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A metallization method for aluminum nitride ceramics

A technology of aluminum nitride ceramics and metallization, which is applied in the field of ceramic metallization technology, can solve the problem of excessive oxidation of aluminum nitride ceramics, high sealing strength of aluminum nitride ceramic-metal seals, and easy hydrolysis of aluminum nitride ceramics and other problems, to achieve the effect of promoting reaction, good wetting, and high sealing tensile strength

Active Publication Date: 2020-06-02
INST OF FLUID PHYSICS CHINA ACAD OF ENG PHYSICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to provide a metallization method of aluminum nitride ceramics, which solves the problem of excessive oxidation of aluminum nitride ceramics caused by the metallization of aluminum nitride ceramics by the existing activated Mo-Mn method, and aluminum nitride in the sintering process. Ceramics are prone to hydrolysis, and oxidation and sintering are completed in one step, and the aluminum nitride ceramic-metal seals prepared have higher sealing strength

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] A method for metallizing aluminum nitride ceramics, comprising the steps of:

[0055] 1), prepare the activated Mo-Mn powder, the activated Mo-Mn powder has the following components by weight:

[0056] 80 parts by weight of Mo powder, 5 parts by weight of Mn powder, SiO 2 Powder 6 parts by weight, Al 2 o 3 Powder 6 parts by weight, CaCO 3 Powder 0.5 parts by weight;

[0057] Mix each powder in proportion and then carry out ball milling: use agate balls or alumina balls with a diameter of 5 mm to add absolute ethanol to ball mill for 72 hours, the ratio of the agate balls or alumina balls to absolute ethanol is 1:1, and the ball milled Rinse the Mo-Mn powder with alcohol, stir evenly, and let it stand for a few minutes. After the suspension settles, pour out the alcohol, repeat three times, and then dry the Mo-Mn powder at 80°C for 1 hour. Then grind and sieve under a 350-mesh sieve, wherein the laser particle size of the Mo powder is D 50 = 1μm, Mn powder laser pa...

Embodiment 2

[0063] 1), prepare the activated Mo-Mn powder, the activated Mo-Mn powder has the following components by weight:

[0064] 60 parts by weight of Mo powder, 10 parts by weight of Mn powder, SiO 2 Powder 15 parts by weight, Al 2 o 3 Powder 12 parts by weight, CaCO 3 Powder 3 parts by weight, MgO powder 0.5 parts by weight, BaCO 3 Powder 0.5 parts by weight, TiO 2 Powder 0.5 parts by weight;

[0065] Mix each powder in proportion and carry out ball milling: use agate balls or alumina balls with a diameter of 30mm to add absolute ethanol ball mill for 120h, the ratio of the agate balls or alumina balls to absolute ethanol is 2:1, the Rinse the Mo-Mn powder with alcohol, stir evenly, and let it stand for a few minutes. After the suspension settles, pour out the alcohol, repeat three times, and then dry the Mo-Mn powder at 150°C for 3 hours. Then grind and sieve under a 350-mesh sieve, wherein the laser particle size of the Mo powder is D 50 = 2μm, Mn powder laser particle si...

Embodiment 3

[0071] 1), prepare the activated Mo-Mn powder, the activated Mo-Mn powder has the following components by weight:

[0072] 70 parts by weight of Mo powder, 8 parts by weight of Mn powder, SiO 2 Powder 10 parts by weight, Al 2 o 3 Powder 8 parts by weight, CaCO 3 Powder 2 parts by weight, MgO powder 2 parts by weight, BaCO 3 Powder 1.5 parts by weight, TiO 2 Powder 1.5 parts by weight, Y 2 o 3 1 part by weight of powder;

[0073]After mixing the powders in proportion, carry out ball milling: use agate balls or alumina balls with a diameter of 20mm to add absolute ethanol ball mill for 100h, the ratio of the agate balls or alumina balls to absolute ethanol is 2:1, the ball milled Rinse the Mo-Mn powder with alcohol, stir evenly, and let it stand for a few minutes. After the suspension settles, pour out the alcohol, repeat three times, and then dry the Mo-Mn powder at 120°C for 2 hours. Then grind and sieve under a 350-mesh sieve, wherein the laser particle size of the Mo...

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Abstract

The invention discloses a metallizing method for aluminum nitride ceramic. The metallizing method comprises the following steps: 1) preparing activated Mo-Mn powder; 2) adding an organic carrier, andpreparing the activated Mo-Mn powder into metallized paste; 3) coating the surface of the aluminum nitride ceramic with the metallized paste; 4) ceramic oxidization and metallized layer sintering: introducing dry hydrogen or hydrogen-nitrogen mixed gas at a low temperature, introducing wet hydrogen or wet hydrogen-nitrogen mixed gas at the temperature of 900 DEG C, preserving heat at the temperature of 900 to 1,100 DEG C for 30 to 90 minutes, and controlling the dew point at 15+ / -5 DEG C to form an aluminum oxide layer on the surface of the aluminum nitride ceramic; then, continually heating,preserving heat at the temperature of 1,400 to 1,500 DEG C for 45 to 90 min, introducing dry hydrogen or hydrogen-nitrogen mixed gas in a heating stage, and controlling the dew point at 5+ / -10 DEG C.By adopting the metallizing method, the problems that the aluminum nitride ceramic is over-oxidized and the aluminum nitride ceramic is susceptible to hydrolysis in a sintering process due to metallization treatment of the aluminum nitride ceramic with an existing Mo-Mn method are solved. Moreover, oxidization and sintering are finished at one step, so that a prepared aluminum nitride ceramic-metal sealed part has higher sealing strength and high airtightness.

Description

technical field [0001] The invention relates to the technical field of ceramic metallization technology, in particular to a metallization method of aluminum nitride ceramics. Background technique [0002] Aluminum nitride (AlN) ceramics is a new type of ceramic material with broad application prospects, with high thermal conductivity (200-320W / (m K)), reliable electrical insulation (10 13 Ω·cm), low dielectric constant (8.7), low dielectric loss (1×10 -3 ) and high mechanical properties (350MPa) and a series of excellent features, are increasingly used in the field of electric vacuum devices. In order to make aluminum nitride ceramics more widely used in electric vacuum devices, welding between aluminum nitride ceramics and metals is often required. At present, there are many metallization and sealing methods for aluminum nitride ceramics, including active sealing method, chemical plating method, thick film method, thin film method, direct copper clad (DBC) method, co-firi...

Claims

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Application Information

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IPC IPC(8): C04B41/88C04B35/581
CPCC04B35/581C04B41/009C04B41/5138C04B41/88C04B41/4535C04B41/0072
Inventor 陈欣杨洁黄刚李天涛向军陈弹蛋刘平龙继东
Owner INST OF FLUID PHYSICS CHINA ACAD OF ENG PHYSICS
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