CN110817815B - Preparation method of high-purity aluminum nitride with controllable particle size distribution - Google Patents
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Abstract
A preparation method of high-purity aluminum nitride with controllable particle size distribution, which relates to the technical field of preparation of high-melting-point nitride powder. The method comprises the steps of preparing industrial-grade aluminum ingots to obtain aluminum powder, pretreating the aluminum powder, preparing aluminum nitride by a chemical vapor deposition method, and finally grinding and grading to obtain high-purity aluminum nitride. The invention realizes the preparation of the high-purity aluminum nitride powder, has the advantages of simple and convenient process, low cost, uniform particle size distribution of the product, high product purity and the like, and can be used for large-scale production. The aluminum powder prepared by using the industrial-grade aluminum ingot is irregular in shape, has a large specific surface area and is high in chemical activity. It is necessary to pretreat the aluminum nitride prior to its preparation. After pretreatment, a layer of coating is formed on the surface of the aluminum powder, so that the aluminum powder can be effectively protected. The nitriding reduction reaction is completed in an inert atmosphere, the influence of oxygen or air on the reaction process can be completely eliminated, and the sufficient amount of the ammonia-hydrogen chloride mixed gas enables the metal aluminum powder to be completely reacted.
Description
Technical Field
The invention relates to the technical field of preparation of high-melting-point nitride powder, in particular to a preparation method of high-purity aluminum nitride with controllable particle size distribution.
Background
Nitride powders having high melting point, high hardness, high chemical stability, and excellent electrical and optical properties have attracted general attention. The unique physical and chemical properties make the nitride have wide application in the fields of semiconductor devices, microelectronics, porous ceramics and the like.
The aluminum nitride can be used in polymer resin, has no obvious adhesion, and is the best high-thermal-conductivity insulating filler at present. The nano aluminum nitride is diamond-like nitride, can be stabilized to 2200 ℃ at most, has high room temperature strength, and has slower strength reduction along with the temperature rise; the nanometer aluminum nitride powder has good heat conductivity, small thermal expansion coefficient and heat conductivityThe theoretical value is 320w/mk, and the insulation is high, and the resistivity is 1015The material can resist the high temperature of 1400 ℃, can greatly improve the thermal conductivity of plastics and silicon rubber, is a good thermal shock resistant material, has strong capability of resisting molten metal erosion, and is an ideal crucible material for casting pure iron, aluminum or aluminum alloy; the nano aluminum nitride has excellent electrical insulation and good dielectric property; the nano aluminum nitride has good injection molding performance; the composite material is used for composite materials, has good matching property with semiconductor silicon and good interface compatibility, and can improve the mechanical property and the heat conduction dielectric property of the composite material.
At present, the conventional methods for synthesizing nitrides, such as solid-phase reaction synthesis and gas-phase reaction synthesis, are mainly used for preparing aluminum nitride powder, and the reduction nitridation method and the Chemical Vapor Deposition (CVD) method are commonly used for preparing aluminum nitride powder. The reduction nitridation method uses ammonia gas and metal oxide as main raw materials to prepare nitride powder. Chemical Vapor Deposition (CVD) is carried out by reacting a metal and a volatile compound (halide or alkyl compound) of the metal with N2Atmosphere is introduced into the reaction chamber with NH3The reaction deposits the crystal grains of the nitride from the gas phase, and then the crystal grains are aggregated into nitride powder. However, the aluminum nitride powder prepared by the above method has many disadvantages and defects, such as the need to prepare a precursor of a reactant with a suitable size and structure, low purity of the powder obtained by the reaction, and easy generation of environmental problems.
Disclosure of Invention
Aiming at the defects of impure products, difficult reaction control, uneven particle size distribution and the like in the preparation of the aluminum nitride powder, the invention provides the preparation method of the high-purity aluminum nitride with controllable particle size distribution, which has the advantages of simple and convenient operation, controllable particle size distribution of the products, higher purity and the like, and provides a simple and efficient method for preparing the aluminum nitride powder.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of high-purity aluminum nitride with controllable grain size distribution utilizes industrial-grade aluminum ingots to prepare and obtain aluminum powder, the aluminum powder is pretreated, aluminum nitride is prepared by a chemical vapor deposition method, and finally the high-purity aluminum nitride is obtained by grinding and grading.
As a preferred technical scheme of the invention, the steps of preparing and obtaining the aluminum powder by using the industrial-grade aluminum ingot are as follows:
melting an industrial-grade aluminum ingot, atomizing by an atomizer under the protection of nitrogen to prepare powder, spraying superfine oil mist into the atomizer, separating by a cyclone separator to obtain oil-containing aluminum powder, and finally performing solid-liquid separation and drying to obtain the aluminum powder.
As a preferred technical scheme of the invention, the step of pretreating the aluminum powder comprises the following steps:
firstly, adding absolute ethyl alcohol into aluminum powder, and performing ultrasonic dispersion; the adding weight ratio of the aluminum powder to the absolute ethyl alcohol is 1: 10-20; then adding a silane coupling agent KH550 and methyl benzoate, heating to 50-70 ℃, stirring and reacting for 1-3 hours; wherein the adding weight ratio of the aluminum powder, the silane coupling agent KH550 and the methyl benzoate is 1: 1: 1; standing and aging for 12-24 h after the reaction is finished, and drying after solid-liquid separation to obtain the pretreated aluminum powder.
As a preferred technical scheme of the invention, the step of preparing the aluminum nitride by the chemical vapor deposition method comprises the following steps:
the reactor is divided into a heating area, a high-temperature area and a cooling area, wherein the temperatures of the heating area and the high-temperature area are respectively as follows: 200-300 ℃ and 600-800 ℃; continuously introducing argon into the heating area, the high-temperature area and the cooling area, and simultaneously introducing ammonia gas and hydrogen chloride gas into the high-temperature area; enabling aluminum powder to enter a heating area of the reactor through automatic feeding equipment, staying for 1-5 minutes, then continuing to advance to a high-temperature area, staying for 5-15 minutes, and then leaving the high-temperature area to enter a cooling area for cooling; and after the temperature is reduced to the room temperature, the aluminum nitride powder is obtained after entering a finished product box.
Further, the volume ratio of ammonia gas to hydrogen chloride in the high temperature zone is 2: 1.
further, the weight ratio of the total weight of the ammonia gas and the hydrogen chloride to the aluminum powder is 5: 1.
further, the ammonia gas and the hydrogen chloride in the high-temperature zone are both gaseous, and the purity of the ammonia gas and the purity of the hydrogen chloride in the high-temperature zone are 99.99%.
As a preferred technical scheme of the invention, the step of obtaining the high-purity aluminum nitride by grinding and grading comprises the following steps:
adding aluminum nitride powder into a grinding machine, and adding a grinding ball, a solvent and a grinding aid; firstly, controlling a stirring shaft of a stirring mill to keep high-speed rotation in the same direction for 5-10 minutes to generate violent collision between materials, then changing the rotation direction of the stirring shaft, reversely rotating for 15-30 minutes at high speed to further grind aluminum nitride powder, and finally grading to obtain the high-purity aluminum nitride with controllable particle size distribution.
Further, the solvent and the grinding aid added in the grinding machine are respectively ethanol and quartz sand.
Further, the weight ratio of the material balls in the grinding machine is 1: 3, the weight ratio of the aluminum nitride powder, the solvent and the grinding aid is 1: 3: 2.
compared with the prior art, the invention has the beneficial effects that:
1) the method realizes the preparation of the high-purity aluminum nitride powder, has the advantages of simple and convenient process, low cost, uniform particle size distribution of the product, high product purity and the like, and can be used for large-scale production.
2) The aluminum powder prepared from the industrial-grade aluminum ingot is irregular in shape, has a large specific surface area and is high in chemical activity. It is necessary to pretreat it prior to preparing the aluminum nitride. After pretreatment, a layer of coating is formed on the surface of the aluminum powder, so that the aluminum powder can be effectively protected. Meanwhile, the protective film can disappear after being heated in a heating area of subsequent reaction, so that the aim of temporarily protecting the aluminum powder is fulfilled. The nitriding reduction reaction is completed in an inert atmosphere, the influence of oxygen or air on the reaction process can be completely eliminated, and the sufficient amount of the ammonia-hydrogen chloride mixed gas enables the metal aluminum powder to be completely reacted.
Drawings
FIG. 1 is an SEM image of the preparation of aluminum powder;
FIG. 2 is an XRD pattern (a) and an SEM pattern (b) before polishing for preparing aluminum nitride;
FIG. 3 is an SEM image of the prepared aluminum nitride after polishing (a, b correspond to low and high magnification, respectively).
Detailed Description
The invention provides a preparation method of high-purity aluminum nitride with controllable particle size distribution. The steps are respectively as follows:
firstly, the steps of preparing and obtaining aluminum powder by using an industrial-grade aluminum ingot are as follows:
melting an industrial-grade aluminum ingot, atomizing by an atomizer under the protection of nitrogen to prepare powder, spraying superfine oil mist into the atomizer, separating by a cyclone separator to obtain oil-containing aluminum powder, and finally performing solid-liquid separation and drying to obtain the aluminum powder. The SEM image of the aluminum powder is shown in fig. 1, and it can be seen from fig. 1 that the aluminum powder has an irregular shape, a large specific surface area, and high chemical activity.
Secondly, the aluminum powder is pretreated by the following steps:
firstly, adding absolute ethyl alcohol into aluminum powder, and performing ultrasonic dispersion; the adding weight ratio of the aluminum powder to the absolute ethyl alcohol is 1: 10-20; then adding a silane coupling agent KH550 and methyl benzoate, heating to 50-70 ℃, stirring and reacting for 1-3 hours; wherein the adding weight ratio of the aluminum powder, the silane coupling agent KH550 and the methyl benzoate is 1: 1: 1; standing and aging for 12-24 h after the reaction is finished, and drying after solid-liquid separation to obtain the pretreated aluminum powder.
Since aluminum powder is very easily oxidized due to its reducibility, it is required to be pretreated before preparing aluminum nitride. After pretreatment, a layer of coating is formed on the surface of the aluminum powder, so that the aluminum powder can be effectively protected. Meanwhile, the protective film can disappear after being heated in a heating area of subsequent reaction, thereby achieving the purpose of temporarily protecting the aluminum powder.
Thirdly, preparing the aluminum nitride by a chemical vapor deposition method comprises the following steps:
the reactor is divided into a heating area, a high-temperature area and a cooling area, wherein the temperatures of the heating area and the high-temperature area are respectively as follows: 200-300 ℃ and 600-800 ℃; continuously introducing argon into the heating area, the high-temperature area and the cooling area, and simultaneously introducing ammonia gas and hydrogen chloride gas into the high-temperature area; enabling aluminum powder to enter a heating area of the reactor through automatic feeding equipment, staying for 1-5 minutes, then continuing to advance to a high-temperature area, staying for 5-15 minutes, and then leaving the high-temperature area to enter a cooling area for cooling; and after the temperature is reduced to room temperature, the aluminum nitride powder is obtained in a finished product box.
The volume ratio of ammonia gas to hydrogen chloride in the high-temperature zone is 2: 1, the weight ratio of the total weight of ammonia gas and hydrogen chloride to the aluminum powder is 5: 1, the ammonia gas and the hydrogen chloride in the high-temperature zone are both gaseous, and the purities of the ammonia gas and the hydrogen chloride are 99.99 percent.
The aluminum nitride powder can be formed through the following two processes: firstly, hydrogen chloride reacts with metal Al powder; then, the generated aluminum chloride reacts with ammonia gas in a combination reaction, and the two processes are represented by the following two formulas:
it is particularly noted that the reaction is a nitridation reduction reaction which is completed in an inert atmosphere, the influence of oxygen or air on the reaction process can be completely eliminated, and the ammonia-hydrogen chloride mixed gas is sufficient to enable the metal aluminum powder to be completely reacted.
FIG. 2a is an XRD spectrum of the prepared aluminum nitride powder, indexed using standard powder diffraction card PD # 251133F. FIG. 2b is an overall SEM image of the aluminum nitride powder, and it can be seen that the powder exists in the form of blocks, the particle size exceeds 10 μm and the distribution is not uniform.
Fourthly, the step of obtaining high-purity aluminum nitride through grinding and grading comprises:
adding aluminum nitride powder into a grinding machine, and adding a grinding ball, a solvent and a grinding aid; firstly, controlling a stirring shaft of a stirring mill to keep high-speed running for 5-10 minutes in the same direction, so that violent collision is generated between materials, then changing the rotating direction of the stirring shaft, reversely running for 15-30 minutes at high speed, further grinding the aluminum nitride powder, and finally grading to obtain the high-purity aluminum nitride with controllable particle size distribution.
The solvent and the grinding aid added in the grinder are respectively ethanol and quartz sand. The weight ratio of the material balls in the grinding machine is 1: 3, the weight ratio of the aluminum nitride powder, the solvent and the grinding aid is 1: 3: 2.
FIG. 3 is the SEM image of the milled aluminum nitride powder, which shows that the particle size distribution of the milled aluminum nitride powder particles is relatively uniform (FIG. 3a), and the average particle size is about 500nm (FIG. 3 b). Through detection, the purity of the prepared aluminum nitride reaches over 99.9 percent.
The preparation of high purity aluminum nitride with controlled particle size distribution according to the present invention is further illustrated by the following examples.
Example 1
The preparation of high-purity aluminum nitride comprises the following steps:
firstly, the steps of preparing and obtaining aluminum powder by using an industrial-grade aluminum ingot are as follows:
melting an industrial-grade aluminum ingot, atomizing by an atomizer under the protection of nitrogen to prepare powder, spraying superfine oil mist into the atomizer, separating by a cyclone separator to obtain oil-containing aluminum powder, and finally performing solid-liquid separation and drying to obtain the aluminum powder.
Secondly, the pretreatment step of the aluminum powder is as follows:
firstly, adding absolute ethyl alcohol into aluminum powder, and performing ultrasonic dispersion; the adding weight ratio of the aluminum powder to the absolute ethyl alcohol is 1: 15; then adding a silane coupling agent KH550 and methyl benzoate, heating to 60 ℃, and stirring for reacting for 2 hours; wherein the adding weight ratio of the aluminum powder, the silane coupling agent KH550 and the methyl benzoate is 1: 1: 1; standing and aging for 18h after the reaction is finished, and drying after solid-liquid separation to obtain the pretreated aluminum powder.
Thirdly, the step of preparing the aluminum nitride by the chemical vapor deposition method comprises the following steps:
the reactor is divided into a heating area, a high-temperature area and a cooling area, wherein the temperatures of the heating area and the high-temperature area are respectively as follows: 260 ℃ and 700 ℃; continuously introducing argon into the heating area, the high-temperature area and the cooling area, and simultaneously introducing ammonia gas and hydrogen chloride gas into the high-temperature area; the volume ratio of ammonia gas to hydrogen chloride in the high-temperature zone is 2: 1, the weight ratio of the total weight of ammonia gas and hydrogen chloride to the aluminum powder is 5: 1, the ammonia gas and the hydrogen chloride in the high-temperature zone are both gaseous, and the purity of the ammonia gas and the hydrogen chloride is 99.99 percent.
Enabling aluminum powder to enter a heating area of the reactor through automatic feeding equipment, staying for 3 minutes, then continuing to advance to a high-temperature area, staying for 8 minutes, and then leaving the high-temperature area to enter a cooling area for cooling; and after the temperature is reduced to the room temperature, the aluminum nitride powder is obtained after entering a finished product box.
Fourthly, the step of obtaining high-purity aluminum nitride through grinding and grading comprises:
adding aluminum nitride powder into a grinding machine, and adding a grinding ball, a solvent and a grinding aid; the solvent and the grinding aid are respectively ethanol and quartz sand, and the weight ratio of material balls in the grinding machine is 1: 3, the weight ratio of the aluminum nitride powder, the solvent and the grinding aid is 1: 3: 2.
firstly, controlling a stirring shaft of a stirring mill to keep high-speed running for 6 minutes in the same direction to generate violent collision among materials, then changing the rotating direction of the stirring shaft, reversely running for 25 minutes at high speed to further grind aluminum nitride powder, and finally grading to obtain high-purity aluminum nitride with controllable particle size distribution.
Example 2
The preparation of high-purity aluminum nitride comprises the following steps:
firstly, the steps of preparing and obtaining aluminum powder by using industrial-grade aluminum ingots are as follows:
melting an industrial-grade aluminum ingot, atomizing by an atomizer under the protection of nitrogen to prepare powder, spraying superfine oil mist into the atomizer, separating by a cyclone separator to obtain oil-containing aluminum powder, and finally performing solid-liquid separation and drying to obtain the aluminum powder.
Secondly, the pretreatment step of the aluminum powder is as follows:
firstly, adding absolute ethyl alcohol into aluminum powder, and performing ultrasonic dispersion; the adding weight ratio of the aluminum powder to the absolute ethyl alcohol is 1: 10; then adding a silane coupling agent KH550 and methyl benzoate, heating to 70 ℃, and stirring for reacting for 3 hours; wherein the adding weight ratio of the aluminum powder, the silane coupling agent KH550 and the methyl benzoate is 1: 1: 1; standing and aging for 12h after the reaction is finished, and drying after solid-liquid separation to obtain the pretreated aluminum powder.
Thirdly, the step of preparing the aluminum nitride by the chemical vapor deposition method comprises the following steps:
the reactor is divided into a heating area, a high-temperature area and a cooling area, wherein the temperatures of the heating area and the high-temperature area are respectively as follows: 300 ℃ and 800 ℃; continuously introducing argon into the heating area, the high-temperature area and the cooling area, and simultaneously introducing ammonia gas and hydrogen chloride gas into the high-temperature area; the volume ratio of ammonia gas to hydrogen chloride in the high-temperature zone is 2: 1, the weight ratio of the total weight of ammonia gas and hydrogen chloride to the aluminum powder is 5: 1, the ammonia gas and the hydrogen chloride in the high-temperature zone are both gaseous, and the purities of the ammonia gas and the hydrogen chloride are 99.99 percent.
Enabling aluminum powder to enter a heating area of the reactor through automatic feeding equipment, staying for 5 minutes, then continuing to advance to a high-temperature area, staying for 12 minutes, and then leaving the high-temperature area to enter a cooling area for cooling; and after the temperature is reduced to the room temperature, the aluminum nitride powder is obtained after entering a finished product box.
Fourthly, the step of obtaining high-purity aluminum nitride through grinding and grading comprises:
adding aluminum nitride powder into a grinding machine, and adding a grinding ball, a solvent and a grinding aid; the solvent and the grinding aid are respectively ethanol and quartz sand, and the weight ratio of material balls in the grinding machine is 1: 3, the weight ratio of the aluminum nitride powder, the solvent and the grinding aid is 1: 3: 2.
firstly, controlling a stirring shaft of a stirring mill to keep high-speed running for 10 minutes in the same direction to generate violent collision among materials, then changing the rotating direction of the stirring shaft, reversely running for 20 minutes at high speed to further grind aluminum nitride powder, and finally grading to obtain high-purity aluminum nitride with controllable particle size distribution.
Example 3
The preparation of high-purity aluminum nitride comprises the following steps:
firstly, the steps of preparing and obtaining aluminum powder by using an industrial-grade aluminum ingot are as follows:
melting an industrial-grade aluminum ingot, atomizing by an atomizer under the protection of nitrogen to prepare powder, spraying superfine oil mist into the atomizer, separating by a cyclone separator to obtain oil-containing aluminum powder, and finally performing solid-liquid separation and drying to obtain the aluminum powder.
Secondly, the pretreatment step of the aluminum powder is as follows:
firstly, adding absolute ethyl alcohol into aluminum powder, and performing ultrasonic dispersion; the adding weight ratio of the aluminum powder to the absolute ethyl alcohol is 1: 20; then adding a silane coupling agent KH550 and methyl benzoate, heating to 50 ℃, and stirring for reacting for 1 hour; wherein the adding weight ratio of the aluminum powder, the silane coupling agent KH550 and the methyl benzoate is 1: 1: 1; standing and aging for 24 hours after the reaction is finished, and drying after solid-liquid separation to obtain the pretreated aluminum powder.
Thirdly, the step of preparing the aluminum nitride by the chemical vapor deposition method comprises the following steps:
the reactor is divided into a heating area, a high-temperature area and a cooling area, wherein the temperatures of the heating area and the high-temperature area are respectively as follows: 230 ℃ and 650 ℃; continuously introducing argon into the heating area, the high-temperature area and the cooling area, and simultaneously introducing ammonia gas and hydrogen chloride gas into the high-temperature area; the volume ratio of ammonia gas to hydrogen chloride in the high-temperature zone is 2: 1, the weight ratio of the total weight of ammonia gas and hydrogen chloride to the aluminum powder is 5: 1, the ammonia gas and the hydrogen chloride in the high-temperature zone are both gaseous, and the purity of the ammonia gas and the hydrogen chloride is 99.99 percent.
Enabling aluminum powder to enter a heating area of the reactor through automatic feeding equipment, staying for 2 minutes, then continuing to advance to a high-temperature area, staying for 15 minutes, and then leaving the high-temperature area to enter a cooling area for cooling; and after the temperature is reduced to the room temperature, the aluminum nitride powder is obtained after entering a finished product box.
Fourthly, the step of obtaining high-purity aluminum nitride through grinding and grading comprises:
adding aluminum nitride powder into a grinding machine, and adding a grinding ball, a solvent and a grinding aid; the solvent and the grinding aid are respectively ethanol and quartz sand, and the weight ratio of material balls in the grinding machine is 1: 3, the weight ratio of the aluminum nitride powder, the solvent and the grinding aid is 1: 3: 2.
firstly, controlling a stirring shaft of a stirring mill to keep running for 10 minutes at a high speed in the same direction to generate violent collision among materials, then changing the rotation direction of the stirring shaft, reversely running for 15 minutes at a high speed to further grind the aluminum nitride powder, and finally grading to obtain the high-purity aluminum nitride with controllable particle size distribution.
The foregoing is illustrative and explanatory only of the present invention, and it is intended that the present invention cover modifications, additions, or substitutions by those skilled in the art, without departing from the spirit of the invention or exceeding the scope of the claims.
Claims (1)
1. A method for preparing high-purity aluminum nitride with controllable grain size distribution firstly utilizes industrial-grade aluminum ingots to prepare and obtain aluminum powder, and comprises the following steps: melting an industrial-grade aluminum ingot, atomizing the industrial-grade aluminum ingot into powder by an atomizer under the protection of nitrogen, spraying superfine oil mist into the atomizer, separating the powder by a cyclone separator to obtain oil-containing aluminum powder, and finally performing solid-liquid separation and drying to obtain the aluminum powder;
the method is characterized by also comprising the steps of pretreating aluminum powder, preparing aluminum nitride by a chemical vapor deposition method, and finally grinding and grading to obtain high-purity aluminum nitride, wherein,
the pretreatment step of the aluminum powder comprises the following steps:
firstly, adding absolute ethyl alcohol into aluminum powder, and performing ultrasonic dispersion; the adding weight ratio of the aluminum powder to the absolute ethyl alcohol is 1: 10-20; then adding a silane coupling agent KH550 and methyl benzoate, heating to 50-70 ℃, stirring and reacting for 1-3 hours; wherein the adding weight ratio of the aluminum powder, the silane coupling agent KH550 and the methyl benzoate is 1: 1: 1; standing and aging for 12-24 hours after the reaction is finished, and drying after solid-liquid separation to obtain pretreated aluminum powder;
the step of preparing the aluminum nitride by the chemical vapor deposition method comprises the following steps:
the reactor is divided into a heating area, a high-temperature area and a cooling area, wherein the temperatures of the heating area and the high-temperature area are respectively as follows: 200-300 ℃ and 600-800 ℃; continuously introducing argon into the heating area, the high-temperature area and the cooling area, and simultaneously introducing ammonia gas and hydrogen chloride gas into the high-temperature area; enabling aluminum powder to enter a heating area of the reactor through automatic feeding equipment, staying for 1-5 minutes, then continuing to advance to a high-temperature area, staying for 5-15 minutes, and then leaving the high-temperature area to enter a cooling area for cooling; after the temperature is reduced to room temperature, the aluminum nitride powder is obtained after entering a finished product box;
the volume ratio of ammonia gas to hydrogen chloride in the high-temperature zone is 2: 1, the weight ratio of the total weight of ammonia gas and hydrogen chloride to the aluminum powder is 5: 1, ammonia gas and hydrogen chloride in the high-temperature zone are gaseous, and the purity of the ammonia gas and the hydrogen chloride is 99.99%;
the step of obtaining the high-purity aluminum nitride by grinding and grading comprises the following steps:
adding aluminum nitride powder into a grinding machine, and adding a grinding ball, a solvent and a grinding aid; firstly, controlling a stirring shaft of a stirring mill to keep high-speed running for 5-10 minutes in the same direction, so that violent collision is generated between materials, then changing the rotating direction of the stirring shaft, reversely running for 15-30 minutes at high speed, further grinding aluminum nitride powder, and finally grading to obtain high-purity aluminum nitride with controllable particle size distribution;
the solvent and the grinding aid added into the grinding machine are respectively ethanol and quartz sand, and the weight ratio of material balls in the grinding machine is 1: 3, the weight ratio of the aluminum nitride powder, the solvent and the grinding aid is 1: 3: 2.
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| 氮化铝粉末的制取方法;李沐山;《硅酸盐通报》;19891231(第3期);第46页左栏倒数第3-19行 * |
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