate K during sintering 2 Heating to T at 30-60deg.C/min 2 1580-1650 ℃, insulating t 1 Pressure P during sintering for 10-30min 2 5-10MPa.
2. The method for producing alumina ceramic according to claim 1, wherein in S2, a temperature rise rate K at the time of sintering is set to 2 40-50 ℃/min.
3. The method for preparing alumina ceramic according to claim 1, wherein in the step (1), an alumina ceramic biscuit is prepared, comprising the steps of:
(a) Uniformly mixing a polyvinyl alcohol solution and alumina powder to obtain mixed slurry;
(b) And (c) ball milling, granulating, press forming and drying the mixed slurry obtained in the step (a) to obtain the alumina ceramic biscuit.
4. The method of producing alumina ceramic according to claim 3, wherein in the step (a), the mass ratio of the polyvinyl alcohol solution to the alumina powder is: alumina powder = 1: (3-5).
5. The method of preparing alumina ceramic according to claim 3, wherein in the step (b), the ball milling time is 1-4 hours, the ball milling rotating speed is 200-400r/min, the ball milling inner and outer lining materials are polyethylene, and the grinding ball materials are alumina.
6. The method of producing alumina ceramic according to claim 3, wherein in the step (b), the granulation is carried out by a spray granulation method, the particle size D50 of the granulated particles is 200 to 300. Mu.m, the pressure of the press molding is 90 to 200MPa, the drying temperature is 85 to 110℃and the drying time is 8 to 12 hours.
7. An alumina ceramic prepared by the method for preparing an alumina ceramic according to any one of claims 1 to 6.
8. Use of the alumina ceramic of claim 7 in a substrate, a ceramic bearing and a ceramic seal.
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