CN111847403B - Preparation method of aluminum nitride powder - Google Patents
Preparation method of aluminum nitride powder Download PDFInfo
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- CN111847403B CN111847403B CN202010786287.0A CN202010786287A CN111847403B CN 111847403 B CN111847403 B CN 111847403B CN 202010786287 A CN202010786287 A CN 202010786287A CN 111847403 B CN111847403 B CN 111847403B
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/072—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
- C01B21/0726—Preparation by carboreductive nitridation
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- C01B21/072—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
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Abstract
The invention discloses a preparation method of aluminum nitride powder, which comprises the following steps: mixing aluminum nitrate, calcium nitrate, acetylene black and polyethylene glycol, dissolving in deionized water, stirring and mixing uniformly, heating to 65-75 ℃, adding urea, dropwise adding an ammonia water solution, heating and keeping for 20-40 minutes, then placing in a heating furnace at 1250 ℃, and preserving heat for 1-2 hours under a nitrogen atmosphere to obtain a precursor; mechanically mixing the precursor; placing the mechanically mixed precursor in a microwave high-temperature sintering furnace, and performing nitridation treatment to obtain carbon-containing aluminum nitride; and (3) putting the carbon-containing aluminum nitride into a decarburization furnace for decarburization to obtain aluminum nitride powder. The aluminum nitride powder prepared by the invention has the characteristics of uniform particle size distribution, fine particle size, high purity and low impurity oxygen content, and the preparation method is simple, the preparation process is easy to operate, and the aluminum nitride powder is suitable for large-scale production and processing.
Description
Technical Field
The invention relates to the technical field of preparation of inorganic nonmetal powder, in particular to a preparation method of aluminum nitride powder.
Background
The aluminum nitride powder has good thermal, electrical and mechanical properties, high thermal conductivity, low thermal expansion coefficient, good insulation property and dielectric property, and strong high-temperature material, and has wide application prospect in the fields of power electronics, aerospace, national defense and military, automobiles and locomotives, communication and other industries.
The existing methods for preparing aluminum nitride powder mainly comprise an aluminum powder direct nitriding method, an alumina carbothermic reduction method, a chemical vapor deposition method, a high-temperature self-propagating synthesis method and a plasma chemical synthesis method. The direct aluminum powder nitriding method is a simple, direct and easy-to-implement method, can be synthesized at a lower temperature, but has the disadvantages of low aluminum powder conversion rate, difficult control of reaction process, easy agglomeration of products and low product quality; the carbothermic method has the characteristics of wide raw material source, low cost, simple process, uniform product particle size distribution and high purity, but the carbon and the aluminum are difficult to be uniformly mixed, the synthesis temperature is high, the reaction time is long, and the subsequent decarburization treatment is needed; the chemical vapor deposition method has the defects of high production cost and being not beneficial to industrial production.
Chinese patent CN106187203A discloses a method for preparing aluminum nitride powder based on aluminum carbide, comprising the following steps: (a) uniformly mixing a proper amount of micron aluminum powder and micron carbon powder, heating to a preset temperature in an inert atmosphere, and preserving heat for a period of time to react to generate aluminum carbide; (b) heating aluminum carbide in flowing ammonia gas or nitrogen gas to a preset temperature, preserving heat for a period of time, and reacting the aluminum carbide with the ammonia gas or the nitrogen gas in a high-temperature environment to generate aluminum nitride. However, the reaction temperature of the aluminum nitride powder prepared by the patent is higher.
Chinese patent CN107986246A discloses a method for preparing spherical aluminum nitride powder by an aluminum powder nitriding method, which comprises the following steps: (1) mixing the aluminum powder with an externally added activator with the mass fraction of 10-40% to obtain powder with good uniformity; (2) putting the powder obtained in the step (1) into a multifunctional sintering furnace, introducing enough nitrogen, respectively preserving heat for 1-3h at the temperature of 700-; (3) and carrying out wet coarse grinding and fine grinding on the aluminum nitride block to obtain powder, and carrying out vacuum drying to obtain the aluminum nitride powder. However, the quality of the aluminum nitride powder prepared by the method is poor.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing aluminum nitride powder, so as to solve the above technical problems. In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of aluminum nitride powder comprises the following steps:
step S10, mixing aluminum nitrate, calcium nitrate, acetylene black and polyethylene glycol, dissolving in deionized water, stirring and mixing uniformly, heating to 65-75 ℃, adding urea, dropwise adding an ammonia water solution while stirring, heating to 95-100 ℃, preserving heat for 20-40 minutes, placing in a heating furnace at 1250 ℃, preserving heat for 1-2 hours in a nitrogen atmosphere, and obtaining a precursor;
step S20, mechanically mixing the precursors obtained in step S10;
step S30, placing the mechanically mixed precursor into a graphite crucible, placing the graphite crucible into a microwave high-temperature sintering furnace, and carrying out nitriding treatment for 1.5-2.5 hours to obtain carbon-containing aluminum nitride;
and step S40, placing the carbon-containing aluminum nitride into a decarburization furnace, and decarburizing for 3 hours at 660-720 ℃ in a reducing atmosphere to obtain aluminum nitride powder.
The preparation method comprises the following steps of introducing a calcium auxiliary agent in a preparation process of a precursor to obtain a precursor containing calcium oxide, reducing the synthesis temperature of aluminum nitride powder by using the calcium auxiliary agent, wherein a small amount of the added calcium auxiliary agent can generate a calcium aluminate phase with aluminum along with the increase of nitriding temperature, but the calcium aluminate phase can be melted into a liquid phase and completely volatilized along with the increase of the nitriding temperature to be higher than 1420 ℃, so that the obtained product only contains a single aluminum nitride phase, and the introduction of the calcium auxiliary agent can promote the growth of aluminum nitride powder particles to a certain extent;
the microwave calcination is adopted, so that the heating temperature difference is uniform, the characteristic of high energy utilization rate is achieved, the energy consumption is reduced, and the nitriding time is shortened;
further, in step S10, the acetylene black and the aluminum nitrate are added in an amount of C/Al 2 O 3 The molar ratio of (A) to (B) is 2.6-3.2: 1. The production quantity and the purity of aluminum nitride powder are directly influenced by the adding amount of carbon source acetylene black, the aluminum oxide cannot be completely reduced due to too little carbon source adding, the decarburization time is prolonged due to too much carbon source adding, and the yield and the purity of aluminum nitride are further influenced.
Further, in step S10, the aluminum nitrate and the calcium nitrate are added in a weight ratio of 100:0.8 to 2.6.
Further, the weight ratio of the aluminum nitrate to the calcium nitrate is 100: 1.7.
Further, in step S10, the concentration of the aqueous ammonia solution is 5wt% to 12 wt%.
Further, in step S20, the mechanical mixing is performed by using alumina balls as a ball milling medium, wherein the weight ratio of the ball milling material to the ball milling medium is 1: 5-6, and the ball milling is performed for 3-6 hours.
The precursor can generate chemical actions such as grain refinement, lattice distortion, a large number of defects, surface broken bonds and the like after ball milling, has a promotion effect on carbothermic reduction reaction, and can reduce the initial temperature and the complete reaction temperature of the reduction reaction.
Further, in step S30, the specific process parameters of the nitridation process are as follows: vacuumizing a microwave high-temperature sintering furnace to be less than 100Pa, introducing nitrogen to 0.01MPa, and heating to 1380-1420 ℃. The flow rate of the nitrogen is 1L/min-10L/min.
The invention also aims to provide aluminum nitride powder prepared by the preparation method.
The technical scheme can show that the invention has the advantages that:
1. the method for preparing the aluminum nitride powder takes aluminum nitrate as an aluminum source, a calcium auxiliary agent is introduced in the process of synthesizing a precursor to obtain a precursor containing calcium oxide, the calcium auxiliary agent is utilized to reduce the synthesis temperature of the aluminum nitride powder, the calcium aluminate phase is melted into a liquid phase along with the increase of the nitridation temperature to be higher than 1420 ℃, and the liquid phase is completely volatilized, so that the obtained product only contains a single aluminum nitride phase, and the introduction of the calcium auxiliary agent can promote the growth of aluminum nitride powder particles to a certain extent;
2. the method for preparing the aluminum nitride powder adopts microwave calcination, so that the heating temperature difference is uniform, the method has the characteristic of high energy utilization rate, and the purposes of reducing energy consumption and shortening nitriding time are achieved;
3. the aluminum nitride powder prepared by the invention has the characteristics of uniform particle size distribution, fine particle size, high purity and low impurity oxygen content, and the preparation method is simple, the preparation process is easy to operate, and the aluminum nitride powder is suitable for large-scale production and processing.
In addition to the objects, features and advantages described above, other objects, features and advantages of the present invention are also provided. The present invention will be described in further detail below.
Detailed Description
The following detailed description of embodiments of the invention, but the invention can be practiced in many different ways, as defined and covered by the claims.
Example 1
A preparation method of aluminum nitride powder comprises the following steps:
step S10, mixing aluminum nitrate, calcium nitrate, acetylene black and polyethylene glycol, wherein the addition amount of the acetylene black and the aluminum nitrate is C/Al 2 O 3 The molar ratio of the aluminum nitrate to the calcium nitrate is 2.9:1, the adding weight ratio of the aluminum nitrate to the calcium nitrate is 100:1.7, the aluminum nitrate to the calcium nitrate is dissolved in deionized water, the mixture is stirred and mixed evenly, the temperature is raised to 70 ℃, urea is added, an ammonia water solution with the concentration of 8.5 wt% is dripped while stirring, the temperature is raised to 9Preserving heat for 30 minutes at 8 ℃, then putting the mixture into a heating furnace at 1250 ℃, and preserving heat for 1.5 hours under the nitrogen atmosphere to obtain a precursor;
step S20, mechanically mixing the precursor obtained in the step S10, wherein the mechanical mixing is to use alumina balls as ball milling media, the weight ratio of the ball milling materials to the ball milling media is 1:5.5, and the ball milling is carried out for 4.5 hours;
step S30, placing the mechanically mixed precursor into a graphite crucible, placing the graphite crucible into a microwave high-temperature sintering furnace, vacuumizing the microwave high-temperature sintering furnace to be below 100Pa, introducing nitrogen to 0.01MPa, heating to 1400 ℃, and performing nitridation treatment for 2 hours to obtain carbon-containing aluminum nitride;
and step S40, placing the carbon-containing aluminum nitride into a decarburization furnace, and decarburizing for 3 hours at 690 ℃ in a reducing atmosphere to obtain high-quality aluminum nitride powder with high purity and small particle size.
And (3) measuring carbon impurities in the prepared aluminum nitride powder body by using a carbon-sulfur analyzer, wherein the content of the carbon impurities is 0.0015%, and the content of the oxygen impurities is 0.22% by using an inert gas pulse infrared thermal conductivity method.
Example 2
A preparation method of aluminum nitride powder comprises the following steps:
step S10, mixing aluminum nitrate, calcium nitrate, acetylene black and polyethylene glycol, wherein the addition amount of the acetylene black and the aluminum nitrate is C/Al 2 O 3 The molar ratio of aluminum nitrate to calcium nitrate is 2.6:1, the adding weight ratio of aluminum nitrate to calcium nitrate is 100:0.8, the aluminum nitrate and the calcium nitrate are dissolved in deionized water, the mixture is stirred and mixed evenly, the temperature is raised to 65 ℃, urea is added, an ammonia water solution with the concentration of 5wt% is dripped while the mixture is stirred, the temperature is raised to 95 ℃, the temperature is kept for 20 minutes, the mixture is placed in a heating furnace with the temperature of 1250 ℃, and the temperature is kept for 1 hour under the nitrogen atmosphere, so that a precursor is obtained;
step S20, mechanically mixing the precursor obtained in the step S10, wherein the mechanical mixing is to use alumina balls as ball milling media, the weight ratio of the ball milling materials to the ball milling media is 1:5, and the ball milling is carried out for 3 hours;
step S30, placing the mechanically mixed precursor into a graphite crucible, placing the graphite crucible into a microwave high-temperature sintering furnace, vacuumizing the microwave high-temperature sintering furnace to be below 100Pa, introducing nitrogen to 0.01MPa, heating to 1380 ℃, and performing nitridation treatment for 1.5 hours to obtain carbon-containing aluminum nitride;
and step S40, placing the carbon-containing aluminum nitride into a decarburization furnace, and decarburizing for 3 hours at 660 ℃ in a reducing atmosphere to obtain high-quality aluminum nitride powder with high purity and small particle size.
And (3) measuring carbon impurities in the prepared aluminum nitride powder body by using a carbon-sulfur analyzer, wherein the content of the carbon impurities is 0.0022%, and the content of the oxygen impurities is 0.34% by using an inert gas pulse infrared thermal conductivity method.
Example 3
A preparation method of aluminum nitride powder comprises the following steps:
step S10, mixing aluminum nitrate, calcium nitrate, acetylene black and polyethylene glycol, wherein the addition amount of the acetylene black and the aluminum nitrate is C/Al 2 O 3 The molar ratio of aluminum nitrate to calcium nitrate is 3.2:1, the adding weight ratio of aluminum nitrate to calcium nitrate is 100:2.6, the aluminum nitrate and the calcium nitrate are dissolved in deionized water, the mixture is stirred and mixed evenly, the temperature is raised to 75 ℃, urea is added, an ammonia water solution with the concentration of 12wt% is dripped while the mixture is stirred, the temperature is raised to 100 ℃, the temperature is kept for 40 minutes, the mixture is placed in a heating furnace with the temperature of 1250 ℃, and the temperature is kept for 2 hours in the nitrogen atmosphere, so that a precursor is obtained;
step S20, mechanically mixing the precursor obtained in the step S10, wherein the mechanical mixing is to use alumina balls as ball milling media, the weight ratio of the ball milling materials to the ball milling media is 1:6, and the ball milling is carried out for 6 hours;
step S30, placing the mechanically mixed precursor into a graphite crucible, placing the graphite crucible into a microwave high-temperature sintering furnace, vacuumizing the microwave high-temperature sintering furnace to be below 100Pa, introducing nitrogen to 0.01MPa, heating to 1420 ℃, and performing nitridation treatment for 2.5 hours to obtain carbon-containing aluminum nitride;
and step S40, placing the carbon-containing aluminum nitride into a decarburization furnace, and decarburizing for 3 hours at 720 ℃ in a reducing atmosphere to obtain high-quality aluminum nitride powder with high purity and small particle size.
And (3) measuring carbon impurities in the prepared aluminum nitride powder body by using a carbon-sulfur analyzer, wherein the content of the carbon impurities is 0.0018%, and the content of the oxygen impurities is 0.20% by using an inert gas pulse infrared thermal conductivity method.
Example 4
A preparation method of aluminum nitride powder comprises the following steps:
step S10, mixing aluminum nitrate, calcium nitrate, acetylene black and polyethylene glycol, wherein the addition amount of the acetylene black and the aluminum nitrate is C/Al 2 O 3 The molar ratio of aluminum nitrate to calcium nitrate is 2.8:1, the adding weight ratio of aluminum nitrate to calcium nitrate is 100:3.2, the aluminum nitrate and the calcium nitrate are dissolved in deionized water, the mixture is stirred and mixed evenly, the temperature is raised to 60 ℃, urea is added, an ammonia water solution with the concentration of 10 wt% is dripped while the mixture is stirred, the temperature is raised to 98 ℃, the temperature is kept for 25 minutes, the mixture is placed in a heating furnace with the temperature of 1250 ℃, and the temperature is kept for 1 hour in the nitrogen atmosphere, so that a precursor is obtained;
step S20, mechanically mixing the precursor obtained in the step S10, wherein the mechanical mixing is to use alumina balls as ball milling media, the weight ratio of the ball milling materials to the ball milling media is 1:5, and the ball milling is carried out for 5 hours;
step S30, placing the mechanically mixed precursor into a graphite crucible, placing the graphite crucible into a microwave high-temperature sintering furnace, vacuumizing the microwave high-temperature sintering furnace to be below 100Pa, introducing nitrogen to 0.01MPa, heating to 1390 ℃, and performing nitridation treatment for 2 hours to obtain carbon-containing aluminum nitride;
and step S40, placing the carbon-containing aluminum nitride into a decarburization furnace, and decarburizing for 3 hours at 710 ℃ in a reducing atmosphere to obtain high-quality aluminum nitride powder with high purity and small particle size.
And (3) measuring carbon impurities in the prepared aluminum nitride powder body by using a carbon-sulfur analyzer, wherein the content of the carbon impurities is 0.0014%, and the content of the oxygen impurities is 0.25% by using an inert gas pulse infrared thermal conductivity method.
Example 5
A preparation method of aluminum nitride powder comprises the following steps:
step S10, mixing 100g of aluminum nitrate, 3.2g of calcium nitrate, 67.2g of acetylene black and 8.5g of polyethylene glycol, dissolving the mixture in 100ml of deionized water, uniformly stirring and mixing, heating to 60 ℃, adding 4g of urea, dropwise adding 8ml of 10 wt% ammonia water solution while stirring, heating to 98 ℃, keeping the temperature for 25 minutes, then placing the mixture in a heating furnace at 1250 ℃, and keeping the temperature for 1 hour under the nitrogen atmosphere to obtain a precursor;
step S20, mechanically mixing the precursor obtained in the step S10, wherein the mechanical mixing is to use alumina balls as ball milling media, the weight ratio of the ball milling materials to the ball milling media is 1:5.5, and the ball milling is carried out for 4.5 hours;
step S30, placing the mechanically mixed precursor into a graphite crucible, placing the graphite crucible into a microwave high-temperature sintering furnace, vacuumizing the microwave high-temperature sintering furnace to be below 100Pa, introducing nitrogen to 0.01MPa, heating to 1380 ℃, and performing nitridation treatment for 2 hours to obtain carbon-containing aluminum nitride;
and step S40, placing the carbon-containing aluminum nitride into a decarburization furnace, and decarburizing for 3 hours at 690 ℃ in a reducing atmosphere to obtain high-quality aluminum nitride powder with high purity and small particle size.
And (3) measuring carbon impurities in the prepared aluminum nitride powder body by using a carbon-sulfur analyzer, wherein the content of the carbon impurities is 0.0018%, and the content of the oxygen impurities is 0.21% by using an inert gas pulse infrared thermal conductivity method.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The preparation method of the aluminum nitride powder is characterized by comprising the following steps:
step S10, mixing aluminum nitrate, calcium nitrate, acetylene black and polyethylene glycol, dissolving in deionized water, stirring and mixing uniformly, heating to 65-75 ℃, adding urea, dropwise adding an ammonia water solution while stirring, heating to 95-100 ℃, preserving heat for 20-40 minutes, placing in a heating furnace at 1250 ℃, preserving heat for 1-2 hours in a nitrogen atmosphere, and obtaining a precursor; the addition amount of the acetylene black and the aluminum nitrate is C/Al 2 O 3 The molar ratio of (A) to (B) is 2.6-3.2: 1; the adding weight ratio of the aluminum nitrate to the calcium nitrate is 100: 0.8-2.6;
step S20, mechanically mixing the precursors obtained in step S10; the mechanical mixing is to ball mill the materials for 3-6 hours by using alumina balls as ball milling media and the weight ratio of the ball milling materials to the ball milling media is 1: 5-6;
step S30, placing the mechanically mixed precursor into a graphite crucible, placing the graphite crucible into a microwave high-temperature sintering furnace, and carrying out nitriding treatment for 1.5-2.5 hours to obtain carbon-containing aluminum nitride;
and step S40, placing the carbon-containing aluminum nitride into a decarburization furnace, and decarburizing for 3 hours at 660-720 ℃ in a reducing atmosphere to obtain aluminum nitride powder.
2. The method of claim 1, wherein the aluminum nitrate and the calcium nitrate are added in a weight ratio of 100: 1.7.
3. The method of claim 1, wherein the concentration of the aqueous ammonia solution in step S10 is 5wt% to 12 wt%.
4. The preparation method according to claim 1, wherein in step S30, the specific process parameters of the nitridation process are: vacuumizing a microwave high-temperature sintering furnace to be less than 100Pa, introducing nitrogen to 0.01MPa, and heating to 1380-1420 ℃.
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