CN115215664B - Low-oxygen-content aluminum nitride micro powder and preparation method and application thereof, and synthetic furnace - Google Patents
Low-oxygen-content aluminum nitride micro powder and preparation method and application thereof, and synthetic furnace Download PDFInfo
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Abstract
The application relates to low-oxygen-content aluminum nitride micro powder, a preparation method, application and a synthesis furnace thereof, which comprise the following steps: weighing 30 to 60 parts of nanoscale carbon source, 100 parts of alumina powder, 50 to 100 parts of water and 1 to 5 parts of dispersing agent, and adding the mixture into mixing equipment to prepare mixture slurry; granulating to obtain aluminum nitride precursor particles; adding aluminum nitride precursor particles into a drying device for drying treatment to obtain a semi-finished product A; loading the semi-finished product A into a reaction boat, placing the reaction boat into a synthesis furnace, and performing high-temperature carbothermic reduction reaction on the semi-finished product A in a nitrogen environment to prepare a semi-finished product B; decarburizing the semi-finished product B to prepare aluminum nitride micro powder. According to the scheme, the preparation process is changed, so that the oxygen content of the prepared aluminum nitride micro powder is low under the condition of small granularity, and therefore, the thermal conductivity and densification of the aluminum nitride ceramic sintered by the aluminum nitride micro powder are high, and the market demand for high-performance aluminum nitride ceramic is met.
Description
Technical Field
The application relates to the technical field of preparation of aluminum nitride micro powder, in particular to low-oxygen-content aluminum nitride micro powder, a preparation method and application thereof, and a synthesis furnace.
Background
With the development of high power and very large scale integrated circuits, the importance of heat dissipation between the integrated circuit and the circuit substrate is becoming more and more evident. Therefore, the circuit substrate must have high thermal conductivity. In order to meet the requirement, researchers at home and abroad develop a series of high-performance ceramic substrate materials, wherein aluminum nitride ceramics have the characteristics of high heat conductivity, low dielectric constant and dielectric loss, reliable electrical insulation, good mechanical property, thermal expansion coefficient matched with silicon and the like, are advanced ceramic materials with the best comprehensive performance, and are considered to be ideal materials for new-generation semiconductor substrates and electronic packages.
The high-quality aluminum nitride powder is a prerequisite for obtaining high-performance aluminum nitride ceramics, and the purity, granularity, oxygen content and other impurity content of the aluminum nitride powder have important influence on the thermal conductivity of the prepared aluminum nitride ceramics and the subsequent sintering forming process. Aluminum nitride belongs to phonon heat conduction mechanism, impurity oxygen is a key factor influencing aluminum nitride heat conductivity, if oxygen enters aluminum nitride crystal lattice, structural defects such as aluminum vacancy, dislocation, reverse domain boundary and the like can be formed, phonon propagation is influenced, and heat conductivity is seriously reduced, so that oxygen impurities in aluminum nitride ceramic are main factors influencing heat conduction, and the higher the oxygen content of aluminum nitride powder, the lower the heat conductivity of aluminum nitride ceramic.
The preparation method of the aluminum nitride powder mainly comprises a carbothermic reduction method, an aluminum powder direct nitriding method, a self-propagating high-temperature synthesis method and a Chemical Vapor Deposition (CVD) method. Among them, the carbothermal reduction method and the aluminum powder direct nitriding method are the most commonly used methods for preparing aluminum nitride powder in industrial production. The aluminum nitride powder prepared by the carbothermal reduction method has the characteristics of high purity, fine granularity, narrow granularity distribution and the like, and is suitable for casting molding, injection molding and other molding processes. The aluminum nitride powder with fine granularity has high specific surface area, good sintering activity and easy densification, so the preparation of the aluminum nitride powder with fine granularity is favorable for obtaining the highly densified aluminum nitride ceramic. In the preparation method of the nano aluminum nitride powder disclosed in the Chinese patent application No. 201810005937.6, the average particle size of the prepared aluminum nitride powder is 30nm to 50nm, and the oxygen content is lower than 1.2%. In a method for preparing aluminum nitride powder at high pressure as disclosed in the Chinese patent of patent No. 201810673458.1, the average particle size of the prepared aluminum nitride powder is 1-1.2 μm, and the oxygen content is lower than 0.95%. In the aluminum nitride powder disclosed in Chinese patent application No. 201811498113.3, as well as the preparation method and application thereof, the average particle size of the prepared aluminum nitride powder is 1-1.6 mu m, and the oxygen content is lower than 0.8%.
Although the aluminum nitride powder with fine granularity is favorable for densification of materials, the aluminum nitride powder with fine granularity has high specific surface area, and the aluminum nitride powder with fine granularity has high oxygen content due to the self-hydrophilic property of the aluminum nitride powder, namely, in order to obtain the high-densification aluminum nitride ceramic, the aluminum nitride powder with fine granularity is required to be sintered, but the aluminum nitride powder with fine granularity has high oxygen content, and the sintered aluminum nitride ceramic has low thermal conductivity; in order to obtain aluminum nitride ceramics with higher thermal conductivity, the oxygen content of the aluminum nitride powder needs to be lower, which leads to larger granularity of the aluminum nitride powder and lower densification of the sintered aluminum nitride ceramics. Therefore, how to balance the relationship between fine particle size and low oxygen content of aluminum nitride powder to obtain aluminum nitride powder with fine particle size and low oxygen content is a urgent problem to be solved by those skilled in the art.
Disclosure of Invention
Based on the above, it is necessary to solve the problem that in the prior art, the aluminum nitride powder has a relatively high oxygen content when the particle size is small, or has a relatively large particle size when the oxygen content is low, and the aluminum nitride powder with a small particle size and a low oxygen content cannot be prepared, so that the aluminum nitride ceramic sintered by the aluminum nitride powder has a low thermal conductivity or a low densification, and it is difficult to meet the market demand for high-performance aluminum nitride ceramics. The preparation process is changed to ensure that the oxygen content of the prepared aluminum nitride micro powder is low under the condition of small granularity, so that the aluminum nitride powder with small granularity and low oxygen content is prepared.
The preparation method of the aluminum nitride micro powder with low oxygen content comprises the following steps:
(1) Weighing 30 to 60 parts of nanoscale carbon source, 100 parts of alumina powder, 50 to 100 parts of water and 1 to 5 parts of dispersing agent, and adding the mixture into mixing equipment to prepare mixture slurry;
(2) Granulating the mixture slurry by using a spray drying tower to obtain aluminum nitride precursor particles (400), wherein the particle size of the aluminum nitride precursor particles is 50-300 mu m, and the apparent density is 0.7g/cm 3 To 1.0g/cm 3 ；
(3) Adding the aluminum nitride precursor particles into a drying device for drying treatment, wherein the drying condition is a drying temperature of 120-170 ℃ and the drying time is 3-6 hours, so as to obtain a semi-finished product A;
(4) Loading the semi-finished product A into a reaction boat, placing the reaction boat into a synthesis furnace, and performing high-temperature carbothermic reduction reaction on the semi-finished product A in a nitrogen environment to prepare a semi-finished product B, wherein the synthesis temperature in the synthesis furnace is 1400-1700 ℃ and the synthesis time is 3-15 hours;
(5) And decarburizing the semi-finished product B to prepare aluminum nitride micro powder.
Preferably, in the preparation method of the aluminum nitride micro powder with low oxygen content, the nanoscale carbon source is any one of carbon nano-black, carbon nano-powder, polyvinyl alcohol and methyl cellulose, and the dispersing agent is any one of polyacrylate ester, triethanolamine, polyethylene glycol and propylene glycol methyl ether.
Preferably, in the preparation method of the aluminum nitride micro powder with low oxygen content, the nanoscale carbon source is nano carbon black, and the step (1) further comprises weighing 1 to 2 parts of polyvinyl alcohol or methyl cellulose.
Preferably, in the preparation method of the aluminum nitride micro powder with low oxygen content, the mixing equipment is a stirred ball mill or a roller ball mill, grinding balls used in the mixing equipment are 95% high-purity aluminum oxide balls, the ball diameter of the grinding balls is 5mm to 15mm, the ball-material ratio is 2:1 to 4:1, the rotating speed of the mixing equipment is 20rpm to 120rpm, and the mixing time is 3 hours to 5 hours.
Preferably, in the above method for preparing aluminum nitride micro powder with low oxygen content, in the step (2), the mixture slurry is pumped into the spray drying tower through a diaphragm pump, and is atomized at high speed and rapidly dried to prepare spherical or spheroid-like aluminum nitride precursor particles, wherein the inlet temperature of the spray drying tower is 160 ℃ to 240 ℃, the outlet temperature is 100 ℃ to 140 ℃, and the rotation speed of an atomization plate is 5000rpm to 10000rpm.
Preferably, in the above method for preparing aluminum nitride micro powder with low oxygen content, the step (5) includes:
blowing inert gas to the semi-finished product B at preset pressure to perform air flow dispersion treatment on the semi-finished product B, and decarburizing the semi-finished product B after the air flow dispersion treatment to prepare aluminum nitride micro powder.
Preferably, in the above method for preparing aluminum nitride micro powder with low oxygen content, the step of decarburizing the semi-finished product B after the gas flow dispersing treatment to prepare aluminum nitride micro powder includes:
pouring the semi-finished product B subjected to the air flow dispersion treatment into a stainless steel crucible or a corundum crucible, loading into a heating furnace, heating to 600-750 ℃ along with the heating furnace, and performing decarburization treatment to obtain aluminum nitride micro powder.
The utility model provides a synthetic furnace, is applied to above-mentioned step (4), the synthetic furnace includes synthetic furnace body and reaction boat, the reaction boat includes casing and inlet portion, the air inlet has been seted up to casing bottom central point department, inlet portion has the inlet channel, the one end of inlet channel is the open end, and the other end is sealed blind end, a plurality of inlet ports have been seted up to the lateral wall of inlet portion, the open end with the air inlet is connected and is linked together, just inlet portion is located in the casing, inlet portion with form between the casing and hold the material space, hold the material space with inlet channel passes through the inlet port intercommunication, in vertical decurrent direction, the inlet port certainly inlet portion's lateral wall is towards hold the downwardly extending setting of material space slope.
The low-oxygen-content aluminum nitride micro powder prepared by the preparation method has the oxygen content of less than 0.8 percent and the average granularity of less than 1.2 microns.
The application of the aluminum nitride micro powder with low oxygen content in preparing electronic ceramic materials.
The technical scheme adopted by the application can achieve the following beneficial effects:
(1) By adopting the wet mixing mode, uneven mixing caused by dry mixing can be effectively prevented, wall sticking is easy, and explosion risks are caused by heat generated in the mixing process. Meanwhile, compared with other solvents adopted in the prior art, the solvent is water, so that the source is wide and the cost is low.
(2) The synthesis furnace used in the process of preparing the semi-finished product B by the high-temperature carbothermal reduction reaction of the semi-finished product A adopts a reaction boat with a novel structure, so that nitrogen gas is uniformly contacted with aluminum nitride precursor particles 400 in the material containing space 300, and carbon monoxide generated by each position in the material containing space 300 can be taken away by the nitrogen gas dispersed in each position in the material containing space 300, so that the carbothermal reduction reaction of the nitrogen gas and the aluminum nitride precursor particles 400 is complete, aluminum nitride powder with high purity and good uniformity is obtained, meanwhile, the consumption of the nitrogen gas can be reduced, the reaction time is shortened, the power consumption of the synthesis furnace is reduced, the nitrogen gas consumption is reduced by 40% compared with the prior art, the equipment power consumption is reduced by 20%, the production cost is reduced, and the economy is good.
(3) The synthesis equipment and the synthesis method of the raw material components, the mixture ratio, the mixing mode and the aluminum nitride precursor particles 400 are mainly adjusted, so that the aluminum nitride micro powder prepared by the preparation method is low in oxygen content under the condition of small granularity, and the relationship between the tiny granularity and the low oxygen content of the aluminum nitride powder is balanced, thereby preparing the aluminum nitride micro powder with tiny granularity and low oxygen content.
Drawings
FIG. 1 is a schematic view of a reaction boat for a synthesis furnace according to an embodiment of the present application;
FIG. 2 is a schematic view of a part of a reaction boat for a synthesis furnace according to an embodiment of the present application;
FIG. 3 is a schematic view showing a part of another structure of a reaction boat for a synthesis furnace according to an embodiment of the present application;
fig. 4 to 6 are electron microscope scanning pictures of low-oxygen-content aluminum nitride micro powder disclosed in the embodiment of the application.
Wherein: the aluminum nitride precursor comprises a shell 100, an air inlet 110, a material bearing plate 120, an air inlet part 200, an air inlet channel 210, an air inlet hole 220, a material containing space 300 and aluminum nitride precursor particles 400.
Detailed Description
In order that the application may be readily understood, a more complete description of the application will be rendered by reference to the appended drawings. The drawings illustrate preferred embodiments of the application. This application may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
It will be understood that when an element is referred to as being "disposed on" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "left," "right," "top," "bottom," "top," and the like are used herein for illustrative purposes only and are not meant to be the only embodiment.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1 to 6, an embodiment of the application discloses a method for preparing low-oxygen-content aluminum nitride micro powder, which comprises the following steps:
(1) Weighing 30 to 60 parts of nanoscale carbon source, 100 parts of alumina powder, 50 to 100 parts of water and 1 to 5 parts of dispersing agent, and adding the mixture into mixing equipment to prepare mixture slurry;
the wet mixing mode is adopted, so that uneven mixing caused by dry mixing can be effectively prevented, wall sticking is easy to occur, and explosion risks caused by heat generation in the mixing process can be effectively prevented, and therefore, compared with the dry mixing mode, the wet mixing mode can be adopted, the mixing uniformity can be improved, the wall sticking is prevented, and the explosion risks are avoided. Meanwhile, compared with other solvents adopted in the prior art, the solvent is water, so that the source is wide and the cost is low.
Preferably, the nanoscale carbon source is any one of carbon nanocarbon, polyvinyl alcohol and methyl cellulose, and carbon nanocarbon is commonly used. The dispersing agent is any one of polyacrylate ester, triethanolamine, polyethylene glycol and propylene glycol methyl ether.
In the case that the nanoscale carbon source is nano carbon black, preferably, 1 to 2 parts of organic carbon source can be weighed in step (1), the organic carbon source can be polyvinyl alcohol or methyl cellulose, the viscosity value of the mixture slurry can be adjusted, and the aluminum nitride precursor particles 400 prepared in step (2) have better strength. Meanwhile, adding an organic carbon source to form carbon residues through the drying process of the step (3) to participate in the high-temperature carbothermic reduction reaction of the step (4).
Preferably, the mixing equipment can be a stirred ball mill or a roller ball mill, grinding balls used in the mixing equipment are 95% high-purity alumina balls, the ball diameters of the grinding balls are 5mm to 15mm, the ball-material ratio is 2:1 to 4:1, the rotating speed of the mixing equipment is 20rpm to 120rpm, and the mixing time is 3 hours to 5 hours, so that the raw materials are uniformly mixed.
(2) Granulating the mixture slurry by using a spray drying tower to obtain aluminum nitride precursor particles 400, wherein the particle size of the aluminum nitride precursor particles 400 is 50-300 mu m, and the apparent density is 0.7g/cm 3 To 1.0g/cm 3 I.e., 0.7 to 1 kg of aluminum nitride precursor particles 400 can be loaded per liter of cartridge.
Preferably, the mixture slurry is pumped into a spray drying tower through a diaphragm pump, and is atomized at high speed and rapidly dried to prepare spherical or spheroid aluminum nitride precursor particles 400, wherein the inlet temperature of the spray drying tower is 160-240 ℃, the outlet temperature is 100-140 ℃, and the rotating speed of an atomizing disc is 5000-10000 rpm. The granulated aluminum nitrideThe precursor particles 400 are spherical or spheroid, and the precursor particles are tiny, fully contacted with nitrogen and C-Al 2 O 3 The interface contact is good, mass transfer and reaction are facilitated, the rapid synthesis in the step (4) can be realized, the time is shortened, and the reaction completion degree can be increased.
(3) Adding the aluminum nitride precursor particles 400 into a drying device for drying treatment, wherein the drying condition is a drying temperature of 120-170 ℃ and the drying time is 3-6 hours, so as to obtain a semi-finished product A; the drying device may be an oven such that more than 99% of the moisture in the aluminum nitride precursor particles 400 is evaporated.
(4) Loading the semi-finished product A into a reaction boat, placing the reaction boat into a synthesis furnace, and performing high-temperature carbothermic reaction on the semi-finished product A in a nitrogen environment to prepare a semi-finished product B, wherein the synthesis temperature in the synthesis furnace is 1400-1700 ℃ and the synthesis time is 3-15 hours; the synthesis furnace is a synthesis furnace disclosed hereinafter, the synthesis furnace comprises a synthesis furnace body and a reaction boat, the semi-finished product A is loaded into the reaction boat, the reaction boat comprises a shell 100 and an air inlet part 200, an air inlet 110 is formed in the center of the bottom of the shell 100, the air inlet part 200 is provided with an air inlet channel 210, one end of the air inlet channel 210 is an open end, the other end is a sealed closed end, a plurality of air inlets 220 are formed in the side wall of the air inlet part 200, the open end is connected and communicated with the air inlet 110, the air inlet part 200 is positioned in the shell 100, a material containing space 300 is formed between the air inlet part 200 and the shell 100, and the material containing space 300 is communicated with the air inlet channel 210 through the air inlets 220.
In the specific process of this step, the semi-finished product a is loaded into the reaction boat, then the reaction boat loaded with the aluminum nitride precursor particles 400 is moved into the synthesis furnace, then the synthesis furnace is started, nitrogen is introduced into the air inlet channel 210 through the air inlet 110, nitrogen in the air inlet channel 210 enters the containing space 300 through the air inlet holes 220, nitrogen is introduced into the containing space 300 through the air inlet holes 220, nitrogen entering the containing space 300 through the air inlet holes 220 is dispersed, the nitrogen can be uniformly dispersed in all positions in the containing space 300, the nitrogen is uniformly contacted with the aluminum nitride precursor particles 400 in the containing space 300, carbon monoxide generated in all positions in the containing space 300 can be taken away by the nitrogen, so that aluminum nitride powder with high purity and good uniformity is obtained through carbon thermal reduction reaction of the nitrogen, meanwhile, the use amount of the nitrogen can be reduced, the reaction time is shortened, the power consumption of the synthesis furnace is reduced, the use amount of the nitrogen is reduced by 40%, the equipment is reduced by 20%, and the production cost is reduced.
(5) Decarburizing the semi-finished product B to prepare aluminum nitride micro powder.
Preferably, inert gas is blown to the semi-finished product B at a preset pressure to perform air flow dispersion treatment on the semi-finished product B, and decarburization treatment is performed on the semi-finished product B after the air flow dispersion treatment to prepare aluminum nitride micro powder. The gas flow dispersion treatment of the semi-finished product B can cause agglomeration among the semi-finished product B particles to be opened to prevent carbon from being trapped among the aluminum nitride particles, so that carbon in the semi-finished product B can be removed in the decarburization treatment, and the oxygen content in the semi-finished product B can be prevented from being increased by the inert gas. The inert gas may be helium or argon, etc., and the preset pressure may be 0.3 mpa.
Further, pouring the semi-finished product B subjected to the air flow dispersion treatment into a stainless steel crucible or a corundum crucible, loading into a heating furnace, heating to 600-750 ℃ along with the heating furnace, and performing decarburization treatment to obtain aluminum nitride micro powder.
In the preparation method of the aluminum nitride micro powder with low oxygen content disclosed by the embodiment of the application, the raw material components, the proportion and the mixing mode as well as the synthesis equipment and the synthesis method of the aluminum nitride precursor particles 400 are mainly adjusted, so that the oxygen content of the aluminum nitride micro powder prepared by the preparation method is lower under the condition of small granularity, the relationship between the small granularity of the aluminum nitride powder and the low oxygen content is balanced, and the aluminum nitride micro powder with small granularity and the low oxygen content is prepared, and the process is simple, safe and low in cost, so that the thermal conductivity and densification of the aluminum nitride ceramic sintered by the aluminum nitride micro powder are higher, and the market demand of the high-performance aluminum nitride ceramic is met.
The embodiment of the application also discloses low-oxygen-content aluminum nitride micro powder, which is prepared by adopting the low-oxygen-content aluminum nitride micro powder preparation method, wherein the oxygen content of the prepared low-oxygen-content aluminum nitride micro powder is less than 0.8%, and the average granularity is less than 1.2 microns.
It will be appreciated by those skilled in the art that the low-oxygen content aluminum nitride micro powder has the general property of aluminum nitride micro powder, and can be used for preparing aluminum nitride ceramics by casting and injection molding. Of course, the low-oxygen-content aluminum nitride micro powder can be used for preparing electronic ceramic materials, semiconductor substrates, circuit substrates and the like.
The embodiment of the application also discloses a synthesis furnace, which is applied to the step (4) described above and is used for performing a high-temperature carbothermic reduction reaction on a semi-finished product A in a nitrogen environment to prepare a semi-finished product B, and specifically, the synthesis furnace comprises a synthesis furnace body and a reaction boat, the reaction boat comprises a shell 100 and an air inlet part 200, an air inlet 110 is formed in the center position of the bottom of the shell 100, the air inlet part 200 is provided with an air inlet channel 210, one end of the air inlet channel 210 is an open end, the other end is a sealed closed end, a plurality of air inlets 220 are formed in the side wall of the air inlet part 200, the open end is connected and communicated with the air inlet 110, the air inlet part 200 is positioned in the shell 100, a material containing space 300 is formed between the air inlet part 200 and the shell 100, and the material containing space 300 is communicated with the air inlet channel 210 through the air inlets 220.
In the synthesis furnace disclosed in the embodiment of the application, by changing the structure of the reaction boat, the air inlet part 200 is provided with the air inlet channel 210, the side wall of the air inlet part 200 is provided with the plurality of air inlet holes 220, and the material containing space 300 is communicated with the air inlet channel 210 through the air inlet holes 220. The nitrogen gas is introduced into the air inlet channel 210 through the air inlet 110, the nitrogen gas in the air inlet channel 210 enters the material containing space 300 through the air inlet holes 220, the nitrogen gas is introduced into the material containing space 300 through the air inlet holes 220, the nitrogen gas entering the material containing space 300 through the air inlet holes 220 is dispersed, the nitrogen gas can be uniformly dispersed to each position in the material containing space 300, the nitrogen gas is uniformly contacted with the aluminum nitride precursor particles 400 in the material containing space 300, and the carbon monoxide generated by each position in the material containing space 300 can be taken away by the nitrogen gas dispersed to each position in the material containing space 300, so that the carbon thermal reduction reaction of the nitrogen gas and the aluminum nitride precursor particles 400 is complete, the aluminum nitride powder with high purity and good uniformity is obtained, the use amount of the nitrogen gas can be reduced, the reaction time is shortened, the power consumption of the synthesis furnace is reduced, the use amount of the nitrogen gas is reduced by 40% compared with the prior art, the power consumption of the equipment is reduced by 20%, the production cost is reduced, and the economical efficiency of synthesizing the aluminum nitride powder through the synthesis furnace is further improved.
As described above, the sidewall of the air inlet portion 200 is provided with the plurality of air inlet holes 220, the nitrogen gas in the air inlet channel 210 enters the material containing space 300 through the plurality of air inlet holes 220, the aluminum nitride precursor particles 400 are contained in the material containing space 300, and the aluminum nitride precursor particles 400 may enter the air inlet holes 220 after the aluminum nitride precursor particles 400 are contained in the material containing space 300 due to the small granularity of the aluminum nitride precursor particles 400, so that the air inlet holes 220 may be blocked. Based on this, in an alternative embodiment, in the vertical downward direction, the air inlet holes 220 may extend obliquely downward from the side wall of the air inlet portion 200 toward the material accommodating space 300, and the air inlet holes 220 disposed obliquely downward can effectively reduce the entry of the aluminum nitride precursor particles 400 into the air inlet holes 220, so that the aluminum nitride precursor particles 400 can be prevented from blocking the air inlet holes 220 to a greater extent, and the use reliability of the reaction boat is improved. Simultaneously, the inlet port 220 that the slope set up downwards can be with nitrogen downward flow guide, nitrogen downward flow contact aluminium nitride precursor granule 400 to take away carbon monoxide and flow upwards, finally follow the export outflow of reaction boat, can make the flow path of nitrogen longer like this, avoid nitrogen direct outflow, thereby can make nitrogen fully contact with aluminium nitride precursor granule 400 in holding material space 300, and can take away the produced carbon monoxide in each position in holding material space 300, further reduce the use amount of nitrogen and shorten reaction time.
Preferably, the angle formed between the extending direction of the air intake hole 220 and the vertical direction may be 20 ° to 50 °.
According to the related knowledge of fluid mechanics, nitrogen flows forward after passing through the air inlet 220 and gradually flows upward, which makes it difficult for nitrogen to flow to the bottom corner of the outer wall of the accommodating space 300, and makes the nitrogen contact with the aluminum nitride precursor particles 400 at the bottom corner of the outer wall of the accommodating space 300 insufficient. Based on this, in an alternative embodiment, the bottom of the shell 100 is obliquely provided with the material bearing plate 120, in the vertical upward direction, the material bearing plate 120 may be obliquely and upwardly extended from the central position of the bottom of the shell 100 toward the inner wall of the shell 100 and connected with the inner wall of the shell 100, the air inlet 200, the inner wall of the shell 100 and the material bearing plate 120 form the material containing space 300, and the obliquely arranged material bearing plate 120 can avoid that the aluminum nitride precursor particles 400 are contained at the bottom angle position of the outer wall of the material containing space 300, and no nitrogen gas is required to flow to the bottom angle position of the outer wall of the material containing space 300, so that the aluminum nitride powder in the same reaction boat can react more completely, and the uniformity of the produced aluminum nitride powder is good. Meanwhile, the nitrogen gas can form airflow rotation after flowing to the material bearing plate 120, so that the nitrogen gas flow path is long, the nitrogen gas can be fully contacted with the aluminum nitride precursor particles 400 in the material containing space 300, carbon monoxide generated at each position in the material containing space 300 can be taken away, the using amount of the nitrogen gas is further reduced, and the reaction time is shortened.
The technical scheme and effect of the present application will be further described by specific comparative examples, and it should be noted that the following comparative examples are only for further explanation of the present application, and are not limiting of the technical scheme of the present application.
The following comparative experiments were set up:
experimental example 1: weighing 50 parts of nano carbon black, 100 parts of alumina powder and 75 parts of water, adding into a roller ball mill to prepare mixture slurry, wherein grinding balls used by the roller ball mill are 95% high-purity alumina balls, the ball diameter of the grinding balls is 10mm, the ball-to-material ratio is 3:1, and the rotating speed of the roller ball mill is 100rpm; granulating the mixture slurry by using a spray drying tower to obtain aluminum nitride precursor particles 400, wherein the particle size of the aluminum nitride precursor particles 400 is 100 μm, and the apparent density is 0.9g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Adding the aluminum nitride precursor particles 400 into an oven for drying treatment, wherein the drying temperature is 150 ℃ and the drying time is 5 hours, so as to obtain a semi-finished product A; semi-finished product A is processed in a nitrogen environment by using a conventional graphite furnacePreparing a semi-finished product B by high-temperature carbothermal reduction reaction, wherein the synthesis temperature is 1650 ℃ and the synthesis time is 10 hours; decarburizing the semi-finished product B to prepare aluminum nitride micro powder.
Experimental example 2: substantially the same as in experimental example 1, except that: weighing 100 parts of nano carbon black, 100 parts of alumina powder and 75 parts of water.
Experimental example 3: substantially the same as in experimental example 1, except that: 50 parts of nano carbon black, 100 parts of alumina powder, 75 parts of water and 2 parts of polyacrylate ester are weighed.
Experimental example 4: substantially the same as in experimental example 1, except that: the semi-finished product A is put into a reaction boat disclosed above, and the reaction boat is placed into a synthesis furnace disclosed above, and the semi-finished product A is subjected to high-temperature carbothermic reduction reaction in a nitrogen environment to prepare a semi-finished product B, wherein the synthesis temperature is 1600 ℃, and the synthesis time is 4 hours.
Experimental example 5: substantially the same as in experimental example 3, except that: the semi-finished product A is put into a reaction boat disclosed above, and the reaction boat is placed into a synthesis furnace disclosed above, and the semi-finished product A is subjected to high-temperature carbothermic reduction reaction in a nitrogen environment to prepare a semi-finished product B, wherein the synthesis temperature is 1600 ℃, and the synthesis time is 4 hours.
The aluminum nitride micropowder obtained in each of Experimental examples 1 to 5 was examined to obtain carbon content, oxygen content and D 50 。
The comparative experiment results are shown in the following table:
| C（ppm） | O（%） | D 50 （μm） | |
| experimental example 1 | 451 | 1.03 | 1.526 |
| Experimental example 2 | 643 | 0.96 | 1.524 |
| Experimental example 3 | 342 | 0.92 | 1.392 |
| Experimental example 4 | 329 | 0.93 | 1.204 |
| Experimental example 5 | 332 | 086 | 1.197 |
As can be seen from the above table data, in experimental example 1, compared with experimental example 2, the proportions of the nano carbon black, the alumina powder and the water are adjusted, and it is found that the components and the proportion relationship thereof in experimental example 1 can reduce the carbon content of the aluminum nitride micro powder, and the oxygen content and the particle size have little change. Compared with experimental example 1, experimental example 3 can reduce the oxygen content of the aluminum nitride micro powder and reduce the granularity by adding the dispersing agent (polyacrylate), and the addition of the dispersing agent proves that the component uniformity of the precursor is improved, so that the contact between carbon and oxide in the reduction process is more uniform, and the granularity is larger or the oxygen content is higher because of the agglomeration or the component segregation of the alumina powder. Experimental example 4 compared with Experimental example 1 and Experimental example 5 compared with Experimental example 3, the synthetic furnace reaction boat disclosed by the application can be used for further reducing the oxygen content and the granularity of the aluminum nitride micro powder.
Meanwhile, in experimental example 4, compared with experimental example 1, and in experimental example 5, compared with experimental example 3, when the carbon and oxygen contents of the aluminum nitride micro powder are substantially the same, the synthesis temperature and synthesis time are both reduced, and of course, the particle size is also reduced due to the reduction of the temperature and time.
The following experiments were set up by using the components and the proportion relation in experimental example 5:
experimental example 6: substantially the same as in experimental example 5, except that: 50 parts of nano carbon black, 100 parts of alumina powder, 75 parts of water, 2 parts of polyacrylate and 2 parts of polyvinyl alcohol are weighed.
Experimental example 7: substantially the same as in experimental example 5, except that: before decarburizing the semi-finished product B, blowing nitrogen gas to the semi-finished product B at a pressure of 0.8 megaPa, carrying out airflow dispersion treatment on the semi-finished product B, pouring the semi-finished product B after the airflow dispersion treatment into a corundum crucible, loading the corundum crucible into a heating furnace, heating the corundum crucible to 650 ℃ along with the heating furnace, and carrying out decarburization treatment to obtain aluminum nitride micro powder.
Experimental example 8: weighing 50 parts of nano carbon black, 100 parts of alumina powder, 75 parts of water, 2 parts of polyacrylate and 2 parts of polyvinyl alcohol, adding into a roller ball mill to prepare mixture slurry conventionally, wherein the roller ball mill adopts 95% high-purity alumina balls, the ball diameter of the grinding balls is 10mm, the ball-material ratio is 3:1, the rotating speed of the roller ball mill is 100rpm, the mixing time is 4 hours, pumping the mixture slurry into a spray drying tower through a diaphragm pump, and preparing spherical aluminum nitride precursor particles 400 after high-speed atomization and rapid drying, wherein the particle diameter of the aluminum nitride precursor particles 400 is 100 mu m, and the apparent density is 0.9g/cm 3 The inlet temperature of the spray drying tower is 200 ℃, the outlet temperature is 120 ℃, the rotating speed of an atomizing disk is 6000rpm, and the aluminum nitride precursor particles 400 are added into a drying oven for drying treatment, wherein the drying temperature is 150 ℃, and the drying time is 5 hours, so that a semi-finished product A is obtained; loading the semi-finished product A into the aboveIn the reaction boat disclosed in the specification, the reaction boat is placed in a synthesis furnace disclosed in the specification, the semi-finished product A is subjected to high-temperature carbothermic reduction reaction in a nitrogen environment to prepare a semi-finished product B, the synthesis temperature is 1600 ℃, the synthesis time is 4 hours, nitrogen is blown to the semi-finished product B at the pressure of 0.8 megapascal before decarburization treatment of the semi-finished product B, gas flow dispersion treatment is carried out on the semi-finished product B, the semi-finished product B after the gas flow dispersion treatment is poured into a corundum crucible, the corundum crucible is filled into a heating furnace, the corundum crucible is heated to 630 ℃ along with the heating furnace, and decarburization treatment is carried out to prepare aluminum nitride micro powder.
The aluminum nitride micropowder obtained in examples 6 to 8 was examined to obtain carbon content, oxygen content and D 50 。
The comparative experiment results are shown in the following table:
| C（ppm） | O（%） | D 50 （μm） | |
| experimental example 5 | 332 | 0.86 | 1.197 |
| Experimental example 6 | 329 | 0.84 | 1.182 |
| Experimental example 7 | 308 | 0.78 | 1.186 |
| Experimental example 8 | 293 | 0.75 | 1.175 |
As can be seen from the above table data, compared with experimental example 5, experimental examples 6 to 8, the carbon content of the aluminum nitride micro powder is kept below 350ppm, which means that the purity of the aluminum nitride micro powder is higher, and at the same time, the oxygen content of the aluminum nitride micro powder is reduced, and the particle size is reduced, wherein the oxygen content of examples 7 and 8 is kept below 0.8%, and the average particle size is kept below 1.2 micrometers.
In particular, in experiment 8, the oxygen content and the particle size of the aluminum nitride micro powder are significantly reduced compared with experiment 1 to experiment 7, and experiment 8 integrates the technology disclosed in the application, and it is seen that the preferred preparation method disclosed in the application is integrated, and compared with the prior art, the oxygen content and the particle size of the prepared aluminum nitride micro powder are significantly reduced, the oxygen content is kept at 0.75, and the average particle size is kept at 1.175 μm.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the application, which are described in detail and are not to be construed as limiting the scope of the claims. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the application, which are all within the scope of the application. Accordingly, the scope of protection of the present application is to be determined by the appended claims.
Claims (7)
1. The preparation method of the aluminum nitride micro powder with low oxygen content is characterized by comprising the following steps:
(1) Weighing 30 to 60 parts of nano carbon black, 100 parts of alumina powder, 50 to 100 parts of water, 1 to 5 parts of dispersing agent, 1 to 2 parts of polyvinyl alcohol or methyl cellulose, and adding the mixture into mixing equipment to prepare mixture slurry, wherein the dispersing agent is any one of polyacrylate ester, triethanolamine, polyethylene glycol and propylene glycol methyl ether;
(2) Granulating the mixture slurry by using a spray drying tower to obtain aluminum nitride precursor particles (400), wherein the particle size of the aluminum nitride precursor particles (400) is 50-300 mu m, and the apparent density is 0.7g/cm 3 To 1.0g/cm 3 ；
(3) Adding the aluminum nitride precursor particles (400) into a drying device for drying treatment, wherein the drying condition is a drying temperature of 120-170 ℃ and the drying time is 3-6 hours, so as to obtain a semi-finished product A;
(4) The synthesis furnace comprises a synthesis furnace body and a reaction boat, wherein the reaction boat comprises a shell (100) and an air inlet part (200), an air inlet (110) is formed in the center position of the bottom of the shell (100), the air inlet part (200) is provided with an air inlet channel (210), one end of the air inlet channel (210) is an open end, the other end of the air inlet channel is a sealed closed end, a plurality of air inlets (220) are formed in the side wall of the air inlet part (200), the open end is connected and communicated with the air inlet (110), the air inlet part (200) is positioned in the shell (100), a material containing space (300) is formed between the air inlet part (200) and the shell (100), the material containing space (300) is communicated with the air inlet channel (210), the air inlet channel (220) is obliquely downwards arranged from the side wall of the air inlet part (200) towards the material containing space (300), the semi-finished boat is filled into the reaction furnace, the semi-finished boat is placed in the synthesis furnace, and the semi-finished boat is subjected to synthesis furnace synthesis at a high temperature of 1700 ℃ and a synthesis furnace temperature of 1700 ℃ when the synthesis furnace is in a high synthesis furnace temperature of 1700 ℃ and a synthesis time of 15 ℃ and a low synthesis temperature of synthesis furnace temperature is reached;
(5) And decarburizing the semi-finished product B to obtain aluminum nitride micro powder, wherein the decarburization temperature is 600-750 ℃, the oxygen content of the aluminum nitride micro powder is less than 0.8%, and the average particle size is less than 1.2 microns.
2. The method for preparing aluminum nitride micro powder with low oxygen content according to claim 1, wherein the mixing equipment is a stirred ball mill or a roller ball mill, grinding balls used in the mixing equipment are 95% high-purity aluminum oxide balls, the ball diameter of the grinding balls is 5mm to 15mm, the ball-material ratio is 2:1 to 4:1, the rotating speed of the mixing equipment is 20rpm to 120rpm, and the mixing time is 3 hours to 5 hours.
3. The method according to claim 1, wherein in the step (2), the mixture slurry is pumped into the spray drying tower through a diaphragm pump, and is atomized at a high speed and rapidly dried to form spherical or spheroid-like aluminum nitride precursor particles (400), wherein the spray drying tower has an inlet temperature of 160 ℃ to 240 ℃, an outlet temperature of 100 ℃ to 140 ℃, and an atomization plate rotation speed of 5000rpm to 10000rpm.
4. The method for producing a low-oxygen-content aluminum nitride fine powder according to claim 1, wherein the step (5) comprises:
blowing inert gas to the semi-finished product B at preset pressure to perform air flow dispersion treatment on the semi-finished product B, and decarburizing the semi-finished product B after the air flow dispersion treatment to prepare aluminum nitride micro powder.
5. The method for producing aluminum nitride fine powder having a low oxygen content according to claim 4, wherein the step of decarburizing the semi-finished product B after the gas flow dispersing treatment to produce aluminum nitride fine powder comprises:
pouring the semi-finished product B subjected to the air flow dispersion treatment into a stainless steel crucible or a corundum crucible, loading into a heating furnace, heating to 600-750 ℃ along with the heating furnace, and performing decarburization treatment to obtain aluminum nitride micro powder.
6. A low-oxygen-content aluminum nitride fine powder prepared by the method according to any one of claims 1 to 5.
7. Use of the aluminium nitride micro powder with low oxygen content according to claim 6 for preparing electronic ceramic materials.
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