CN110272282B - Low-temperature preparation method of AlON transparent ceramic - Google Patents

Low-temperature preparation method of AlON transparent ceramic Download PDF

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CN110272282B
CN110272282B CN201910570775.5A CN201910570775A CN110272282B CN 110272282 B CN110272282 B CN 110272282B CN 201910570775 A CN201910570775 A CN 201910570775A CN 110272282 B CN110272282 B CN 110272282B
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alon
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transparent ceramic
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孙泽汉
施鹰
谢建军
章蕾
雷芳
范灵聪
丁毛毛
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University of Shanghai for Science and Technology
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Abstract

The invention discloses a low-temperature preparation method of transparent aluminum oxynitride (AlON) ceramic, which is characterized in that an all-round planetary ball mill is adopted to crush and modify AlON powder prepared by the method, a single MgO sintering aid is added into the crushed powder, and the powder is calcined at 600-700 ℃ to remove carbon to obtain the AlON powder with the characteristics of small particle size, high sintering activity and the like. And then, carrying out dry pressing and cold isostatic pressing tabletting molding to obtain a blank with higher density, wherein the blank can be subjected to pressureless sintering at the temperature of below 1600-1800 ℃ to obtain AlON transparent ceramic with optical transmittance of more than 80%. The process only adds a single sintering aid, has simple operation, high preparation efficiency, low sintering temperature and low cost, and is easy for industrialized popularization.

Description

Low-temperature preparation method of AlON transparent ceramic
Technical Field
The invention relates to a preparation method of transparent ceramic, in particular to a preparation method of high-transmittance aluminum oxynitride (AlON) ceramic, which is applied to the technical field of preparation of transparent ceramic materials.
Background
The polycrystalline AlON transparent ceramic is a visible-infrared dual-waveband wave-transmitting material with a spinel structure, has excellent mechanical properties, chemical stability and optical properties, and has wide application prospects in aspects such as missile fairings, transparent armors and infrared windows. The AlON transparent ceramic is mostly prepared from powder synthesized by manual fine synthesis through a special sintering process, and the preparation process has higher difficulty due to higher sintering temperature (1880-1950 ℃). The research on the preparation of AlON under the low-temperature condition has important scientific significance and is also helpful for promoting the material to be applied as early as possible.
The process for preparing the high-density AlON ceramic can be summarized into a one-step method and a two-step method, wherein the one-step method is used for reaction sintering of Al2O3AlN mixture with Al2O3The AlN mixture is initial powder, and the AlON forming and sintering densification process is realized in one step through high-temperature sintering after the AlN mixture is formed. The reaction sintering method has simple and easy technological process and has the defect that the uniformity of the ceramic sintered by the method is poor, and the purity and the transmittance of the product are influenced. At the end of the 70 s of the 20 th century, McCauley and Corbin firstly sintered for 1h at 1950-2100 ℃ by a reaction sintering method to obtain the translucent AlON ceramic.
The two-step method is to sinter the pre-synthesized AlON powder, and the sintering method comprises pressureless sintering, hot pressing sintering (HP), hot isostatic pressing sintering (HIP), Spark Plasma Sintering (SPS), microwave sintering and the like. Compared with reaction sintering, the hot-pressing sintering method can obtain fine-grain, compact and high-strength ceramic products at lower sintering temperature and in shorter time. In recent years, there has been concern about AlON powder or Al by hot press sintering2O3AlON ceramics prepared from AlN mixture. However, the principle and structure of the hot pressing equipment limit its practical applicability and cannot meet the production requirements of conformal optical AlON ceramic products.
The pressureless sintering has low requirements on equipment, and is the most widely applied method in the preparation of AlON ceramics. In order to obtain a polycrystalline ceramic having a high light transmittance, it is necessary to reduce residual pores in the sintered ceramic as much as possible. The main function of the sintering additive is to eliminate pores during sintering. Over the years, there have been many studies on the mechanism of action of additives, but many conclusions on the mechanism have not been widely accepted, and many studies on the addition of MgO and La have been made in the early days2O3And Y2O3Preparation of translucent Al2O3The ceramic is reported. Coble et Al, general electric company, to avoid grain boundary cracks and intra-grain pores caused by excessive grain growth during sintering, was directed to Al2O3Adding MgO 0.06-0.5 wt% into the powder, and calciningThe Al with higher linear light transmittance is obtained2O3A ceramic. Kobayashi et al 0.01-0.1 wt% MgO, 0.05-0.5 wt% La2O3And 0.05-0.5 wt% Y2O3As a composite sintering aid, high-transmittance Al is prepared2O3A ceramic. They believe that MgO inhibits grain boundary migration, prevents grain boundary coils from enveloping pores, and limits grain growth. It was found that the incorporation of a small amount of MgO only inhibited the discontinuous grain growth and did not prevent the continuous grain growth. When the grain size is small, pores inside the material are discharged, and then the grains grow rapidly. Therefore, the method for preparing the AlON transparent ceramic through low-temperature pressureless sintering is key to the preparation of the AlON transparent ceramic through the steps of obtaining the AlON powder with small particle size and high activity and introducing a proper sintering aid to promote the densification of the ceramic.
Disclosure of Invention
In order to solve the problems of the prior art, the invention aims to overcome the defects in the prior art and provide a low-temperature preparation method of AlON transparent ceramic, which comprises the steps of carrying out ball-milling crushing modification on self-made high-purity AlON powder by adopting an all-round planetary ball mill to obtain AlON powder with smaller particle size, ensuring the activity of the powder, adding a single MgO sintering aid into the obtained submicron single-phase AlON powder to mix, carrying out decarburization molding, then sintering through pressureless sintering, and carrying out heat preservation at lower temperature for a period of time to obtain the AlON transparent ceramic with higher transmittance.
In order to achieve the purpose, the invention adopts the following technical scheme:
a low-temperature preparation method of AlON transparent ceramic comprises the following steps:
a. taking high-purity AlON powder as a raw material, adding absolute ethyl alcohol to prepare slurry, carrying out ball milling on the slurry for 12-36h on an all-directional planetary ball mill at a rotating speed of 200-300 r/min, carrying out crushing modification on the AlON powder, drying the slurry after ball milling, and passing through a 120-mesh screen to obtain submicron single-phase AlON powder;
b. mixing the submicron single-phase AlON powder obtained in the step a with an MgO sintering aid to obtain mixed powder, continuously performing ball milling and mixing for 6-12 hours in a planetary ball mill at the rotating speed of 100-250 r/min by taking absolute ethyl alcohol as a ball milling medium, drying the slurry after ball milling, and passing through a 200-mesh screen to obtain uniformly mixed powder;
c. b, calcining the powder obtained in the step b at 600-700 ℃ to remove carbon and activate, keeping the temperature for 4-20h, cooling the powder to natural temperature, then carrying out dry pressing molding on the obtained powder at 2-10 MPa, and further carrying out cold isostatic pressing at 100-300 MPa to further mold and densify to obtain an AlON blank;
d. and (c) placing the AlON blank obtained in the step (c) into a boron nitride crucible, then placing the crucible into a flowing nitrogen atmosphere high-temperature furnace, controlling the nitrogen flow to be 0.7-1.5L/min, and carrying out segmented pressureless sintering treatment:
firstly, heating to 1600-1700 ℃, and preserving heat for 1-4 h;
then heating to 1700-1800 ℃ and preserving the heat for 12-24 h;
and finally, cooling to room temperature along with the furnace to obtain the sintered AlON transparent ceramic.
In a preferred embodiment of the present invention, in the step a, the high purity AlON powder as a raw material is made of Al2O3the/C mixture is synthesized by a carbothermic method, the purity of the powder is more than or equal to 99 percent, the median particle size is 56.3 mu m, and the specific surface area (BET) is 0.316m2/g。
As a preferable technical scheme of the invention, in the step a, the obtained submicron single-phase AlON powder has the median particle diameter of less than or equal to 1 μm and the specific surface area (BET) of not less than 10m2(ii) in terms of/g. Further preferably, the median particle size of the obtained submicron single-phase AlON powder is 0.2-0.7 μm.
In a preferred embodiment of the present invention, in the step b, the addition amount of the sintering aid MgO is 0.4 to 0.8% by mass of the submicron single-phase AlON powder obtained in the step a.
As a preferable technical scheme of the invention, in the step a or b, the purity of the absolute ethyl alcohol is not lower than that of analytical purity, and a ball grinding ball is Al with the diameter of 3-5 mm2O3The amount of the absolute ethyl alcohol is 0.5-1.5 times of the mass of the mixed powder, and the mass ratio of the ball material is (10 ℃15):1。
In the step c, the relative density of the AlON blank subjected to isostatic pressing is 45-55%.
In the step d, the heating rate of each stage of heating process of the segmented pressureless sintering treatment is controlled to be 3-10 ℃/min respectively.
In the step d, the sintered AlON transparent ceramic is subjected to thinning, grinding and polishing treatment to enable the thickness of the ceramic to be 1-5 mm, so that an AlON transparent ceramic product is obtained.
Compared with the prior art, the invention has the following obvious and prominent substantive characteristics and remarkable advantages:
1. the method adopts the omnibearing planetary ball mill to perform ball milling, crushing and modification on the self-made high-purity AlON powder to obtain AlON ceramic powder with small particle size and high reaction activity, wherein the particle size is 0.2-0.7 mu m, the powder with smaller particle size is beneficial to uniform dispersion when a small amount of sintering aids are mixed, and the growth of crystal grains is more uniform in the ceramic sintering process;
2. the method of the invention adopts the addition of single sintering aid MgO to ensure that the ceramics can obtain AlON transparent ceramics with higher transmittance at lower temperature by a pressureless sintering method, the relative density of the AlON transparent ceramics reaches more than 99 percent of theoretical density, the transmittance of a sample with the thickness of 1mm reaches more than 80 percent in a visible light wave band, the performance is excellent, the AlON transparent ceramics are suitable for being used as high-temperature window materials and cover body materials, and simultaneously, the production cost is low, the operation is convenient, the requirement on production equipment is relatively low, and the AlON transparent ceramics are suitable for industrial production.
3. The method has the advantages of simple process, convenient control and operation, low cost, high quality of the obtained AlON transparent ceramic material product and easy popularization and application.
Drawings
Fig. 1 is an SEM picture of AlON powder as a raw material before ball milling according to an embodiment of the present invention.
FIG. 2 is an SEM picture of a submicron single-phase AlON powder obtained after ball milling and crushing in an embodiment of the invention.
Fig. 3 is a graph showing the particle size distribution of AlON powder as a raw material before ball milling according to an embodiment of the present invention.
FIG. 4 is a graph showing the particle size distribution of the single-phase AlON powder in submicron order obtained after ball milling and crushing in the embodiment of the present invention.
FIG. 5 is an SEM image of a cross section of a transparent AlON ceramic prepared by a method in an embodiment of the invention.
FIG. 6 is a graph showing the optical transmittance of a transparent AlON ceramic prepared by a method according to an embodiment of the present invention.
FIG. 7 is an SEM image of a sample cross section of a transparent AlON ceramic prepared by the second method of the embodiment of the invention.
Fig. 8 is a graph of optical transmittance of the transparent AlON ceramic prepared by the second method according to the embodiment of the present invention.
FIG. 9 is an SEM image of a sample cross section of a transparent AlON ceramic prepared by the method of the third aspect of the embodiment of the present invention.
FIG. 10 is a graph showing the optical transmittance of a transparent AlON ceramic prepared by the three-way method according to the embodiment of the present invention.
FIG. 11 is an SEM image of a sample cross section of a transparent AlON ceramic prepared by the tetragonal method of the embodiment of the invention.
Fig. 12 is a graph showing an optical transmittance of a transparent AlON ceramic prepared by a tetragonal method according to an embodiment of the present invention.
Fig. 13 is an SEM picture of a sample cross-section of the transparent AlON ceramic prepared by the fifth method according to the example of the present invention.
Fig. 14 is a graph of optical transmittance of a transparent AlON ceramic prepared by the fifth method according to an embodiment of the present invention.
Detailed Description
The above-described scheme is further illustrated below with reference to specific embodiments, which are detailed below:
the first embodiment is as follows:
in this embodiment, a low-temperature preparation method of an AlON transparent ceramic includes the following steps:
a. weighing 30g of high-purity AlON powder serving as a raw material, putting the AlON powder into an alumina ball-milling tank, putting 600g of alumina balls with the diameter of 5mm, and adding anhydrous ethyl acetate with the mass of 0.8 time of that of the powderAlcohol is a ball milling medium; the purity of the absolute ethyl alcohol is not lower than that of analytical purity; adding absolute ethyl alcohol to prepare slurry, wherein the high-purity AlON powder is prepared from Al2O3the/C mixture is synthesized by a carbothermic method, the powder purity is 99 percent, the median particle size is 56.3 mu m, and the specific surface area (BET) is 0.316m2(ii)/g; putting the ball milling tank with the prepared materials into an all-directional planetary ball mill, ball milling for 24h at the rotating speed of 250r/min, crushing and modifying the AlON powder, putting the slurry into a container after ball milling and crushing, then putting the ball-milled slurry into a drying box, drying for 12h at the temperature of 60 ℃, then heating to 100 ℃, drying for 6h till complete drying, and sieving with a 120-mesh sieve to obtain the submicron single-phase AlON powder;
as shown in fig. 1, is an SEM picture of AlON powder before ball milling; FIG. 2 shows SEM pictures of submicron single-phase AlON powder obtained before and after ball milling, wherein powder particles are obviously refined; as shown in fig. 3 and 4, the particle size distribution diagrams of the AlON powder before and after ball milling and the submicron single-phase AlON powder distribution diagrams are respectively shown, the particle size of the submicron single-phase AlON powder obtained after ball milling reaches submicron, and the median particle size is reduced to below 1 μm; specific surface area (BET) greater than 10m2/g；
b. Weighing 15g of submicron single-phase AlON powder obtained after ball milling in the step a, filling the submicron single-phase AlON powder into a polytetrafluoroethylene tank, weighing 0.6% of MgO sintering aid in the mass of the submicron single-phase AlON powder, filling the MgO sintering aid into the polytetrafluoroethylene tank, mixing to obtain mixed powder, then putting 150.9g of alumina balls with the diameter of 5mm, taking absolute ethyl alcohol as a ball milling medium, adding absolute ethyl alcohol with the mass of 1 time of that of the powder as the ball milling medium, putting the ball milling tank with the materials into an all-directional planetary ball mill, carrying out ball milling for 12 hours at the rotating speed of 250r/min, putting slurry into a container after ball milling and mixing, putting the container into a drying box, drying for 20 hours at the temperature of 60 ℃, taking out the powder, and passing through a 200-mesh screen to obtain uniformly mixed powder;
c. b, putting the sieved powder obtained in the step b into an alumina crucible, calcining the crucible at 650 ℃ for 12 hours, and carrying out calcination decarbonization and activation treatment; cooling the powder subjected to the decarbonization treatment to room temperature, pouring 1.5g of the obtained powder into a mold with the diameter of 20mm, putting the mold into a dry press, and performing dry pressing molding under the pressure of 4 MPa; sealing the blank body after dry pressing into a sealing bag, placing the sealing bag in cold isostatic pressing, and carrying out cold isostatic pressing at the pressure of 200Mpa for further molding and densification to obtain an AlON blank body; the relative density of the AlON blank formed by isostatic pressing can reach 55 percent;
d. and c, placing the AlON blank obtained in the step c into a boron nitride crucible, then placing the crucible into a flowing nitrogen atmosphere high-temperature furnace, vacuumizing the furnace to negative pressure, then filling pure nitrogen to normal pressure, controlling the flow of the nitrogen to be 0.8L/min, raising the temperature to 1700 ℃ at the heating rate of 10 ℃/min, preserving the temperature for 2h, then raising the temperature to 1800 ℃ at the heating rate of 3 ℃/min, preserving the temperature for 24h, carrying out segmented pressureless sintering treatment, and finally cooling to room temperature along with the furnace to obtain the sintered AlON transparent ceramic.
And d, taking out the AlON ceramic sintered in the step d, and thinning, grinding and polishing the AlON transparent ceramic to enable the thickness of the ceramic to be 1mm to obtain an AlON transparent ceramic product.
Experimental test analysis:
microscopic observation is carried out on the AlON transparent ceramic product prepared by the method of the embodiment, fig. 5 shows the cross-sectional morphology of the sample without obvious pores, and fig. 6 shows the optical transmittance curve of the sample, and the optical transmittance curve reaches 83.8% at 1100 nm.
The AlON transparent ceramic prepared by the embodiment has good transparency, the AlON powder is subjected to ball milling, crushing and modification to obtain the refined powder with the particle size of 1 mu m, and the high-transmittance transparent ceramic can be obtained by introducing a single sintering aid in a pressureless sintering mode and keeping the temperature at a low temperature for a period of time. The transparent AlON ceramic obtained by the embodiment has high transmittance, good ceramic grain growth, uniform grain size and high preparation repetition rate, and can be suitable for industrial production.
Example two:
this embodiment is substantially the same as the first embodiment, and is characterized in that:
in this embodiment, a low-temperature preparation method of an AlON transparent ceramic includes the following steps:
a. the step is the same as the first embodiment;
b. weighing 15g of submicron single-phase AlON powder obtained after ball milling in the step a, filling the submicron single-phase AlON powder into a polytetrafluoroethylene tank, weighing 0.4% of MgO sintering aid in the mass of the submicron single-phase AlON powder, filling the MgO sintering aid into the polytetrafluoroethylene tank, mixing to obtain mixed powder, then putting 150.9g of alumina balls with the diameter of 5mm, taking absolute ethyl alcohol as a ball milling medium, adding absolute ethyl alcohol with the mass of 1 time of that of the powder as the ball milling medium, putting the ball milling tank with the materials into an all-directional planetary ball mill, carrying out ball milling for 12 hours at the rotating speed of 250r/min, putting slurry into a container after ball milling and mixing, putting the container into a drying box, drying for 20 hours at the temperature of 60 ℃, taking out the powder, and passing through a 200-mesh screen to obtain uniformly mixed powder;
c. the step is the same as the first embodiment;
d. the procedure is the same as in the first embodiment.
And d, taking out the AlON ceramic sintered in the step d, and thinning, grinding and polishing the AlON transparent ceramic to enable the thickness of the ceramic to be 1mm to obtain an AlON transparent ceramic product.
Experimental test analysis:
microscopic observation is carried out on the AlON transparent ceramic product prepared by the method of the embodiment, fig. 7 shows the cross-sectional morphology of the sample without obvious pores, and fig. 8 shows the optical transmittance curve of the sample, and the optical transmittance can reach 82.1% at 1100 nm.
The AlON transparent ceramic prepared by the embodiment has good transparency, the AlON powder is subjected to ball milling, crushing and modification to obtain the refined powder with small particle size of 1 mu m, and the high-transmittance transparent ceramic can be obtained by introducing a single sintering aid in a pressureless sintering mode and keeping the temperature at a low temperature for a period of time. The transparent AlON ceramic obtained by the embodiment has high transmittance, good ceramic grain growth, uniform grain size and high preparation repetition rate, and can be suitable for industrial production.
Example three:
this embodiment is substantially the same as the previous embodiment, and is characterized in that:
in this embodiment, a low-temperature preparation method of an AlON transparent ceramic includes the following steps:
a. the step is the same as the first embodiment;
b. weighing 30g of submicron single-phase AlON powder obtained after ball milling in the step a, filling the submicron single-phase AlON powder into a nylon tank, weighing 0.6% MgO sintering aid of the mass of the submicron single-phase AlON powder, filling the MgO sintering aid into the nylon tank, mixing to obtain mixed powder, putting 301.8g of alumina balls with the diameter of 5mm, taking absolute ethyl alcohol as a ball milling medium, adding absolute ethyl alcohol with the mass of 1 time of the powder as the ball milling medium, and putting the ball milling tank with the materials on an omnibearing planetary ball mill to ball mill for 12 hours at the rotating speed of 250 r/min; after ball milling and mixing are finished, placing the slurry into a container, placing the container into a drying box for drying for 20 hours at the temperature of 60 ℃, taking out the powder, and sieving the powder by a 200-mesh sieve to obtain uniformly mixed powder;
c. b, putting the sieved powder obtained in the step b into an alumina crucible, calcining the crucible at 650 ℃ for 12 hours, and carrying out calcination decarbonization and activation treatment; cooling the powder subjected to the decarbonization treatment to room temperature, pouring 25g of the obtained powder into a mold with the diameter of 50mm, putting the mold on a dry press, and performing dry pressing molding at the pressure of 6 MPa; sealing the blank body after dry pressing into a sealing bag, placing the sealing bag in cold isostatic pressing for further molding and densification by the cold isostatic pressing at the pressure of 200Mpa to obtain an AlON blank body; the relative density of the AlON blank formed by isostatic pressing can reach 55 percent;
d. the procedure is the same as in the first embodiment.
And d, taking out the AlON ceramic sintered in the step d, and thinning, grinding and polishing the AlON transparent ceramic to ensure that the thickness of the ceramic is 5mm to obtain an AlON transparent ceramic product.
Experimental test analysis:
microscopic observation is carried out on the AlON transparent ceramic product prepared by the method of the embodiment, FIG. 9 shows the cross-sectional morphology of the sample without obvious pores, and FIG. 10 shows the optical transmittance curve of the sample, and the optical transmittance can reach 70.5% at 1100 nm.
The AlON transparent ceramic prepared by the embodiment has good transparency, the AlON powder is subjected to ball milling, crushing and modification to obtain the refined powder with small particle size of 1 mu m, and the high-transmittance transparent ceramic can be obtained by introducing a single sintering aid in a pressureless sintering mode and keeping the temperature at a low temperature for a period of time. The transparent AlON ceramic obtained by the embodiment has high transmittance, good ceramic grain growth, uniform grain size and high preparation repetition rate, and can be suitable for industrial production.
Example four:
this embodiment is substantially the same as the previous embodiment, and is characterized in that:
in this embodiment, a low-temperature preparation method of an AlON transparent ceramic includes the following steps:
a. weighing 30g of AlON powder serving as a raw material, putting the AlON powder into an alumina ball-milling tank, putting 675g of alumina balls with the diameter of 3mm, and adding absolute ethyl alcohol with the mass of 0.5 time of that of the powder serving as a ball-milling medium; the purity of the absolute ethyl alcohol is not lower than that of analytical purity; adding absolute ethyl alcohol to prepare slurry, wherein the high-purity AlON powder is prepared from Al2O3the/C mixture is synthesized by a carbothermic method, the powder purity is 99 percent, the median particle size is 56.3 mu m, and the specific surface area (BET) is 0.316m2(ii)/g; putting the ball milling tank with the prepared materials into an all-directional planetary ball mill, ball milling for 36h at the rotating speed of 200r/min, crushing and modifying AlON powder, putting the slurry into a container after ball milling and crushing, then putting the ball-milled slurry into a drying box, drying for 12h at the temperature of 60 ℃, then heating to 100 ℃, drying for 6h till complete drying, and passing through a 120-mesh screen to obtain submicron single-phase AlON powder;
compared with the high-purity AlON powder used as a raw material, the submicron single-phase AlON powder particles are obviously refined, the particle size of the submicron single-phase AlON powder obtained after ball milling reaches the submicron level, and the median particle size is reduced to 0.7 mu m; specific surface area (BET) greater than 10m2/g；
b. Weighing 15g of submicron single-phase AlON powder obtained after ball milling in the step a, filling the submicron single-phase AlON powder into a polytetrafluoroethylene tank, weighing 0.8% of MgO sintering aid in the mass of the submicron single-phase AlON powder, filling the MgO sintering aid into the polytetrafluoroethylene tank, mixing to obtain mixed powder, then putting 226.8g of alumina balls with the diameter of 5mm, taking absolute ethyl alcohol as a ball milling medium, adding absolute ethyl alcohol with the mass of 1.5 times of that of the powder as the ball milling medium, putting the ball milling tank with the prepared materials into an omnibearing planetary ball mill, carrying out ball milling for 6h at the rotating speed of 100r/min, putting slurry into a container after ball milling and mixing, putting the container into a drying box, drying for 20h at the temperature of 60 ℃, taking out the powder, and sieving the powder by a 200-mesh sieve to obtain uniformly mixed powder;
c. b, putting the sieved powder obtained in the step b into an alumina crucible, and calcining the crucible at 600 ℃ for 20 hours to perform calcination decarbonization and activation treatment; cooling the powder subjected to the decarbonization treatment to room temperature, pouring 1.5g of the obtained powder into a mold with the diameter of 20mm, putting the mold into a dry press, and performing dry pressing molding under the pressure of 2 MPa; sealing the blank body after dry pressing into a sealing bag, placing the sealing bag in cold isostatic pressing, and carrying out cold isostatic pressing at the pressure of 100Mpa for further molding and densification to obtain an AlON blank body; the relative density of the AlON blank subjected to isostatic pressing is 45 percent;
d. and c, placing the AlON blank obtained in the step c into a boron nitride crucible, then placing the crucible into a flowing nitrogen atmosphere high-temperature furnace, vacuumizing the furnace to negative pressure, then filling pure nitrogen to normal pressure, controlling the flow of the nitrogen to be 0.7L/min, heating to 1600 ℃ at the heating rate of 10 ℃/min, preserving the heat for 4h, then heating to 1700 ℃ at the heating rate of 3 ℃/min, preserving the heat for 12h, carrying out segmented pressureless sintering treatment, and finally cooling to room temperature along with the furnace to obtain the sintered AlON transparent ceramic.
And d, taking out the AlON ceramic sintered in the step d, and thinning, grinding and polishing the AlON transparent ceramic to enable the thickness of the ceramic to be 2mm to obtain an AlON transparent ceramic product.
Experimental test analysis:
for the AlON transparent ceramic product prepared by the method of this embodiment, fig. 11 is a sample cross-sectional profile without significant pores, and fig. 12 is an optical transmittance curve of the sample, where the optical transmittance reaches 72.1% at 1100 nm. The AlON transparent ceramic prepared by the embodiment has good transparency, the AlON powder is subjected to ball milling, crushing and modification to obtain the refined powder with the particle size of 1 mu m, and the high-transmittance transparent ceramic can be obtained by introducing a single sintering aid in a pressureless sintering mode and keeping the temperature at a low temperature for a period of time. The transparent AlON ceramic obtained by the embodiment has high transmittance, good ceramic grain growth, uniform grain size and high preparation repetition rate, and can be suitable for industrial production.
Example five:
this embodiment is substantially the same as the previous embodiment, and is characterized in that:
in this embodiment, a low-temperature preparation method of an AlON transparent ceramic includes the following steps:
a. weighing 30g of AlON powder serving as a raw material, putting the AlON powder into an alumina ball-milling tank, putting 675g of alumina balls with the diameter of 3mm, and adding absolute ethyl alcohol with the mass of 0.5 time of that of the powder serving as a ball-milling medium; the purity of the absolute ethyl alcohol is not lower than that of analytical purity; adding absolute ethyl alcohol to prepare slurry, wherein the high-purity AlON powder is prepared from Al2O3the/C mixture is synthesized by a carbothermic method, the powder purity is 99 percent, the median particle size is 56.3 mu m, and the specific surface area (BET) is 0.316m2(ii)/g; putting the ball milling tank with the prepared materials into an all-directional planetary ball mill, carrying out ball milling for 12h at the rotating speed of 300r/min, carrying out crushing modification on AlON powder, putting the slurry into a container after the ball milling and crushing are finished, then putting the slurry after ball milling into a drying box, drying for 12h at the temperature of 60 ℃, then heating to 100 ℃, drying for 6h till complete drying, and passing through a 120-mesh screen to obtain submicron single-phase AlON powder;
compared with the high-purity AlON powder used as a raw material, the submicron single-phase AlON powder particles are obviously refined, the particle size of the submicron single-phase AlON powder obtained after ball milling reaches the submicron level, and the median particle size is reduced to 0.2 mu m; specific surface area (BET) greater than 10m2/g；
b. Weighing 15g of submicron single-phase AlON powder obtained after ball milling in the step a, filling the submicron single-phase AlON powder into a polytetrafluoroethylene tank, weighing 0.8% of MgO sintering aid in the mass of the submicron single-phase AlON powder, filling the MgO sintering aid into the polytetrafluoroethylene tank, mixing to obtain mixed powder, then putting 226.8g of alumina balls with the diameter of 5mm, taking absolute ethyl alcohol as a ball milling medium, adding absolute ethyl alcohol with the mass of 1.5 times of that of the powder as the ball milling medium, putting the ball milling tank with the prepared materials into an omnibearing planetary ball mill, carrying out ball milling for 6h at the rotating speed of 100r/min, putting slurry into a container after ball milling and mixing, putting the container into a drying box, drying for 20h at the temperature of 60 ℃, taking out the powder, and sieving the powder by a 200-mesh sieve to obtain uniformly mixed powder;
c. b, putting the sieved powder obtained in the step b into an alumina crucible, and calcining the crucible at 700 ℃ for 4 hours to perform calcination decarbonization and activation treatment; cooling the powder subjected to the decarbonization treatment to room temperature, pouring 1.5g of the obtained powder into a mold with the diameter of 20mm, putting the mold into a dry press, and performing dry pressing molding under the pressure of 10 MPa; sealing the blank body after dry pressing into a sealing bag, placing the sealing bag in cold isostatic pressing, and carrying out cold isostatic pressing at the pressure of 300Mpa for further molding and densification to obtain an AlON blank body; the relative density of the AlON blank subjected to isostatic pressing is 55 percent;
d. and c, placing the AlON blank obtained in the step c into a boron nitride crucible, then placing the crucible into a flowing nitrogen atmosphere high-temperature furnace, vacuumizing the furnace to negative pressure, then filling pure nitrogen to normal pressure, controlling the flow of the nitrogen to be 1.5L/min, raising the temperature to 1700 ℃ at the heating rate of 10 ℃/min, preserving the temperature for 1h, then raising the temperature to 1750 ℃ at the heating rate of 3 ℃/min, preserving the temperature for 16h, carrying out segmented pressureless sintering treatment, and finally cooling to room temperature along with the furnace to obtain the sintered AlON transparent ceramic.
And d, taking out the AlON ceramic sintered in the step d, and thinning, grinding and polishing the AlON transparent ceramic to enable the thickness of the ceramic to be 2mm to obtain an AlON transparent ceramic product.
Experimental test analysis:
for the AlON transparent ceramic product prepared by the method of this embodiment, fig. 11 is a sample cross-sectional profile without obvious pores, and fig. 12 is an optical transmittance curve diagram of the sample, where the optical transmittance reaches 73.6% at 1100 nm. The AlON transparent ceramic prepared by the embodiment has good transparency, the AlON powder is subjected to ball milling, crushing and modification to obtain the refined powder with the particle size of 1 mu m, and the high-transmittance transparent ceramic can be obtained by introducing a single sintering aid in a pressureless sintering mode and keeping the temperature at a low temperature for a period of time. The transparent AlON ceramic obtained by the embodiment has high transmittance, good ceramic grain growth, uniform grain size and high preparation repetition rate, and can be suitable for industrial production.
In summary, in the low-temperature preparation method of transparent aluminum oxynitride (AlON) ceramic according to the embodiments of the present invention, an all-directional planetary ball mill is used to crush and modify AlON powder prepared in the present invention, a single MgO sintering aid is added to the crushed AlON powder, and the AlON powder is calcined at 600 to 700 ℃ to remove carbon, so that AlON powder having characteristics of small particle size, high sintering activity, and the like is obtained. And then, carrying out dry pressing and cold isostatic pressing tabletting molding to obtain a blank with higher density, wherein the blank can be subjected to pressureless sintering at the temperature of below 1600-1800 ℃ to obtain AlON transparent ceramic with optical transmittance of more than 80%. The process only adds a single sintering aid, has simple operation, high preparation efficiency, low sintering temperature and low cost, and is easy for industrialized popularization.
The embodiments of the present invention have been described with reference to the accompanying drawings, but the present invention is not limited to the embodiments, and various changes and modifications can be made according to the purpose of the invention, and any changes, modifications, substitutions, combinations or simplifications made according to the spirit and principle of the technical solution of the present invention shall be equivalent substitutions, as long as the purpose of the present invention is met, and the invention shall fall within the protection scope of the present invention as long as the technical principle and the inventive concept of the method for preparing the AlON transparent ceramic at low temperature of the present invention are not deviated.

Claims (9)

1. A low-temperature preparation method of AlON transparent ceramic is characterized by comprising the following steps:
a. taking high-purity AlON powder as a raw material, adding absolute ethyl alcohol to prepare slurry, carrying out ball milling on the slurry for 12-36h on an all-directional planetary ball mill at a rotating speed of 200-300 r/min, carrying out crushing modification on the AlON powder, drying the slurry after ball milling, and passing through a 120-mesh screen to obtain submicron single-phase AlON powder;
b. mixing the submicron single-phase AlON powder obtained in the step a with an MgO sintering aid to obtain mixed powder, continuously performing ball milling and mixing for 6-12 hours in a planetary ball mill at the rotating speed of 100-250 r/min by taking absolute ethyl alcohol as a ball milling medium, drying the slurry after ball milling, and passing through a 200-mesh screen to obtain uniformly mixed powder; the addition content of the added sintering aid MgO is 0.4-0.8% of the mass of the submicron single-phase AlON powder obtained in the step a;
c. b, calcining the powder obtained in the step b at 600-700 ℃ to remove carbon and activate, keeping the temperature for 4-20h, cooling the powder to natural temperature, then carrying out dry pressing molding on the obtained powder at 2-10 MPa, and further carrying out cold isostatic pressing at 100-300 MPa to further mold and densify to obtain an AlON blank;
d. and (c) placing the AlON blank obtained in the step (c) into a boron nitride crucible, then placing the crucible into a flowing nitrogen atmosphere high-temperature furnace, controlling the nitrogen flow to be 0.7-1.5L/min, and carrying out segmented pressureless sintering treatment:
firstly, heating to 1600-1700 ℃, and preserving heat for 1-4 h;
then heating to 1700-1800 ℃ and preserving the heat for 12-24 h;
and finally, cooling to room temperature along with the furnace to obtain the sintered AlON transparent ceramic.
2. The method for preparing AlON transparent ceramic at low temperature according to claim 1, wherein in the step a, high-purity AlON powder used as a raw material is made of Al2O3the/C mixture is synthesized by a carbothermic method, the powder purity is more than or equal to 99 percent, the median particle size is 56.3 mu m, and the specific surface area (BET) is 0.316m2/g。
3. The low-temperature preparation method of the AlON transparent ceramic according to claim 1, characterized in that in the step a, the obtained submicron single-phase AlON powder has a median particle size of less than or equal to 1 mu m and a specific surface area (BET) of not less than 10m2/g。
4. The low-temperature preparation method of the AlON transparent ceramic is characterized in that in the step a, the median particle size of the obtained submicron single-phase AlON powder is 0.2-0.7 mu m.
5. The low-temperature preparation method of AlON transparent ceramic according to claim 1, wherein in the step a, the purity of the absolute ethyl alcohol is not lower than that of analytical grade, and a ball milling ball is Al with a diameter of 3-5 mm2O3The amount of the absolute ethyl alcohol is 0.5-1.5 times of the mass of the AlON powder, and the mass ratio of the ball material is (10-15): 1.
6. The method for preparing the AlON transparent ceramic at low temperature according to claim 1, wherein in the step b, the absolute ethyl alcohol has purityNot less than analytically pure purity, and the ball grinding ball is Al with the diameter of 3-5 mm2O3The amount of the absolute ethyl alcohol is 0.5-1.5 times of the mass of the mixed powder, and the mass ratio of the ball material is (10-15): 1.
7. The low-temperature preparation method of the AlON transparent ceramic is characterized in that in the step c, the relative density of the isostatic pressed AlON blank is 45-55%.
8. The low-temperature preparation method of the AlON transparent ceramic according to claim 1, wherein in the step d, the temperature rise rate of each temperature rise process of each stage of the segmented pressureless sintering treatment is controlled to be 3-10 ℃/min.
9. The low-temperature preparation method of the AlON transparent ceramic is characterized in that in the step d, the sintered AlON transparent ceramic is subjected to thinning, grinding and polishing treatment to enable the thickness of the ceramic to be 1-5 mm, so that an AlON transparent ceramic product is obtained.
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