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Method for synthesizing aluminum nitride ceramic powder at low temperature based on surface modification

A technology of aluminum nitride ceramics and surface modification, which is applied in the field of materials, can solve the problems of easy leakage, uniform mixing, and low synthesis temperature, and achieve the effects of wide application prospects, increased compatibility, and low synthesis temperature

Active Publication Date: 2022-03-25
沈阳金瓷科技开发有限责任公司
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AI Technical Summary

Problems solved by technology

[0002] With the rapid development of microelectronics technology, electronic machines and electronic components are developing in the direction of miniaturization, light weight, integration, high reliability and high power output. The heat dissipation of packaging materials puts forward higher 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 is 320W / (m K), and it has good electrical insulation, low dielectric constant and dielectric loss, a thermal expansion coefficient that matches silicon well, and has good chemical properties. With the advantages of stability, environmental protection and non-toxicity, it has become the most ideal substrate material and electronic device packaging material
[0003] The easiest way to produce aluminum nitride powder is the carbothermal reduction method, that is, using alumina as the aluminum source, adding a part of carbon through mechanical mixing, and under high-temperature flowing nitrogen, a carbothermal reduction reaction occurs to form aluminum nitride. Method; the finer the particle size and the higher the activity of alumina powder, the lower the synthesis temperature; the more uniform the mixing of aluminum source, carbon source and nitrogen source, the lower the synthesis temperature required for the synthesis of aluminum nitride powder ; but the existing problem is that the finer the particle size of alumina powder, the easier it is to agglomerate, and the more difficult it is to achieve uniform mixing between the aluminum source and the carbon source, so it is necessary to disperse the alumina powder; on the other hand, alumina powder It is an inorganic material, while the carbon source (such as sucrose or phenolic resin) is an organic material, and the inorganic and organic materials cannot be uniformly mixed by mechanical mixing. Therefore, it is also necessary to modify the surface of the alumina powder to make the aluminum source and carbon source phase In order to ensure that the aluminum source and carbon source are evenly mixed; in addition, people focus on the aluminum source and carbon source, while the influence of nitrogen source is often not taken seriously
So far, the nitrogen sources used are flowing nitrogen or ammonia. Nitrogen is an inert gas, which is a main reason for the high temperature of the carbothermal reduction reaction, while ammonia is a highly corrosive gas that is easy to leak, which poses a threat to production safety and the environment. Protection poses a great threat

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  • Method for synthesizing aluminum nitride ceramic powder at low temperature based on surface modification
  • Method for synthesizing aluminum nitride ceramic powder at low temperature based on surface modification

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Experimental program
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Effect test

Embodiment 1

[0029] Prepare aluminum source alumina superfine powder, catalyst ammonia, surfactant coupling agent and polyethylene glycol; wherein the particle diameter of alumina superfine powder is 40 nanometers, and the mass concentration of ammonia is 5%; ammonia is alumina superfine 25% of the mass of the fine powder, the coupling agent is 1% of the mass of the alumina ultrafine powder, polyethylene glycol is 1% of the mass of the alumina ultrafine powder; the degree of polymerization of polyethylene glycol is 20,000;

[0030] Put the alumina ultrafine powder in absolute ethanol and stir until a slurry is formed; add ammonia water, coupling agent and polyethylene glycol to the slurry in sequence, and stir for 2 hours. Under the action of ammonia water, the surface active The surface modification and dispersion of ultrafine alumina powder is carried out with the agent; the amount of anhydrous ethanol is based on the complete dissolution of the coupling agent and polyethylene glycol;

...

Embodiment 2

[0037] Method is with embodiment 1, and difference is:

[0038] (1) The mass concentration of ammonia water is 10%; ammonia water is 10% of the quality of alumina superfine powder, the coupling agent is 3% of the quality of alumina superfine powder, and polyethylene glycol is alumina superfine powder 3% by mass; the degree of polymerization of polyethylene glycol is 4000;

[0039] (2) Stir for 3 hours after adding ammonia water, coupling agent and polyethylene glycol;

[0040] (3) Stir in absolute ethanol for 30 minutes after the material is filtered;

[0041] (4) The paste is dried at 100°C; the molar ratio of phenolic resin to alumina ultrafine powder is 4;

[0042] (5) The mol ratio of nitrogen source urea and alumina superfine powder is 40;

[0043] (6) Purge with argon gas; heat up to 1000°C, keep warm for 3 hours to carry out nitriding synthesis;

[0044] (7) Insulate at 600° C. for 4 hours to remove carbon, and the particle size of the aluminum nitride ceramic powde...

Embodiment 3

[0046] Method is with embodiment 1, and difference is:

[0047] (1) The particle diameter of the alumina superfine powder is 30 nanometers, and the mass concentration of ammonia water is 15%; the ammonia liquor is 15% of the quality of the alumina superfine powder, and the coupling agent is 5% of the quality of the alumina superfine powder , polyethylene glycol is 5% of the quality of alumina ultrafine powder; the degree of polymerization of polyethylene glycol is 6000;

[0048] (2) Stir for 4 hours after adding ammonia water, coupling agent and polyethylene glycol;

[0049] (3) Stir in absolute ethanol after filtering the material for 60 minutes;

[0050] (4) The paste is dried at 150°C; the molar ratio of the phenolic resin to the superfine alumina powder is 5;

[0051] (5) The nitrogen source is melamine, and the mol ratio with the alumina superfine powder is 30;

[0052] (6) be heated up to 1050 ℃, keep warm for 3 hours and carry out nitriding synthesis;

[0053] (7) I...

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Abstract

A method for synthesizing aluminum nitride ceramic powder at low temperature based on surface modification, which is carried out in the following steps: (1) prepare aluminum source alumina ultrafine powder, ammonia water, coupling agent and polyethylene glycol; (2) prepare Put the alumina ultrafine powder in absolute ethanol and stir to form a slurry; add ammonia water, coupling agent and polyethylene glycol and stir; (3) filter and then stir in absolute ethanol, and separate and remove by secondary filtration liquid phase; (4) add phenolic resin to absolute ethanol under stirring condition, and stir to form a paste; grind after drying; (5) grind and mix with nitrogen source; (6) air pressure in the heating furnace Raise the temperature to 950-1500°C under the atmospheric pressure to carry out the nitriding synthesis reaction; cool with the furnace; (7) remove carbon under the condition of 550-650°C. The method of the invention has low synthesis temperature, environmental protection and low cost, and has wide application prospects.

Description

technical field [0001] The invention belongs to the technical field of materials, in particular to a method for synthesizing aluminum nitride ceramic powder at low temperature based on surface modification. Background technique [0002] With the rapid development of microelectronics technology, electronic machines and electronic components are developing in the direction of miniaturization, light weight, integration, high reliability and high power output. The heat dissipation of packaging materials puts forward higher 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 is 320W / (m K), and it has good electrical insulation, low dielectric constant and dielectric loss, a thermal expansion coefficient that matches silicon well, and has good c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/072C04B35/581C04B35/626
CPCC01B21/0726C04B35/581C04B35/62675C04B35/6268C01P2004/61C01P2004/62
Inventor 张宁茹红强茹敬雨
Owner 沈阳金瓷科技开发有限责任公司
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