Method for preparing aluminum nitride ceramic powder based on urea/melamine nitrogen source

A technology of melamine nitrogen source and aluminum nitride ceramics, which is applied in the field of materials, can solve problems such as hindering nitrogen diffusion, particle growth, and aluminum frit

Active Publication Date: 2019-03-08
SHENYANG UNIV
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Problems solved by technology

[0002] Aluminum nitride is a ceramic material with excellent comprehensive performance. With the deepening of research, the preparation technology of aluminum nitride is becoming more and more mature, and its application range is also expanding; especially since the 21st century, with the rapid development of microelectronics technology With the development, electronic machines and electronic components are developing towards the direction of miniaturization, light weight, integration, high reliability and high power output. high requirements; the thermal conductivity of traditional resin substrates and alumina ceramic substrates is below 30W / (m K), which is far from meeting the development needs of large-scale integrated circuits and complex devices; the theoretical thermal conductivity of aluminum nitride ceramics The conductivity is 320W / (m K), and it has good electrical insulation, low dielectric constant and dielectric loss, a good thermal expansion coefficient with silicon, good chemical stability, environmental protection and non-toxicity, etc. Advantages, has become the most ideal substrate material and electronic device packaging material
[0003] At present, the methods for producing aluminum nitride ceramic powder mainly include direct nitriding of aluminum powder, carbothermal reduction and high-energy ball milling; in the direct nitriding of aluminum powder, since the nitriding reaction of aluminum powder is a strong exothermic reaction, the reaction The process is not easy to control, and the large amount of heat released can easily cause aluminum to form a fused block, which hinders the diffusion of nitrogen, resulting in incomplete reaction, and the reaction product often needs to be pulverized, so it is difficult to synthesize high-purity, fine-grained products; in the carbothermal reduction method, The mixed powder of alumina and carbon is in high temperature, flowing N 2 Reductive nitriding reaction occurs in the air to generate AlN powder; the nitrogen source used in this method is a flowing inert gas—nitrogen, which requires a higher temperature (1500-1800°C) for the carbothermal reduction reaction to occur, resulting in particle growth and sintering activity. Reduced; it is easy to introduce impurities in the high-energy ball milling method, resulting in lower purity of the powder, and this method has not been widely used so far

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  • Method for preparing aluminum nitride ceramic powder based on urea/melamine nitrogen source
  • Method for preparing aluminum nitride ceramic powder based on urea/melamine nitrogen source

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Prepare aluminum source nonahydrate aluminum nitrate, precipitation agent ammonium bicarbonate solution, concentration of 0.1M; surfactant coupling agent and polyethylene glycol, carbon source phenolic resin, nitrogen source urea; wherein the coupling agent is nonahydrate aluminum nitrate 0.01% of the total mass, polyethylene glycol is 0.011% of the total mass of aluminum nitrate nonahydrate, the molar ratio of phenolic resin to aluminum nitrate nonahydrate is 1.2, the molar ratio of urea to aluminum nitrate nonahydrate is 3, the amount of precipitation agent The molar ratio of ammonium bicarbonate to aluminum nitrate nonahydrate is 8; the polymerization degree of polyethylene glycol is 6000;

[0035] Dissolve aluminum nitrate nonahydrate in deionized water, then add coupling agent and polyethylene glycol, and stir to make a mixed solution; the amount of deionized water can completely dissolve aluminum nitrate nonahydrate, coupling agent and polyethylene glycol Prevail

[0...

Embodiment 2

[0041] The method is the same as in Example 1, the difference is:

[0042] (1) The precipitation agent is ammonia water with a concentration of 0.1M; the nitrogen source is melamine; the coupling agent is 1% of the total mass of aluminum nitrate nonahydrate, polyethylene glycol is 1% of the total mass of aluminum nitrate nonahydrate, phenolic resin and The molar ratio of aluminum nitrate nonahydrate is 3, the molar ratio of melamine to aluminum nitrate nonahydrate is 6, and the amount of precipitant is NH 3 ·H 2 The molar ratio of O to aluminum nitrate nonahydrate is 8; the degree of polymerization of polyethylene glycol is 8000;

[0043] (2) Drying temperature 80℃, time 10 hours; calcination temperature 400℃, time 2 hours;

[0044] (3) Nitriding synthesis reaction temperature is 1000℃, time is 2 hours;

[0045] (4) The coarse aluminum nitride powder is kept at 620°C for 4 hours to remove carbon; the particle size of the aluminum nitride ceramic powder is 280-430 nanometers.

Embodiment 3

[0047] The method is the same as in Example 1, the difference is:

[0048] (1) The concentration of the precipitation agent ammonium bicarbonate solution is 2M; the coupling agent is 5% of the total mass of aluminum nitrate nonahydrate, polyethylene glycol is 5% of the total mass of aluminum nitrate nonahydrate, phenolic resin and aluminum nitrate nonahydrate The molar ratio of urea is 6, the molar ratio of urea to aluminum nitrate nonahydrate is 12, the amount of precipitant is 2 according to the molar ratio of ammonium bicarbonate to aluminum nitrate nonahydrate; the degree of polymerization of polyethylene glycol is 20,000;

[0049] (2) Drying temperature 60℃, time 48 hours; calcination temperature 300℃, time 4 hours;

[0050] (3) Nitriding synthesis reaction temperature is 1050℃, time is 2 hours;

[0051] (4) The coarse aluminum nitride powder is kept at 600°C for 3 hours to remove carbon; the particle size of the aluminum nitride ceramic powder is 300-500 nanometers.

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Abstract

The invention relates to a method for preparing aluminum nitride ceramic powder based on a urea/melamine nitrogen source. The method comprises the following steps: (1) preparing raw materials; (2) dissolving aluminum nitrate nonahydrate into water, adding a coupling agent and polyethylene glycol and uniformly stirring; (3) adding a precipitant, stirring to form a precursor gel, and filtering afteralcohol washing to obtain a gel; (4) putting the gel into absoluteethyl alcohol, adding phenolic resin under a stirring condition, stirring to form a paste body, baking, calcining and grinding to obtain a precursor powder; (5) grinding and mixing with a nitrogen source, placing into a heating furnace, increasing temperature to 950-1500 DEG C for performing nitridation synthesis when the air pressure in the heating furnace is higher than barometric pressure, performing furnace cooling, and grinding to obtain rough powder; and (6) and heating to 550-650 DEG C for removing carbon. According to the method provided by the invention, high-activity urea/melamine instead of nitrogen is taken as a nitrogen source, and a surface modification dispersion technology is adopted, so that atom- or molecule-level uniform mixing between an aluminum source and a carbon source is realized, and the temperature of carbon thermal reduction reaction is lowered.

Description

Technical field [0001] The invention belongs to the technical field of materials, and particularly relates to a method for preparing aluminum nitride ceramic powder based on a urea / melamine nitrogen source. Background technique [0002] Aluminum nitride is a ceramic material with excellent comprehensive properties. With the continuous deepening of research, the preparation process of aluminum nitride has become more mature and its application scope has been expanding; especially since the 21st century, with the rapid development of microelectronics technology With the development, electronic complete machines and electronic components are moving towards miniaturization, light weight, integration, and high reliability and high power output. More and more complex devices have improved the heat dissipation of substrates and packaging materials. High requirements; the thermal conductivity of traditional resin substrates and alumina ceramic substrates is below 30W / (m·K), which is far ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/581C04B35/626
CPCC04B35/581C04B35/6265C04B2235/48
Inventor 张宁马洋洋
Owner SHENYANG UNIV
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