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Sealing method for ceramic vitrification

A technology of ceramic glass and glass, which is applied in the sealing field of ceramic vitrification, can solve the problems of increased cost and difficulty, certain requirements for control, and difficulty in guaranteeing the airtightness, stability and reliability of the sealing interface, etc. Achieve good air tightness, reduce energy consumption, and high interface stability

Active Publication Date: 2015-01-14
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

First of all, the ceramic metallization process needs to be sintered and solidified at high temperature in a reducing atmosphere, which has certain requirements for the control of the atmosphere, which undoubtedly increases the cost and difficulty of the operation; secondly, the sealing parts obtained by using the ceramic metallization process are used for metal When molybdenum or tungsten has a certain corrosive environment, it will be difficult to guarantee the airtightness, stability and reliability of the sealing interface; in addition, the sealing parts obtained by using ceramic metallization process contain multiple interface layers at the sealing place (such as the interface between the ceramic part and the metallization layer, the interface between the metallization layer and the solder, the interface between the solder and the metal part), and the interface layer is the weakest part of the entire seal, so the ceramic metallization Sealing technology puts forward higher requirements for the control of the sealing process

Method used

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  • Sealing method for ceramic vitrification

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0027] (1) Preparation of glass powder with matching thermal expansion coefficient

[0028] Based on conventional borosilicate glass, the basic component is SiO 2 , B 2 o 3 or H 3 BO 3 、Al 2 o 3 , R 2 O or R 2 CO 3 (R 2 O is for Li 2 O, Na 2 O, K 2 One or more of O, R 2 CO 3 for Li 2 CO 3 、Na 2 CO 3 、K 2 CO 3 One or more of them), and according to the composition and thermal expansion coefficient of the ceramic matrix, add MgO, Bi 2 o 3 , ZrO 2 、TiO 2 Control the composition and thermal expansion coefficient of the glass to match the ceramic matrix; melt all the raw materials at a high temperature of 1200-1600°C for 30-360 minutes; obtain glass slag after rapid cooling; the glass slag is ball milled and sieved Finally, glass powder is obtained, preferably the particle size of the glass powder is 2-200 μm.

[0029](2) Mix the glass powder in step (1) with a binder and a solvent to make a paste. The binder includes but not limited to polyvinyl butyral (...

Embodiment 1

[0042] (a) Preparation of glass frits with matched thermal expansion coefficients

[0043] beta-Al 2 o 3 The coefficient of thermal expansion is 6~7×10 -6 K -1 (25~300℃), select the thermal expansion coefficient to match it and the composition contains Al 2 o 3 borosilicate glass as sealing glass. SiO 2 、Al 2 o 3 、H 3 BO 3 、Na 2 CO 3 、K 2 CO 3 , Li 2 CO 3 、 Bi 2 o 3 According to composition SiO 2 :Al 2 o 3 :B 2 o 3 : Na 2 O:K 2 O: Li 2 O: Bi 2 o 3 =40:3:18:3:3:1:32 for batching; use absolute ethanol as the medium, ball mill for 4 hours, dry; sinter at 800°C for 2 hours, and then melt at 1400°C for 2 hours; After cooling, glass slag is obtained; the glass slag is ball milled and sieved to obtain glass powder, preferably with a particle size of 10-20 μm. The coefficient of thermal expansion of the glass powder at 25-300°C is 6.2×10 -6 K -1 .

[0044] (b) Preparation of glass paste

[0045] Using absolute ethanol as solvent and PVB with a weight r...

Embodiment 2

[0053] (a) Preparation of glass powder with matching coefficient of thermal expansion: same as Example 1;

[0054] (b) Preparation of glass paste: use a mixture of ethanol and terpineol (1:4) as a solvent, and EC with a weight ratio of 3% as a binder, and prepare the glass powder obtained in (a) so that the composition is uniform ointment;

[0055] (c) same as embodiment 1;

[0056] (d) Vitrification of the surface of the sealing part of the ceramic sealing element: same as in Example 1;

[0057] (e) Sealing of ceramics and metals: same as Example 1;

[0058] The detection results of the helium mass spectrometer leak detector show that the helium leakage rate of the seal is 10 -11 Pa·m 3 ·s -1 ; Mechanical performance test results show that the seal strength of the seal is about 91MPa.

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Abstract

The invention relates to a sealing method for ceramic vitrification. The sealing method comprises the following steps: preparation of glass powder matched with thermal expansion coefficient of a ceramic substrate: during preparation of borosilicate glass, adding compositions of the ceramic substrate and adjusting compositions for adjusting thermal expansion coefficient into basic ingredients, ball-milling and evenly mixing, smelting, cooling and ball-milling to obtain the glass powder; preparation of a ceramic vitrification sealing part: mixing the glass powder with a binder and a solvent, then blending into paste, evenly coating on the sealing surface of the ceramic substrate to form a glass coating layer, and performing thermal treatment under air atmosphere to obtain the ceramic vitrification sealing part; and matching the ceramic vitrification sealing part with a to-be-sealed metal component and then sealing under inert atmosphere.

Description

technical field [0001] The invention relates to a method for vitrifying ceramics and then sealing them with metals. Background technique [0002] The application of ceramic and metal sealing technology in modern industrial technology is of great significance. Not only is it a key process in vacuum electronic devices, but its application scope is becoming wider and wider. It is also widely used in integrated circuit packaging, atomic energy, high-energy physics, energy, medical equipment, chemical industry, automobile industry, national defense technology and other fields. Ceramic and metal sealing technology has doubled development with the intersection of multiple disciplines. It is an extension of material application and a basic technology with strong craftsmanship and practicability. With the development of vacuum electronic devices in the direction of high power and the increasing application of ceramic and metal sealing technology, higher requirements are put forward ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B37/02C03C8/24
Inventor 温兆银吴相伟鹿燕胡英瑛张敬超吴梅芬
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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