CN112225564B - Aluminum oxynitride transparent ceramic and preparation method thereof - Google Patents
Aluminum oxynitride transparent ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an aluminum oxynitride transparent ceramic and a preparation method thereof, AlN powder and Al2O3 powder are used as raw materials, B (OH)3, a Mg source and a rare earth source are used as sintering aids, and the aluminum oxynitride transparent ceramic is obtained by mixing, molding and sintering; the Mg source is MgAl2O 4; the rare earth source is selected from rare earth oxide or/and rare earth composite oxide, preferably at least one selected from Y3Al5O12, Y2O3, Lu3Al5O12, Lu2O3 and Sc2O 3.
Description
Technical Field
The invention relates to an aluminum oxynitride transparent ceramic and a preparation method thereof, belonging to the field of transparent ceramics.
Background
The transparent aluminum oxynitride ceramic is Al at high temperature2O3And AlN in a certain composition range (16 to 35.7 mol% AlN), belonging to a cubic systemThe material has optical isotropy, has excellent light transmittance in near ultraviolet to middle infrared bands (0.2-6 mu m), and has the theoretical transmittance of 85.2%. And the aluminum oxynitride transparent ceramic has high hardness, high strength and excellent dielectric property,
corrosion resistance, excellent wear resistance and scratch resistance, are preferred materials for high temperature infrared window, hood and transparent armor.
Since McCauly produced the first aluminum oxynitride translucent ceramic in the world in 1976, various processes for producing aluminum oxynitride transparent ceramic materials have been developed. These processes are divided into two categories based on the differences in starting materials: a) sintering after forming by taking aluminum oxynitride powder synthesized by a precursor as a raw material; the method has the advantage that the generated aluminum oxynitride powder has good sintering performance. However, the preparation period of the powder is long, and the reaction product is difficult to control due to temperature, atmosphere and raw material composition, and the powder parameters are unstable, which is not favorable for preparing aluminum oxynitride transparent ceramics on a large scale. b) With Al2O3Reacting and sintering with AlN; the method avoids the steps of preparing and treating the aluminum oxynitride powder, has simple process and low cost, and is easy for batch production. But because of mismatching of sintering performance of raw materials, the obtained aluminum oxynitride has low light transmittance or is devitrified. Researchers generally achieve the preparation of the aluminum oxynitride transparent ceramic by a reaction sintering method by adding a sintering aid to promote the sintering process and removing pores. Since the sintering temperature of the method is usually higher than 1900 ℃, the person skilled in the art generally selects a substance with a higher melting point as a sintering aid.
For example, patent 1 (US patent 20100167907a1) discloses a method for preparing polycrystalline aluminum oxynitride as MgO (< 0.5 wt.%), Y2O3(< 0.5 wt.%) and/or BN (< 0.5 wt.%) as sintering aid, and through presintering at 1550-1750 deg.C and sintering at 1900 deg.C, aluminum oxynitride with good light transmittance can be obtained. Patent 2 (Chinese publication No. CN106342081B) discloses a solid-phase preparation method of aluminum oxynitride transparent ceramic, which uses Al2O3And AlN as raw material, adding 0.1-2.0 wt.% of rare earth oxide with purity not less than 99.9% and 0.5-10 wt%As a sintering additive, or a corresponding salt thereof; the rare earth oxide comprises La2O3、Gd2O3、Yb2O3(ii) a The metal oxide includes Li2O、MgO、CaO、Y2O3、TiO2、SiO2The aluminum oxynitride transparent ceramic with the thickness of 3.5mm is prepared by adopting a high-temperature solid-phase reaction process, and the transmittance in a visible light wave band is only 40%. Patent 3 (Chinese publication No. CN107344854A) discloses Al2O3And the mass ratio of AlN to AlN is (70-73): (30 to 27), 0.1 wt.% of Y is added2O30.1 wt.% MgO, bonded to N by spark plasma sintering2The aluminum oxynitride transparent ceramic is prepared by atmosphere sintering, a 2mm sample is obtained, and the transmittance of the visible light wave band is only about 70%. However, in the case of the aluminum oxynitride transparent ceramic prepared by the reactive sintering method, the optical transmittance is far from the ideal transmittance of 85.2%. And the transmittance of the aluminum oxynitride transparent ceramic prepared by the reactive sintering method in the visible-infrared region is only 80 percent, so that the possibility of production and application can be realized.
Disclosure of Invention
In order to solve the problems, the invention provides high-transmittance aluminum oxynitride transparent ceramic and a preparation method thereof.
On one hand, the invention provides a preparation method of aluminum oxynitride transparent ceramic, which adopts AlN powder and Al2O3The powder is used as raw material and adopts B (OH)3Mixing, forming and sintering the Mg source and the rare earth source which are used as sintering aids to obtain the aluminum oxynitride transparent ceramic; the Mg source is selected from MgAl2O4(ii) a The rare earth source is selected from rare earth oxide or/and rare earth composite oxide, preferably Y3Al5O12、Y2O3、Lu3Al5O12、Lu2O3And Sc2O3At least one of (1).
In the present disclosure, a low melting point B (OH) is used3And combined with a source of Mg (e.g. MgAl)2O4) And rare earth oxide or/and rare earth composite oxide (e.g. Y)3Al5O12、Y2O3、Lu3Al5O12、Lu2O3、Sc2O3Etc.) as sintering aid, adding raw material powder Al2O3And AlN, and preparing the high-optical-quality aluminum oxynitride transparent ceramic by reaction sintering. In Al2O3In reaction sintering with AlN, Al2O3A source of Mg (e.g., MgAl) that is more easily sintered and less deliquescent than AlN2O4) Can effectively inhibit Al in early stage of sintering as sintering aid2O3The crystal grains of (1) grow up, pores formed due to the oversize crystal grains are reduced, and the crystal grains can be mixed with Al2O3Capable of forming a liquid phase at high temperatures. The rare earth oxide or/and the rare earth composite oxide forms a liquid phase (e.g., Y) at grain boundaries during sintering3Al5O12、Lu3Al5O12、Sc3Al5O12And the like), the grain boundary migration rate can be improved, but the grain boundary migration rate is too high, so that pores are easily wrapped in the crystal grains, and the transmittance of the sample is reduced. B (OH)3Decomposition to B at low temperature2O3Liquid phase, B2O3The liquid phase may restrict the movement of grain boundaries. And the ternary composite auxiliary agent is doped, so that the relative migration rate of air holes and grain boundaries is regulated, the air holes are eliminated, and the sample transmittance is improved.
Preferably, the AlN powder and Al2O3The molar ratio of the powder (25-35): (75-65).
Preferably, the Mg source is added with AlN powder and Al2O3(0.02-0.5) wt.% of the total mass of the powder; the B (OH)3The adding amount of the aluminum nitride powder and the Al2O3(0.02-0.5) wt.%, preferably (0.02-0.4) wt.% of the total mass of the powder; the addition amount of the rare earth source is AlN powder and Al2O3(0.02 to 0.1) wt.%, preferably (0.05 to 0.1) wt.% of the total mass of the powder.
Preferably, the AlN powder has the purity of more than or equal to 99.99 percent and the particle size of 0.5-1 mu m; the Al is2O3The purity of the powder is more than or equal to 99.99%, and the particle size is 0.5-2 μm.
Preferably, said B (OH)3The purity of the product is not lower than 99.99 percent; the purity of the Mg source is not lower than 99.99%; the purity of the rare earth source is not less than 99.99%.
Preferably, the mixing mode is ball milling mixing; the rotation speed of ball milling mixing is 200-300 r/min, and the time is 15-48 hours; preferably, the rotational speed of the ball milling mixing is 250 rpm for 20 hours.
Preferably, the forming method is dry pressing forming or/and cold isostatic pressing forming; the pressure of the dry pressing is 10-20 MPa, and the pressure maintaining time is 1-3 minutes; the pressure of the cold isostatic pressing treatment is 150-250 MPa, and the pressure maintaining time is 3-20 minutes.
Preferably, the sintering atmosphere is nitrogen atmosphere, the temperature is 1930-1980 ℃, and the time is 20-30 hours.
Preferably, the nitrogen atmosphere is nitrogen flowing at a flow rate of 1 to 2L/min; preferably, the nitrogen atmosphere is flowing nitrogen at a flow rate of 1.5L/min.
On the other hand, the invention provides the aluminum oxynitride transparent ceramic prepared by the preparation method, the density of the aluminum oxynitride transparent ceramic is more than or equal to 99.9%, the porosity of the aluminum oxynitride transparent ceramic is less than 0.1%, and the linear transmittance at 700nm is 75-83%.
Has the advantages that:
the high-optical-quality aluminum oxynitride transparent ceramic obtained by the invention is characterized in that: the transmittance of a sample (4mm thick) subjected to double-side polishing in a visible-infrared region can reach more than 83%, so that the material meets the application requirements of the material in the fields of transparent armors, infrared optical windows, missile windows, hood materials and the like, and has potential application value.
Compared with the prior art, the preparation method has the advantages of easily obtained raw materials, simple process, easily controlled material components, low cost and the like, and most importantly, the optical quality of a sample prepared by reaction sintering is greatly improved.
Drawings
FIG. 1 is a photograph of an aluminum oxynitride ceramic having a thickness of 4mm after double-side polishing treatment, which was obtained by the method described in example 1;
FIG. 2 is an XRD diffraction pattern of a sample prepared according to the method described in example 1;
FIG. 3 is a graph of the transmittance of a sample prepared according to the method described in example 1;
FIG. 4 is a cross-sectional microstructure of an aluminum oxynitride transparent ceramic produced by the method of example 1;
FIG. 5 is a photograph of an aluminum oxynitride ceramic having a thickness of 4mm after double-side polishing treatment, which was obtained by the method described in comparative example 1;
FIG. 6 is a cross-sectional microstructure of an aluminum oxynitride transparent ceramic prepared in comparative example 1;
FIG. 7 is a graph of the transmittance of a sample prepared according to the method described in comparative example 2;
fig. 8 is a sectional microstructure of the aluminum oxynitride transparent ceramic prepared in comparative example 2.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive.
In the present disclosure, AlN and Al are used2O3The raw material powder is B (OH)3Mg source (e.g., MgAl)2O4) And the rare earth oxide/rare earth composite oxide is used as a sintering aid and is prepared by mixing, molding and sintering. Wherein the rare earth oxide can be Y2O3、Lu2O3、Sc2O3At least one of them. The rare earth composite oxide is selected from Y3Al5O12Or/and Lu3Al5O12。
The preparation method of the aluminum oxynitride transparent ceramic has the advantages of simple process and easy and accurate control of ceramic components, and the aluminum oxynitride transparent ceramic with high visible light band transmittance is obtained by adopting the method. The following exemplarily illustrates a method for preparing the aluminum oxynitride transparent ceramic provided by the present invention.
Weighing AlN and Al according to the molar ratio of the sample required by the aluminum oxynitride transparent ceramic2O3Raw material powder, addition sinteringAnd the auxiliary agent is prepared by mixing the raw material powder by a ball milling method, drying and sieving the raw material powder to obtain mixed powder. Wherein the AlN has a purity of not less than 99.99% and a particle size of 0.5 to 1 μm (preferably 0.5 to 0.1 μm). Al (Al)2O3The purity of the product is more than or equal to 99.99 percent, and the particle size is 0.5-2 mu m. AlN and Al2O3The powder molar ratio can be (25-35) mol%: (75-65) mol%, and the sum of the two is 100 mol%. As an example, alumina, aluminum nitride and sintering aid are mixed by a ball milling method, and the specific steps are as follows: weighing AlN and Al2O3Adding sintering aid B (OH) into the powder3、MgAl2O4And Y3Al5O12/Y2O3/Lu3Al5O12/Lu2O3/Sc2O3(any one of the above materials) is prepared by ball milling and mixing the raw material powder with absolute ethyl alcohol as a dispersion medium and high-purity alumina balls as a ball milling medium, and then drying and sieving the mixture to obtain mixed powder. Wherein, the ball milling process can be 250 rpm for 20 hours. The drying conditions may be 60 ℃ for 24 hours. The screening process can be 100-mesh screening.
In alternative embodiments, the B (OH)3The addition amount of AlN and Al2O3(0.02-0.4) wt.% of the total mass of the raw material powder. MgAl2O4Can be added in AlN or Al2O3(0.02-0.5) wt.% of the total mass of the raw material powder. Rare earth oxide or/and rare earth composite oxide (e.g., Y)3Al5O12、Y2O3、Lu3Al5O12、Lu2O3、Sc2O3Etc.) may be added in amounts of AlN and Al2O3(0.05-0.1) wt.% of the total mass of the raw material powder. The B (OH)3、MgAl2O4、Y3Al5O12、Y2O3、Lu3Al5O12、Lu2O3、Sc2O3The purity of (A) is not less than 99.99%.
And (3) preparing the ceramic biscuit by dry pressing or/and cold isostatic pressing of the mixed powder. Preferably, the molding method is dry pressing combined cold isostatic pressing molding or powder is directly subjected to cold isostatic pressing molding. Wherein, the pressure of the dry pressing molding can be 10-20 MPa, and the pressure maintaining time can be 1-3 minutes. The pressure of the cold isostatic pressing treatment can be 150-250 MPa, and the pressure maintaining time is 3-5 minutes. As an example of the preparation of a ceramic biscuit, it comprises: (1) filling the treated mixed powder into a mold, and maintaining the pressure at normal temperature and 10-20 MPa for 1-3 minutes for molding; (2) and (3) carrying out cold isostatic pressing treatment on the biscuit subjected to dry pressing, wherein the pressure is 200MPa, and the pressure maintaining time is 3-5 minutes.
And placing the ceramic biscuit in a flowing nitrogen atmosphere for pressureless sintering to obtain the aluminum oxynitride transparent ceramic. The pressureless sintering temperature can be 1930-1980 ℃. The pressureless sintering time may be 20 to 30 hours, for example 30 hours. Preferably, the temperature rise rate of the pressureless sintering can be 5-10 ℃/min, such as 5 ℃/min. The flow rate of nitrogen gas may be 1-2L/min, for example, 1.5L/min.
And finally, further polishing the sintered aluminum oxynitride transparent ceramic. For example, double-side polishing treatment gives a 4 mm-thick aluminum oxynitride transparent ceramic. The obtained aluminum oxynitride transparent ceramic has high optical quality, and the transmittance of a sample (4mm thick) subjected to double-side polishing in a visible-infrared region can reach over 81 percent.
In the invention, the prepared aluminum oxynitride optical transparent ceramic has a uniform microstructure, no obvious air holes are seen, and the grain boundary bonding is tight. The prepared aluminum oxynitride optical transparent ceramic has high relative density (not less than 99.9%) and low porosity (less than 0.1%).
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Example 1: the technological process mainly comprises the steps of mixing, molding, sintering and the like
(1) Mixing materials: according to AlN to Al2O3AlN (purity > 99.9%, average particle size 0.8 μm) and Al were weighed in a molar ratio of 31:69, respectively2O3(purity of>99.99% and an average particle diameter of 0.52 μm). Addition of B (OH)3(purity > 99.99 percent) and MgAl2O4(purity > 99.99%) and Y2O3(purity > 99.99%) as sintering aid, wherein the addition amounts of the sintering aid are AlN and Al2O30.1 wt.%, 0.4 wt.%, 0.1 wt.% of the total mass of the raw material powder, using absolute ethyl alcohol as a dispersion medium, adopting a high-purity alumina ball milling tank, using high-purity alumina balls as a ball milling medium to ball mill and mix the mixed powder, performing ball milling and mixing for 20 hours under the condition of 250 revolutions per minute, placing the ball-milled slurry in an oven at 60 ℃ for drying for 24 hours, and then sieving by a 100-mesh sieve to obtain mixed powder;
(2) molding: loading the treated mixed powder into a mold, and molding by combining a dry pressing (10MPa, pressure maintaining for 1 minute) method with a cold isostatic pressing (200MPa, pressure maintaining for 3 minutes) method to obtain a ceramic biscuit;
(3) and (3) sintering: the shaped biscuit was placed in a crucible and heated to 1950 ℃ at a rate of 5 ℃/min under a flowing nitrogen atmosphere of 1.5L/min and then held for 30 hours.
The sintered sample was polished by a flat grinder and a polisher to obtain a sample having a thickness of 4mm as shown in FIG. 1. As shown in FIG. 1, the prepared aluminum oxynitride transparent ceramic material has good light transmittance in the visible light range.
The sample was tested by XRD as a single aluminum oxynitride phase, as shown in figure 2.
FIG. 3 is a graph showing transmittance curves of a transparent ceramic material having a thickness of 4mm obtained in example 1. As can be seen from fig. 3: the linear transmittance of the sample in a visible region can reach more than 81 percent at most, and is far more than the numerical value reported by preparing the aluminum oxynitride transparent ceramic by adopting a reaction sintering method in the prior art.
Fig. 4 is a cross-sectional microstructure of the sample. It can be seen from the figure that the microstructure of the aluminum oxynitride transparent ceramic prepared in example 1 is more compact and has no significant pores.
Example 2: the technological process mainly comprises the steps of mixing, molding, sintering and the like
(1) Mixing materials: according to AlN to Al2O3In a molar ratio of 35:65, AlN (purity > 99.9%, average particle diameter 0.8 μm) and Al were weighed out separately2O3(purity > 99.99%, average particle diameter 0.52 μm) powder. Addition of B (OH)3(purity > 99.99 percent) and MgAl2O4(purity > 99.99%) and Y2O3(purity > 99.99%) as sintering aid, wherein the addition amounts of the sintering aid are AlN and Al2O30.05 wt.%, 0.3 wt.%, 0.1 wt.% of the total mass of the raw material powder. Using absolute ethyl alcohol as a dispersion medium, adopting a high-purity alumina ball milling tank and high-purity alumina balls as a ball milling medium to ball mill and mix the mixed powder, carrying out ball milling and mixing for 20 hours under the condition of 250 revolutions per minute, drying the ball-milled slurry in an oven at 60 ℃ for 24 hours, and then sieving the dried slurry by a sieve of 100 ℃ to obtain mixed powder;
(2) molding: loading the treated mixed powder into a mold, and molding by combining a dry pressing (10MPa, pressure maintaining for 1 minute) method with a cold isostatic pressing (200MPa, pressure maintaining for 3 minutes) method to obtain a ceramic biscuit;
(3) and (3) sintering: the shaped biscuit was placed in a crucible and heated to 1970 ℃ at a heating rate of 5 ℃/min for 30 hours under a flowing nitrogen atmosphere of 1.5L/min.
And polishing the obtained sintered sample by using a surface grinder and a polishing machine to obtain a sample with the thickness of 4 mm. The linear transmittance of the obtained sample at a wavelength of 700nm was 79.3.
Examples 3 to 10
The preparation processes of examples 3 to 10 are the same as those of examples 1 and 2, except that: modification of AlN and Al2O3The composition of the sintering aid, the combination and the dosage of the sintering aid and the sintering temperature.
Table 1 details the raw material compositions, sintering aid combinations and amounts, the corresponding sintering temperatures, and the in-line transmittances at 700nm of the obtained samples of examples 3-10, and it can be seen that the samples of examples 3-10 all have higher optical qualities:
comparative example 1: the technological process mainly comprises the steps of mixing, molding, sintering and the like
(1) Mixing materials: according to AlN to Al2O3AlN (purity > 99.9%, average particle size 0.8 μm) and Al were weighed in a molar ratio of 31:69, respectively2O3(purity > 99.99%, average particle diameter 0.52 μm) powder. Using absolute ethyl alcohol as a dispersion medium, adopting a high-purity alumina ball milling tank and high-purity alumina balls as a ball milling medium to perform ball milling mixing on raw material powder, performing ball milling mixing for 20 hours under the condition of 250 revolutions per minute, drying the ball-milled slurry in an oven at 60 ℃ for 24 hours, and then sieving the dried slurry by a sieve of 100 meshes to obtain mixed powder;
(2) molding: loading the treated mixed powder into a mold, and molding by combining a dry pressing (10MPa, pressure maintaining for 1 minute) method with a cold isostatic pressing (200MPa, pressure maintaining for 3 minutes) method to obtain a ceramic biscuit;
(3) and (3) sintering: the shaped biscuit was placed in a crucible and heated to 1950 ℃ at a heating rate of 5 ℃/min under a flowing nitrogen atmosphere of 1.5L/min and then heat-preserved for 30 hours.
The sintered sample was polished by a flat grinder and a polisher to obtain a sample having a thickness of 4mm as shown in FIG. 5. As can be seen from fig. 5, the prepared aluminum oxynitride ceramic material is opaque.
Fig. 6 is a cross-sectional microstructure of the aluminum oxynitride ceramic prepared in comparative example 1. The aluminum oxynitride ceramic prepared in the comparative example 1 has more grain boundary pores in the crystal and the sample is opaque.
Comparative example 2: the technological process mainly comprises the steps of mixing, molding, sintering and the like
(1) Mixing materials: according to AlN to Al2O3AlN (purity > 99.9%, average particle size 0.8 μm) and Al were weighed in a molar ratio of 31:69, respectively2O3(purity > 99.99%, average particle diameter 0.52 μm) powder. Adding MgAl2O4(purity > 99.99%) and Y2O3(purity > 99.99%) as sintering aid, wherein the addition amounts of the sintering aid are AlN and Al2O30.4 wt.% and 0.1 wt.% of the total mass of the raw material powder. Using absolute ethyl alcohol as a dispersion medium, adopting a high-purity alumina ball milling tank and high-purity alumina balls as a ball milling medium to ball mill and mix the mixed powder, carrying out ball milling and mixing for 20 hours under the condition of 250 revolutions per minute, drying the ball-milled slurry in an oven at 60 ℃ for 24 hours, and then sieving the dried slurry by a sieve of 100 ℃ to obtain mixed powder;
(2) molding: loading the treated mixed powder into a mold, and molding by combining a dry pressing (10MPa, pressure maintaining for 1 minute) method with a cold isostatic pressing (200MPa, pressure maintaining for 3 minutes) method to obtain a ceramic biscuit;
(3) and (3) sintering: the shaped biscuit was placed in a crucible and heated to 1950 ℃ at a heating rate of 5 ℃/min under a flowing nitrogen atmosphere of 1.5L/min and then heat-preserved for 30 hours.
And polishing the obtained sintered sample by using a surface grinder and a polishing machine to obtain an aluminum oxynitride ceramic sample with the thickness of 4 mm. FIG. 7 is a graph showing transmittance of a transparent ceramic material having a thickness of 4mm obtained in comparative example 2, and the in-line transmittance at 700nm of visible light is 57%.
Fig. 8 shows a cross-sectional microstructure of the aluminum oxynitride ceramic prepared in comparative example 2, which indicates that grain boundaries in the aluminum oxynitride ceramic prepared in comparative example 2 have pore distribution, and that many small pores are present in the grain boundaries, the density is 99.8%, and the porosity is 0.2%.
Claims (11)
1. A preparation method of aluminum oxynitride transparent ceramic is characterized in that AlN powder and Al are adopted2O3The powder is used as raw material and adopts B (OH)3Mg source and rare earth source as sintering aids, and mixing, molding and sintering to obtain the aluminum oxynitrideBright ceramics; the AlN powder and Al2O3The molar ratio of the powder (25-35): (75-65); the Mg source is MgAl2O4(ii) a The rare earth source is selected from Y3Al5O12、Y2O3、Lu3Al5O12、Lu2O3And Sc2O3At least one of; the Mg source is added with AlN powder and Al2O3(0.02-0.5) wt.% of the total mass of the powder; the B (OH)3The adding amount of the aluminum nitride powder and the Al2O3(0.02-0.5) wt.% of the total mass of the powder; the addition amount of the rare earth source is AlN powder and Al2O3(0.02-0.1) wt.% of the total mass of the powder;
the density of the aluminum oxynitride transparent ceramic is more than or equal to 99.9%, the porosity is less than 0.1%, and the linear transmittance at 700nm is 75-83%.
2. The method according to claim 1, wherein B (OH)3The adding amount of the aluminum nitride powder and the Al2O3(0.02-0.4) wt.% of the total mass of the powder; the addition amount of the rare earth source is AlN powder and Al2O3(0.05-0.1) wt.% of the total mass of the powder.
3. The preparation method according to claim 1, wherein the AlN powder has a purity of not less than 99.99% and a particle size of 0.5 to 1 μm; the Al is2O3The purity of the powder is more than or equal to 99.99%, and the particle size is 0.5-2 μm.
4. The method according to claim 1, wherein B (OH)3The purity of the product is not lower than 99.99 percent; the purity of the Mg source is not lower than 99.99%; the purity of the rare earth source is not less than 99.99%.
5. The method of claim 1, wherein the mixing is performed by ball milling; the rotation speed of ball milling mixing is 200-300 r/min, and the time is 15-48 hours.
6. The method of claim 5, wherein the ball milling is performed at a speed of 250 rpm for 20 hours.
7. The production method according to any one of claims 1 to 6, wherein the molding method is dry press molding or/and cold isostatic press molding; the pressure of the dry pressing is 10-20 MPa, and the pressure maintaining time is 1-3 minutes; the pressure of the cold isostatic pressing treatment is 150-250 MPa, and the pressure maintaining time is 3-5 minutes.
8. The method according to any one of claims 1 to 6, wherein the sintering atmosphere is a flowing nitrogen atmosphere, and the temperature is 1930 to 1980 ℃ for 20 to 30 hours.
9. The method according to claim 8, wherein the nitrogen gas atmosphere is nitrogen gas flowing at a flow rate of 1 to 2L/min.
10. The method according to claim 9, wherein the nitrogen atmosphere is nitrogen gas flowing at a flow rate of 1.5L/min.
11. The aluminum oxynitride transparent ceramic prepared by the preparation method according to any one of claims 1 to 10, wherein the aluminum oxynitride transparent ceramic has a density of 99.9% or more, a porosity of less than 0.1%, and a linear transmittance at 700nm of 75 to 83%.
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