CN109053192B - Preparation method of MgAlON transparent ceramic powder - Google Patents
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Abstract
A preparation method of MgAlON transparent ceramic powder comprises the following steps: (1) weighing raw materials: weighing Al powder, gamma-Al 2O3 powder and MgO powder according to a certain proportion to obtain mixed powder for later use; (2) ball milling and dispersing: dispersing the mixed powder obtained in the step (1) in absolute ethyl alcohol, and performing ball milling to obtain slurry; (3) drying the slurry: drying the slurry obtained in the step (2) to obtain dry powder; (4) reaction synthesis: and (4) putting the dried powder obtained in the step (3) into a crucible, putting the crucible and the dried powder into a high-temperature sintering furnace, introducing flowing nitrogen, heating to 1500-1700 ℃ at the heating rate of 5-15 ℃/min, preserving the heat for 1-3 h, and naturally cooling to obtain the MgAlON transparent ceramic powder. The MgAlON transparent ceramic powder prepared by the method has high purity and fine granularity, and is suitable for preparing transparent ceramics.
Description
Technical Field
The invention relates to a preparation method of MgAlON transparent ceramic powder, belonging to the field of optical materials.
Background
MgAlON is a material for stabilizing AlON structure by MgO, and the MgAlON transparent ceramic manufactured into a block is a new material with structure and function integration and has the functions of being combined with AlON and MgAl2O4And the like of typical spinel-structured ceramics, such as: wide electromagnetic wave transmission range (0.2-6.5 microns), optical isotropy, excellent mechanical properties (high bending strength and high hardness), and the like, and is expected to be applied to the fields of infrared windows, antenna covers, detector optical windows, transparent armor, and the like.
There are two main methods reported for the preparation of this material: one is a reaction sintering method, in which AlN (or Al or N) is usually used2)、Al2O3MgO is used as a raw material, and MgAlON transparent ceramic is obtained in one step by reaction sintering after mixing, so that the method can also be called a one-step method (J.Eur.Ceram.Soc,15(2015) 249-254); secondly, MgAlON powder is firstly synthesized and then sintered to obtain MgAlON transparent ceramics, which is also called a two-step method, and reference can be made to Liu et al (J.Am.Ceram.Soc,97(2014), 63-66). The main technical difficulties of the reaction sintering method (one-step method) are that: the sintering and the reaction are usually carried out synchronously, the process is complex, and a second phase is easy to generate; furthermore, there is a problem with the reaction of such materials in that volume expansion generates secondary air holes, which can have a serious impact on optical performance. In contrast, the two-step process does not suffer from these problems and is thus a gainThe optimization method of the MgAlON transparent ceramic has better comprehensive performance in the aspects of large-size preparation, optical transmission performance and the like of the MgAlON transparent ceramic.
The premise of the two-step method is to prepare the MgAlON transparent ceramic powder with high performance. Currently, the preparation method of the MgAlON transparent ceramic powder mainly includes: (1) with AlN and Al2O3MgO is used as a raw material and is obtained by a solid phase reaction method (refer to patent CN 200910272607.4); (2) at C, Al2O3、N2MgO is used as a raw material and is obtained by carbothermal reduction nitridation reaction (refer to ceramics. Inter.,44(2018), 4512-4515). The two methods are the main methods for obtaining the MgAlON transparent ceramic powder at present. Sintering and densifying the obtained MgAlON transparent ceramic powder to obtain the MgAlON transparent ceramic. It is worth mentioning that the solid-phase reaction method has high preparation cost due to the high market price of the AlN raw material; the carbothermic reduction method adopts C as a raw material, so that residual C in the product is difficult to remove, the subsequent link usually needs to be calcined in air or oxygen, and the oxidation of MgAlON is difficult to avoid although a part of residual C can be removed.
In view of the above-mentioned problems of the two methods in the preparation of MgAlON transparent ceramic powder, there is a report in the literature that a direct nitriding method (also referred to as Al thermal reduction method) is proposed. Al has a lower melting point and can be nitrided at a lower temperature. For example, Su et Al (J.Eur.Ceram.Soc,35(2015),1173-2、Al2O3AlON powder is synthesized by a direct nitridation method of raw materials, and the AlON transparent ceramic with excellent optical transmission performance is prepared by adopting the powder obtained by the method for the first time. For another example, Yan et al (ceramic. int.44(2018), 3856-.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of MgAlON transparent ceramic powder, which has the advantages of low raw material cost, high purity of synthesized powder, low C content and excellent optical transmission performance.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of MgAlON transparent ceramic powder comprises the following steps:
(1) weighing raw materials: weighing Al powder and gamma-Al according to a certain proportion2O3Mixing the powder and MgO powder to obtain mixed powder for later use;
the proportions are as follows: al powder, gamma-Al2O3The weight percentages of the powder and the MgO powder are respectively 4wt% -9 wt%, 78wt% -88 wt% and 7wt% -16 wt%;
(2) ball milling and dispersing: dispersing the mixed powder obtained in the step (1) in absolute ethyl alcohol, and performing ball milling to obtain slurry;
(3) drying the slurry: drying the slurry obtained in the step (2) to obtain dry powder;
(4) reaction synthesis: and (4) putting the dried powder obtained in the step (3) into a crucible, putting the crucible and the dried powder into a high-temperature sintering furnace, introducing flowing nitrogen, heating to 1500-1700 ℃ at the heating rate of 5-15 ℃/min, preserving the heat for 1-3 h, and naturally cooling to obtain the MgAlON transparent ceramic powder.
Further, in the step (1), the average granularity of the Al powder is less than or equal to 2.5 mu m, and the purity is more than or equal to 99 wt%; gamma-Al2O3The average particle size of the powder is less than or equal to 100nm, and the purity is more than or equal to 99.5 wt%; the average granularity of MgO powder is less than or equal to 100nm, and the purity is more than or equal to 99.5 wt%.
Further, in the step (2), the ball milling rotating speed is 60 r-120 r/m; the ball milling time is more than or equal to 16 h.
Further, in the step (2), the grinding balls selected for ball milling are alumina balls or zirconia balls, and the purity is more than or equal to 99 wt%;
further, in the step (2), the mass ratio of the grinding balls to the mixed powder is 5: 1-10: 1.
Further, in the step (3), in order to avoid the oxidation of Al powder in the raw materials as much as possible, the slurry is placed in a vacuum chamber (the air pressure is not higher than 20Pa), and the drying temperature is not lower than 60 ℃, so that the absolute ethyl alcohol in the slurry is fully volatilized.
Further, in the step (4), the crucible is an alumina or boron nitride crucible, and the purity is more than or equal to 97 wt%;
further, in the step (4), the flowing nitrogen has an absolute value of air pressure of 0.1MPa to 0.3MPa, a purity of not less than 99.99vol% and a flow rate of 0.1L to 1.0L/min.
The invention has the beneficial effects that:
1) under the conditions that expensive AlN powder or C powder which has high melting point and is difficult to completely remove is not selected, Al powder which has low price and low melting point is selected as a raw material, and MgAlON powder can be obtained by a direct nitriding method, and the MgAlON powder has low cost of raw materials, high purity of synthesized powder and low content of C and is very suitable for popularization and application;
2) the obtained MgAlON powder can be used for preparing transparent MgAlON ceramics, has excellent optical transmission performance and provides a new method for preparing the materials.
Drawings
FIG. 1 is an XRD spectrum of MgAlON powder synthesized in examples 1, 3 and 5 of the present invention;
FIG. 2 is a transmittance curve of MgAlON transparent ceramic prepared from MgAlON powder synthesized in example 3 of the present invention.
Detailed Description
For a better understanding of the present invention, the contents of the present invention will be further explained below with reference to the drawings and examples, but the contents of the present invention are not limited to the following examples.
Example 1
A preparation method of MgAlON transparent ceramic powder comprises the following steps:
(1) weighing raw materials: weighing Al powder and gamma-Al according to a certain proportion2O3Mixing the powder and MgO powder to obtain mixed powder for later use;
the proportions are as follows: al powder, gamma-Al2O3The mass fractions of the powder and the MgO powder are respectively 4wt%, 80 wt% and 16 wt%;
the average granularity of the Al powder is 2.5 mu m, and the purity is 99.95 wt%; gamma-Al2O3The average particle size of the powder is 20nm, and the purity is 99.5wtPercent; the average granularity of MgO powder is 100nm, and the purity is 99.99 wt%;
(2) ball milling and dispersing: dispersing the mixed powder obtained in the step (1) in absolute ethyl alcohol, and carrying out ball milling for 16h to obtain slurry;
the ball milling speed is 120 r/m; the grinding balls selected for ball milling are alumina balls, and the purity is 99 wt%; the mass ratio of the grinding ball to the mixed powder is 5: 1;
(3) drying the slurry: drying the slurry obtained in the step (2) to obtain dry powder;
in order to avoid the oxidation of Al powder in the raw materials as much as possible, the slurry is placed in a vacuum chamber (the air pressure is 20Pa), the drying temperature is 60 ℃, and the drying time is 4 hours;
(4) reaction synthesis: putting the dried powder obtained in the step (3) into a crucible, putting the crucible and the dried powder into a high-temperature sintering furnace, introducing flowing nitrogen, heating to 1500 ℃ at the heating rate of 5 ℃/min, preserving the heat for 3 hours, and naturally cooling to obtain MgAlON transparent ceramic powder;
the crucible is an alumina crucible, and the purity is 97 wt%;
the flowing nitrogen has the absolute value of air pressure of 0.1MPa, the purity of 99.99vol% and the flow rate of 0.1L/min.
Example 2
A preparation method of MgAlON transparent ceramic powder comprises the following steps:
(1) weighing raw materials: weighing Al powder and gamma-Al according to a certain proportion2O3Mixing the powder and MgO powder to obtain mixed powder for later use;
the proportions are as follows: al powder, gamma-Al2O3The mass fractions of the powder and the MgO powder are respectively 5wt%, 88wt% and 7 wt%;
the average granularity of the Al powder is 2.5 mu m, and the purity is 99.5 wt%; gamma-Al2O3The average particle size of the powder is 20nm, and the purity is 99.99 wt%; the average granularity of MgO powder is 100nm, and the purity is 99.5 wt%;
(2) ball milling and dispersing: dispersing the mixed powder obtained in the step (1) in absolute ethyl alcohol, and carrying out ball milling for 18h to obtain slurry;
the ball milling speed is 100 r/m; the grinding balls selected for ball milling are zirconia balls, and the purity is 99 wt%; the mass ratio of the grinding ball to the mixed powder is 5: 1;
(3) drying the slurry: drying the slurry obtained in the step (2) to obtain dry powder;
in order to avoid the oxidation of Al powder in the raw materials as much as possible, the slurry is placed in a vacuum chamber (the air pressure is 20Pa), the drying temperature is 60 ℃, and the drying time is 10 hours;
(4) reaction synthesis: putting the dried powder obtained in the step (3) into a crucible, putting the crucible and the dried powder into a high-temperature sintering furnace, introducing flowing nitrogen, heating to 1550 ℃ at a heating rate of 15 ℃/min, preserving heat for 2.5h, and naturally cooling to obtain MgAlON transparent ceramic powder;
the crucible is a boron nitride crucible, and the purity is 97 wt%;
the flowing nitrogen has the absolute value of air pressure of 0.3MPa, the purity of 99.99wt percent and the flow rate of 0.3L/min.
Example 3
A preparation method of MgAlON transparent ceramic powder comprises the following steps:
(1) weighing raw materials: weighing Al powder and gamma-Al according to a certain proportion2O3Mixing the powder and MgO powder to obtain mixed powder for later use;
the proportions are as follows: al powder, gamma-Al2O3The mass fractions of the powder and the MgO powder are respectively 6wt%, 82 wt% and 12 wt%;
the average granularity of the Al powder is 2 mu m, and the purity is 99.9 wt%; gamma-Al2O3The average particle size of the powder is 50nm, and the purity is 99.99 wt%; the average granularity of MgO powder is 70nm, and the purity is 99.5 wt%;
(2) ball milling and dispersing: dispersing the mixed powder obtained in the step (1) in absolute ethyl alcohol, and performing ball milling for 20 hours to obtain slurry;
the ball milling speed is 100 r/m; the grinding balls selected for ball milling are alumina balls, and the purity is 99.9 wt%; the mass ratio of the grinding ball to the mixed powder is 8: 1;
(3) drying the slurry: drying the slurry obtained in the step (2) to obtain dry powder;
in order to avoid the oxidation of Al powder in the raw materials as much as possible, the slurry is placed in a vacuum chamber (the air pressure is 10Pa), the drying temperature is 70 ℃, and the drying time is 8 hours;
(4) reaction synthesis: putting the dried powder obtained in the step (3) into a crucible, putting the crucible and the dried powder into a high-temperature sintering furnace, introducing flowing nitrogen, heating to 1600 ℃ at a heating rate of 10 ℃/min, preserving the heat for 2 hours, and naturally cooling to obtain MgAlON transparent ceramic powder;
the crucible is an alumina crucible, and the purity is 98 wt%;
the flowing nitrogen has the absolute value of air pressure of 0.2MPa, the purity of 99.995 vol% and the flow rate of 0.5L/min.
Example 4
A preparation method of MgAlON transparent ceramic powder comprises the following steps:
(1) weighing raw materials: weighing Al powder and gamma-Al according to a certain proportion2O3Mixing the powder and MgO powder to obtain mixed powder for later use;
the proportions are as follows: al powder, gamma-Al2O3The mass fractions of the powder and the MgO powder are respectively 7wt%, 83 wt% and 10 wt%;
the average granularity of the Al powder is 1.5 mu m, and the purity is 99.5 wt%; gamma-Al2O3The average particle size of the powder is 50nm, and the purity is 99.5 wt%; the average granularity of MgO powder is 70nm, and the purity is 99.99 wt%;
(2) ball milling and dispersing: dispersing the mixed powder obtained in the step (1) in absolute ethyl alcohol, and performing ball milling for 20 hours to obtain slurry;
the ball milling speed is 80 r/m; the grinding balls selected for ball milling are zirconia balls, and the purity is 99.9 wt%; the mass ratio of the grinding ball to the mixed powder is 8: 1;
(3) drying the slurry: drying the slurry obtained in the step (2) to obtain dry powder;
in order to avoid the oxidation of Al powder in the raw materials as much as possible, the slurry is placed in a vacuum chamber (the air pressure is 10Pa), the drying temperature is 70 ℃, and the drying time is 8 hours;
(4) reaction synthesis: putting the dried powder obtained in the step (3) into a crucible, putting the crucible and the dried powder into a high-temperature sintering furnace, introducing flowing nitrogen, heating to 1600 ℃ at a heating rate of 10 ℃/min, preserving the heat for 2 hours, and naturally cooling to obtain MgAlON transparent ceramic powder;
the crucible is a boron nitride crucible with the purity of 98 wt%;
the flowing nitrogen has the absolute value of air pressure of 0.2MPa, the purity of 99.995 vol% and the flow rate of 0.7L/min.
Example 5
A preparation method of MgAlON transparent ceramic powder comprises the following steps:
(1) weighing raw materials: weighing Al powder and gamma-Al according to a certain proportion2O3Mixing the powder and MgO powder to obtain mixed powder for later use;
the proportions are as follows: al powder, gamma-Al2O3The mass fractions of the powder and the MgO powder are respectively 8wt%, 85 wt% and 7 wt%;
the average granularity of the Al powder is 1 mu m, and the purity is 99 wt%; gamma-Al2O3The average granularity of the powder is 80nm, and the purity is 99.5 wt%; the average granularity of MgO powder is 40nm, and the purity is 99.99 wt%;
(2) ball milling and dispersing: dispersing the mixed powder obtained in the step (1) in absolute ethyl alcohol, and performing ball milling for 24 hours to obtain slurry;
the ball milling speed is 60 r/m; the grinding balls selected for ball milling are alumina balls, and the purity is 99.99 wt%; the mass ratio of the grinding ball to the mixed powder is 10: 1;
(3) drying the slurry: drying the slurry obtained in the step (2) to obtain dry powder;
in order to avoid the oxidation of Al powder in the raw materials as much as possible, the slurry is placed in a vacuum chamber (the air pressure is 5Pa), the drying temperature is 80 ℃, and the drying time is 4 hours;
(4) reaction synthesis: putting the dried powder obtained in the step (3) into a crucible, putting the crucible and the dried powder into a high-temperature sintering furnace, introducing flowing nitrogen, heating to 1700 ℃ at the heating rate of 5 ℃/min, preserving heat for 1h, and naturally cooling to obtain MgAlON transparent ceramic powder;
the crucible is an alumina crucible, and the purity is 99.5 wt%;
the flowing nitrogen has the absolute value of air pressure of 0.1MPa, the purity of 99.999vol percent and the flow rate of 1.0L/min.
Example 6
A preparation method of MgAlON transparent ceramic powder is characterized by comprising the following steps:
(1) weighing raw materials: weighing Al powder and gamma-Al according to a certain proportion2O3Mixing the powder and MgO powder to obtain mixed powder for later use;
the proportions are as follows: al powder, gamma-Al2O3The mass fractions of the powder and the MgO powder are respectively 9wt%, 78wt% and 13 wt%;
the average granularity of the Al powder is 1 mu m, and the purity is 99.95 wt%; gamma-Al2O3The average granularity of the powder is 100nm, and the purity is 99.99 wt%; the average granularity of MgO powder is 40nm, and the purity is 99.5 wt%;
(2) ball milling and dispersing: dispersing the mixed powder obtained in the step (1) in absolute ethyl alcohol, and performing ball milling for 24 hours to obtain slurry;
the ball milling speed is 60 r/m; the grinding balls selected for ball milling are zirconia balls, and the purity is 99.99 wt%; the mass ratio of the grinding ball to the mixed powder is 10: 1;
(3) drying the slurry: drying the slurry sample obtained in the step (2) to obtain dry powder;
in order to avoid the oxidation of Al powder in the raw materials as much as possible, the slurry is placed in a vacuum chamber (the air pressure is 5Pa), the drying temperature is 80 ℃, and the drying time is 10 hours;
(4) reaction synthesis: putting the dried powder sample obtained in the step (3) into a crucible, putting the crucible and the dried powder sample into a high-temperature sintering furnace, introducing flowing nitrogen, heating to 1700 ℃ at the heating rate of 15 ℃/min, preserving heat for 3h, and naturally cooling to obtain MgAlON transparent ceramic powder;
the crucible is a boron nitride crucible with the purity of 99.5 wt%;
the flowing nitrogen has the absolute value of air pressure of 0.3MPa, the purity of 99.999vol percent and the flow rate of 1.0L/min.
The XRD spectrum of the MgAlON powder synthesized in the above examples 1, 3 and 5 is shown in fig. 1, and according to the XRD spectrum, it can be judged that the synthesized product is MgAlON single-phase material and has no other obvious residual phase.
The phase purity, carbon content, and average particle size of the MgAlON powders synthesized in examples 1-6 above are shown in Table 1.
TABLE 1
As can be seen from Table 1, the MgAlON powder obtained in the embodiment has high purity (not less than 99.5%) and extremely low carbon content (31 ppm-60 ppm); the granularity is very fine (below 1000 nm), the powder performance is excellent, and the method is suitable for preparing transparent ceramics.
The transmittance curve of the MgAlON transparent ceramic prepared from the MgAlON powder synthesized in example 3 is shown in fig. 2, and the transparent ceramic prepared from MgAlON has a wide light transmission range covering the ultraviolet-visible light-laser-near infrared band (0.2 μm to 2.0 μm), and has high optical transmittance, such as transmittances of about 75%, 77%, and 80% at 0.4 μm, 1.0 μm, and 2.0 μm, respectively, and excellent optical transmittance.
Claims (6)
1. A preparation method of MgAlON transparent ceramic powder is characterized by comprising the following steps:
(1) weighing raw materials: weighing Al powder and gamma-Al according to a certain proportion2O3Mixing the powder and MgO powder to obtain mixed powder for later use;
the proportions are as follows: al powder, gamma-Al2O3The weight percentages of the powder and the MgO powder are respectively 4wt% -9 wt%, 78wt% -88 wt% and 7wt% -16 wt%;
(2) ball milling and dispersing: dispersing the mixed powder obtained in the step (1) in absolute ethyl alcohol, and performing ball milling to obtain slurry;
(3) drying the slurry: drying the slurry obtained in the step (2) to obtain dry powder;
(4) reaction synthesis: putting the dried powder obtained in the step (3) into a crucible, putting the crucible and the dried powder into a high-temperature sintering furnace, introducing flowing nitrogen, heating to 1500-1700 ℃ at the heating rate of 5-15 ℃/min, preserving the heat for 1-3 h, and naturally cooling to obtain MgAlON transparent ceramic powder; in the step (1), the average granularity of the Al powder is less than or equal to 2.5 mu m, and the purity is more than or equal to 99 wt%; gamma-Al2O3The average particle size of the powder is less than or equal to 100nm, and the purity is more than or equal to 99.5 wt%; average particle of MgO powderThe degree is less than or equal to 100nm, and the purity is more than or equal to 99.5 wt%; in the step (4), the flowing nitrogen has an absolute value of air pressure of 0.1-0.3 MPa, a purity of not less than 99.99vol% and a flow rate of 0.1-1.0L/min.
2. The preparation method of MgAlON transparent ceramic powder according to claim 1, wherein in the step (2), the ball milling rotation speed is 60 r-120 r/m; the ball milling time is more than or equal to 16 h.
3. The preparation method of MgAlON transparent ceramic powder according to claim 1 or 2, wherein in the step (2), the grinding balls selected by ball milling are alumina balls or zirconia balls, and the purity is not less than 99 wt%.
4. The preparation method of MgAlON transparent ceramic powder according to claim 1 or 2, wherein in the step (2), the mass ratio of the grinding balls to the mixed powder is 5: 1-10: 1.
5. The method for preparing MgAlON transparent ceramic powder according to claim 1 or 2, wherein in the step (3), in order to avoid oxidation of Al powder in the raw material as much as possible, the slurry is placed in a vacuum chamber, the air pressure is not higher than 20Pa, the drying temperature is not lower than 60 ℃, and the anhydrous ethanol in the slurry is fully volatilized.
6. The preparation method of MgAlON transparent ceramic powder according to claim 1 or 2, wherein in the step (4), the crucible is an alumina or boron nitride crucible with purity not less than 97 wt%.
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