CN110577403A - high-purity aluminum nitride powder and preparation method thereof - Google Patents
high-purity aluminum nitride powder and preparation method thereof Download PDFInfo
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Abstract
the invention belongs to the technical field of powder material processing, and particularly relates to high-purity aluminum nitride powder and a preparation method thereof. The preparation method of the high-purity aluminum nitride powder takes the aluminum oxide as the raw material, and can form more gaps in reactants through a grading mixing mode of mixing with the nanoscale carbon powder for the first time and mixing with the micron-sized carbon powder for the second time, effectively promote the discharge of high-temperature reaction products, namely carbon monoxide, and exchange of reaction gas, namely nitrogen and solid-phase raw materials, and contribute to improving the nitridation rate of the raw materials, so that the high-purity aluminum nitride powder is obtained. The prepared aluminum nitride powder has excellent performance, is beneficial to obtaining a compact aluminum nitride ceramic substrate by sintering, improves the thermal conductivity of the substrate, and is widely used as a heat dissipation substrate of a high-power electronic device.
Description
Technical Field
The invention belongs to the technical field of powder material processing, and particularly relates to high-purity aluminum nitride powder and a preparation method thereof.
background
With the rapid development of modern electronic technology, the electronic devices are developed in the direction of miniaturization, light weight, high integration, high density, high power and high reliability. Moreover, as the structure of the electronic device is more and more complex, the size of the substrate is increased and the integration level is improved, so that the dissipation power of the substrate is further increased. Therefore, higher demands are made on the heat dissipation performance of electronic devices, particularly substrates.
Because the thermal conductivity coefficient of the aluminum nitride ceramic is 8-10 times higher than that of the aluminum oxide ceramic, and the electrical properties such as volume resistivity, breakdown field strength, dielectric loss and the like can be compared favorably with those of the aluminum oxide ceramic, the aluminum nitride ceramic has the advantages of low dielectric constant, high mechanical strength, thermal expansion coefficient close to that of silicon, and capability of carrying out multilayer wiring, can meet the heat dissipation requirement of a high-power device, and is considered as a new generation of excellent insulating heat dissipation substrate material with good development prospect. Therefore, the LED power generation system is widely applied to the fields of high-speed rails, new energy automobiles, smart power grids, wind power generation, high-power LEDs and the like.
the aluminum nitride powder is a core material for forming the aluminum nitride ceramic substrate and has decisive influence on the performance of the substrate. Therefore, high-performance AlN powder is the key for preparing the high-thermal-conductivity aluminum nitride ceramic. The method for preparing aluminum nitride powder in the prior art mainly comprises an aluminum powder direct nitriding method, a carbothermic reduction method, a chemical vapor deposition method, a self-propagating combustion synthesis method, a microwave synthesis method and the like. Among them, the direct nitriding method and carbothermic reduction method of aluminum powder realize the industrialized production, and the carbothermic reduction method is most widely applied.
The carbothermic reduction method is that the mixed material of alumina and carbon is reacted for 4 to 10 hours in nitrogen flow at the temperature of 1600-1800 ℃ to obtain aluminum nitride powder containing excessive carbon, then the heat preservation is carried out for 10 to 16 hours at the temperature of 600-900 ℃ and the aluminum nitride powder is obtained after decarburization. The carbothermic method has the characteristics of wide raw material source, low price, simple process and suitability for large-scale production, and the synthesized aluminum nitride powder is nearly spherical, has fine granularity and good dispersibility, has great advantages in the aspects of purity, granularity, stability and the like, and is beneficial to the densification of a sintered substrate.
However, in the carbothermic process, after the alumina and the carbon powder are mixed, the powder is accumulated in the reaction equipment and is roasted in a high-temperature nitrogen atmosphere, and the gaps among the raw materials are small, so that the discharge of the generated product carbon monoxide gas and the material exchange of nitrogen, alumina and carbon powder are not facilitated, and the nitridation reaction is often incomplete. In order to solve the above problems, for example, chinese patent CN106882773A discloses a method of reacting and grinding alumina and carbon powder under high temperature vacuum condition, and performing high temperature nitridation under nitrogen atmosphere; however, this method still has a problem that the nitriding is not complete because of a small gap between the reactants. As in the scheme of chinese patent CN105836717A, in order to increase the nitridation rate of the reactant, the method adds aluminum powder into the mixture of alumina and carbon powder to promote the nitridation rate; however, the aluminum nitride powder is not suitable for preparing a substrate because the aluminum powder is melted at about 660 ℃ and the generated aluminum nitride is seriously agglomerated. Therefore, the development of a method for efficiently preparing high-purity aluminum nitride powder has positive significance.
Disclosure of Invention
Therefore, the technical problem to be solved by the present invention is to provide a method for preparing high purity aluminum nitride powder, so as to solve the problem that the purity of the aluminum nitride powder prepared by the conventional carbothermic method in the prior art is slightly low.
In order to solve the technical problems, the method for preparing the high-purity aluminum nitride powder comprises the following steps:
(1) taking aluminum oxide powder and a nano carbon source, adding grinding balls, fully mixing, and sieving to obtain a first mixture;
(2) adding a micron carbon source into the first mixture, fully mixing, and sieving to obtain a second mixture;
(3) Roasting the second mixture at 1550-;
(4) and (4) carrying out heat preservation reaction on the roasting product obtained in the step (3) at the temperature of 600-800 ℃ in the air atmosphere, and carrying out decarbonization treatment to obtain the high-purity aluminum nitride powder.
In the step (1), the median particle diameter D50 of the alumina powder is 0.2-0.4 μm.
In the step (1), the median particle size D50 of the nano carbon source is 10-50 nm.
In the step (1), the mass ratio of the alumina powder to the nano carbon source is 2: 0.6-1.0.
In the step (1), the grinding balls are alumina balls or aluminum nitride balls with the diameter of 5-20 mm.
In the step (1), the mass ratio of the grinding balls to the mixture of the alumina split body and the nano carbon source is 2: 0.5-1.5.
In the step (2), the median particle size D50 of the micron carbon source is 0.5-5 μm.
In the step (2), the mass ratio of the first mixture to the micron carbon source is 2: 0.1-0.3.
In the step (3), the roasting step is carried out for 8-15 h;
In the step (4), the time of the heat preservation reaction is 3-5 h.
The preparation method of the high-purity aluminum nitride split body takes the aluminum oxide as the raw material, and can form more gaps in reactants through a grading mixing mode of mixing with the nano-scale carbon powder for the first time and mixing with the micron-scale carbon powder for the second time, effectively promotes the discharge of high-temperature reaction products of carbon monoxide and the exchange of reaction gas nitrogen and solid-phase raw materials, is beneficial to improving the nitridation rate of the raw materials, and thus the high-purity aluminum nitride powder is obtained. The prepared aluminum nitride powder has excellent performance, is beneficial to obtaining a compact aluminum nitride ceramic substrate by sintering, improves the thermal conductivity of the substrate, and is widely used as a heat dissipation substrate of a high-power electronic device.
The method for preparing the aluminum nitride powder has the advantages of simple process, low requirement on equipment, low raw material cost and low energy consumption, and is more suitable for large-scale industrial production.
drawings
in order that the present disclosure may be more readily and clearly understood, the following detailed description of the present disclosure is provided in connection with specific embodiments thereof and the accompanying drawings, in which,
FIG. 1 is an XRD diffraction pattern of the aluminum nitride powder obtained in example 1;
FIG. 2 is a microscopic morphology of the aluminum nitride powder prepared in example 1.
Detailed Description
example 1
The preparation method of the high-purity aluminum nitride comprises the following steps:
(1) accurately weighing 200g of alumina powder with the median particle size D50 of 0.2 mu m and 60g of nano carbon powder with the median particle size D50 of 10nm, adding 800g of alumina balls with the diameter of 10mm as grinding balls, placing the grinding balls in a mixing device, carrying out ball milling and mixing for 24 hours, and sieving to obtain a first mixture;
(2) taking 200g of the first mixture after sieving, adding 25g of micron carbon powder with the median particle size D50 of 5 mu m, mixing for the second time for 30min, and sieving to obtain a second mixture;
(3) Roasting the obtained second mixture for 10 hours at 1650 ℃ in nitrogen atmosphere;
(4) and after the obtained roasted product is cooled, placing the obtained roasted product in a muffle furnace, carrying out heat preservation reaction for 5 hours at 700 ℃ under the air condition, carrying out oxidation and decarbonization to obtain high-purity aluminum nitride powder, and testing to obtain the powder with the oxygen content of 0.85%.
The XRD diffraction pattern and the microstructure pattern of the aluminum nitride powder obtained in this example are shown in fig. 1 and 2, respectively.
As can be seen from fig. 1, the powder phase prepared in this example is an aluminum nitride pure phase, and no diffraction peak of other phases exists. This indicates that the raw material alumina has been completely converted to aluminum nitride through the steps in the examples. As shown in FIG. 2, the single particle size of the obtained powder is 1-2 microns, and the particles have good dispersibility.
Example 2
the preparation method of the high-purity aluminum nitride comprises the following steps:
(1) accurately weighing 200g of alumina powder with the median particle size D50 of 0.4 mu m and 80g of nano carbon powder with the median particle size D50 of 20nm, adding 700g of alumina balls with the diameter of 15mm as grinding balls, placing the grinding balls in a mixing device, performing ball milling and mixing for 24 hours, and sieving to obtain a first mixture;
(2) Taking 200g of the first mixture after sieving, adding 20g of micron carbon powder with the median particle size D50 of 2 mu m, mixing for the second time for 30min, and sieving to obtain a second mixture;
(3) roasting the obtained second mixture for 15 hours at 1550 ℃ in a nitrogen atmosphere;
(4) and after the obtained roasted product is cooled, placing the obtained roasted product in a muffle furnace, carrying out heat preservation reaction for 2 hours at 800 ℃ under the air condition, carrying out oxidation and decarbonization to obtain high-purity aluminum nitride powder, and testing to obtain the powder with the oxygen content of 0.92%.
example 3
The preparation method of the high-purity aluminum nitride comprises the following steps:
(1) Accurately weighing 200g of alumina powder with the median particle size D50 of 0.3 mu m and 60g of nano carbon powder with the median particle size D50 of 30nm, adding 520g of alumina balls with the diameter of 10mm as grinding balls, placing the grinding balls in a mixing device, performing ball milling and mixing for 24 hours, and sieving to obtain a first mixture;
(2) Taking 200g of the first mixture after sieving, adding 25g of micron carbon powder with the median particle size D50 of 1 mu m, mixing for the second time for 30min, and sieving to obtain a second mixture;
(3) Roasting the obtained second mixture for 8 hours at 1700 ℃ in a nitrogen atmosphere;
(4) and after the obtained roasted product is cooled, placing the obtained roasted product in a muffle furnace, carrying out heat preservation reaction for 5 hours at the temperature of 600 ℃ under the air condition, carrying out oxidation and decarbonization to obtain high-purity aluminum nitride powder, and testing to obtain the powder with the oxygen content of 0.81%.
example 4
The preparation method of the high-purity aluminum nitride comprises the following steps:
(1) accurately weighing 200g of alumina powder with the median particle size D50 of 0.3 mu m and 70g of nano carbon powder with the median particle size D50 of 40nm, adding 360g of alumina balls with the diameter of 5mm as grinding balls, placing the grinding balls in a mixing device, performing ball milling and mixing for 24 hours, and sieving to obtain a first mixture;
(2) taking 200g of the first mixture after sieving, adding 15g of micron carbon powder with the median particle size D50 of 0.5 mu m, mixing for the second time for 30min, and sieving to obtain a second mixture;
(3) Roasting the obtained second mixture for 8 hours at 1600 ℃ in a nitrogen atmosphere;
(4) and after the obtained roasted product is cooled, placing the obtained roasted product in a muffle furnace, carrying out heat preservation reaction for 4 hours at 700 ℃ under the air condition, carrying out oxidation and decarbonization to obtain high-purity aluminum nitride powder, and testing to obtain the powder with the oxygen content of 0.84%.
example 5
The preparation method of the high-purity aluminum nitride comprises the following steps:
(1) Accurately weighing 200g of alumina powder with the median particle size D50 of 0.25 mu m and 70g of nano carbon powder with the median particle size D50 of 50nm, adding 600g of alumina balls with the diameter of 20mm as grinding balls, placing the grinding balls in a mixing device, performing ball milling and mixing for 24 hours, and sieving to obtain a first mixture;
(2) taking 200g of the first mixture after sieving, adding 10g of micron carbon powder with the median particle size D50 of 2 mu m, mixing for 30min twice, and sieving to obtain a second mixture;
(3) Roasting the obtained second mixture for 10 hours at 1650 ℃ in nitrogen atmosphere;
(4) and after the obtained roasted product is cooled, placing the obtained roasted product in a muffle furnace, carrying out heat preservation reaction for 4 hours at 650 ℃ under the air condition, carrying out oxidation and decarbonization to obtain high-purity aluminum nitride powder, and testing to obtain the powder with the oxygen content of 0.82%.
Example 6
The preparation method of the high-purity aluminum nitride comprises the following steps:
(1) Accurately weighing 200g of alumina powder with the median particle size D50 of 0.28 mu m and 75g of nano carbon powder with the median particle size D50 of 40nm, adding 500g of alumina balls with the diameter of 15mm serving as grinding balls, placing the grinding balls in a mixing device, performing ball milling and mixing for 24 hours, and sieving to obtain a first mixture;
(2) taking 200g of the first mixture after sieving, adding 20g of micron carbon powder with the median particle size D50 of 2 mu m, mixing for the second time for 30min, and sieving to obtain a second mixture;
(3) Roasting the obtained second mixture for 8 hours at 1650 ℃ in a nitrogen atmosphere;
(4) And after the obtained roasted product is cooled, placing the obtained roasted product in a muffle furnace, carrying out heat preservation reaction for 2 hours at 700 ℃ under the air condition, carrying out oxidation and decarbonization to obtain high-purity aluminum nitride powder, and testing to obtain the powder with the oxygen content of 0.83%.
Example 7
The preparation method of the high-purity aluminum nitride comprises the following steps:
(1) Accurately weighing 200g of alumina powder with the median particle size D50 of 0.35 mu m and 100g of nano carbon powder with the median particle size D50 of 50nm, adding 400g of alumina balls with the diameter of 10mm as grinding balls, placing the grinding balls in a mixing device, performing ball milling and mixing for 24 hours, and sieving to obtain a first mixture;
(2) Taking 200g of the first mixture after sieving, adding 30g of micron carbon powder with the median particle size D50 of 1 mu m, mixing for 30min twice, and sieving to obtain a second mixture;
(3) roasting the obtained second mixture for 10 hours at 1600 ℃ in a nitrogen atmosphere;
(4) And after the obtained roasted product is cooled, placing the obtained roasted product in a muffle furnace, carrying out heat preservation reaction for 3 hours at 680 ℃ under the air condition, carrying out oxidation and decarbonization to obtain high-purity aluminum nitride powder, and testing to obtain the powder with the oxygen content of 0.86%.
Example 8
the preparation method of the high-purity aluminum nitride comprises the following steps:
(1) Accurately weighing 200g of alumina powder with the median particle size D50 of 0.32 mu m and 85g of nano carbon powder with the median particle size D50 of 30nm, adding 1140g of alumina balls with the diameter of 20mm serving as grinding balls, placing the grinding balls in a mixing device, performing ball milling and mixing for 24 hours, and sieving to obtain a first mixture;
(2) taking 200g of the first mixture after sieving, adding 20g of micron carbon powder with the median particle size D50 of 4 mu m, mixing for the second time for 30min, and sieving to obtain a second mixture;
(3) Roasting the obtained second mixture for 15 hours at 1550 ℃ in a nitrogen atmosphere;
(4) and after the obtained roasted product is cooled, placing the obtained roasted product in a muffle furnace, carrying out heat preservation reaction for 2 hours at 750 ℃ under the air condition, carrying out oxidation and decarbonization to obtain high-purity aluminum nitride powder, and testing to obtain the powder with the oxygen content of 0.91%.
comparative example 1
The preparation method of the aluminum nitride in the comparative example is the same as that in example 1, and the difference is only that the carbon source adopts micron carbon powder with the same particle size, and the carbon source is added at one time for reaction to prepare the aluminum nitride powder. The aluminum nitride powder is obtained after oxidation and decarbonization, and the oxygen content in the powder is 1.13 percent through testing.
Comparative example 2
The preparation method of the aluminum nitride in the comparative example is the same as that in example 1, and the difference is only that the carbon source adopts micron carbon powder with the same particle size, and the carbon source is added at one time for reaction to prepare the aluminum nitride powder. The aluminum nitride powder is obtained after oxidation and decarbonization, and the oxygen content in the powder is 1.18 percent through testing.
A comparison of the experimental conditions of the respective steps of examples 1 to 8 and comparative examples 1 to 2 is shown in Table 1, and the oxygen contents of the aluminum nitride powders obtained in the above examples 1 to 8 and comparative examples 1 to 2 were measured according to the prior art method and are shown in Table 2 below.
TABLE 1 comparison of experimental conditions for different examples
TABLE 2 comparison of the oxygen contents of the aluminum nitride powders obtained in the different examples
| Examples | oxygen content of the obtained aluminum nitride powder |
| Example 1 | 0.85％ |
| example 2 | 0.92％ |
| Example 3 | 0.81％ |
| example 4 | 0.84％ |
| example 5 | 0.82％ |
| Example 6 | 0.83％ |
| Example 7 | 0.86％ |
| Example 8 | 0.91％ |
| Comparative example 1 | 1.13％ |
| comparative example 2 | 1.18％ |
As can be seen from the data in table 2 above, according to the high-purity nitride powder and the preparation method thereof provided by the invention, by using aluminum oxide as a raw material and performing a fractional mixing manner of mixing with nano-scale carbon powder for the first time and mixing with micro-scale carbon powder for the second time, more gaps can be formed in a reactant, the discharge of a high-temperature reaction product, namely carbon monoxide, and the exchange of reaction gas, namely nitrogen, with a solid-phase raw material are effectively promoted, the nitridation rate of the raw material is improved, and thus, high-purity aluminum nitride powder with low oxygen content is obtained.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A method for preparing high-purity aluminum nitride powder is characterized by comprising the following steps:
(1) taking aluminum oxide powder and a nano carbon source, adding grinding balls, fully mixing, and sieving to obtain a first mixture;
(2) adding a micron carbon source into the first mixture, fully mixing, and sieving to obtain a second mixture;
(3) Roasting the second mixture at 1550-;
(4) And (4) carrying out heat preservation reaction on the roasting product obtained in the step (3) at the temperature of 600-800 ℃ in the air atmosphere, and carrying out decarbonization treatment to obtain the high-purity aluminum nitride powder.
2. the method according to claim 1, wherein in the step (1), the alumina powder has a median particle diameter D50 of 0.2-0.4 μm.
3. The method for preparing high-purity aluminum nitride powder according to claim 1 or 2, wherein in the step (1), the nano-carbon source has a median particle diameter D50 of 10-50 nm.
4. The method for preparing high-purity aluminum nitride powder according to any one of claims 1 to 3, wherein in the step (1), the mass ratio of the aluminum oxide powder to the nano carbon source is 2: 0.6-1.0.
5. The method for preparing high-purity aluminum nitride powder according to any one of claims 1 to 4, wherein in the step (1), the grinding balls are alumina balls or aluminum nitride balls with the diameter of 5-20 mm.
6. The method for preparing high-purity aluminum nitride powder according to any one of claims 1 to 5, wherein in the step (1), the mass ratio of the grinding balls to the mixture of the aluminum oxide powder and the nano carbon source is 2: 0.5-1.5.
7. The method for preparing high-purity aluminum nitride powder according to any one of claims 1 to 6, wherein in the step (2), the micron carbon source has a median particle diameter D50 of 0.5 to 5 μm.
8. the method for preparing high-purity aluminum nitride powder according to any one of claims 1 to 7, wherein in the step (2), the mass ratio of the first mixture material to the micron carbon source is 2: 0.1-0.3.
9. The method for preparing high-purity aluminum nitride powder according to any one of claims 1 to 8, wherein in the step (3), the time of the roasting step is 8 to 15 hours.
10. The method for producing a high-purity aluminum nitride powder according to any one of claims 1 to 9, characterized in that: in the step (4), the time of the heat preservation reaction is 3-5 h.
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| CN113233432A (en) * | 2021-07-01 | 2021-08-10 | 东北大学 | Method for preparing aluminum nitride powder from secondary aluminum ash |
| CN113956051A (en) * | 2021-11-26 | 2022-01-21 | 厦门钜瓷科技有限公司 | Decarbonization method for preparing aluminum nitride powder by carbothermic method |
| CN114031052A (en) * | 2021-11-26 | 2022-02-11 | 厦门钜瓷科技有限公司 | Method for preparing low-oxygen-content aluminum nitride powder |
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