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Ceramic low-temperature active metallization paste, ceramic metallization method and vacuum electronic device prepared according to the method

A technology of ceramic metallization and active metal, which is applied in the field of metallization treatment, can solve the problems of thermal stress concentration at the brazing interface, cracking of the brazing interface, and high material cost, and achieve the goal of reducing sintering temperature, improving welding performance, and strong versatility Effect

Active Publication Date: 2021-09-17
BEIJING INST OF NONFERROUS METALS & RARE EARTH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, active solders are mainly classified into Ag-based, Cu-based, Au-based, Ni-based and other alloys. The temperature of Cu-based and Ni-based brazing ceramics exceeds 950°C. If the temperature is too high, the thermal stress on the brazing interface will be concentrated, and the occurrence of A large number of cracks, voids, etc., the Au base not only has a high temperature, but also is expensive and not suitable for promotion
The Ag base is mainly composed of AgCuTi alloys, in which the Ag content is basically greater than 70wt.%, and the material cost is high; the brazing temperature exceeds 850°C, and the temperature is relatively high; the linear expansion coefficient of the solder is greater than 15×10 -6 m / m.k, 2~5 times higher than the linear expansion coefficient of ceramics, it is easy to cause cracking of the brazing interface during brazing

Method used

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  • Ceramic low-temperature active metallization paste, ceramic metallization method and vacuum electronic device prepared according to the method
  • Ceramic low-temperature active metallization paste, ceramic metallization method and vacuum electronic device prepared according to the method
  • Ceramic low-temperature active metallization paste, ceramic metallization method and vacuum electronic device prepared according to the method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Example 1 Preparation of Low-Temperature Active Metallized Alumina Ceramics (1)

[0037] 1. Material preparation

[0038] Weigh Mo powder in proportion: 3g, binder: 8g, AgCuInTiLi alloy powder: 89g; wherein, binder is acetone: 0.4g, triethanolamine: 0.08g, cellulose nitrate: 7.52g; Mo powder particle size The particle size of AgCuInTiLi alloy powder is 25-45 μm.

[0039] The preparation method of AgCuInTiLi alloy powder is as follows:

[0040] (1) The raw materials are Ag, Cu, In, Ti, Li elemental metals with a purity of 99.99%;

[0041] (2) Preparation of InLi master alloy: according to the proportion of Li 5wt.%, and the balance of In, the non-vacuum melting method of medium frequency induction furnace is adopted, and the melting temperature is 400 °C;

[0042] (3) Preparation of AgCuInTiLi alloy powder: According to the ratio of Cu 21.5 wt.%, Ti 3.0wt.%, InLi 19wt.%, Ag balance ratio, adopt the medium frequency induction furnace vacuum melting method, the vacuum c...

Embodiment 2

[0050] Example 2 Preparation of Low-Temperature Active Metallized Alumina Ceramics (2)

[0051] 1. Material preparation

[0052] Weigh Mo powder in proportion: 5g, binder: 15g, AgCuInTiLi alloy powder: 80g; wherein, binder is acetone: 1.5g, triethanolamine: 0.45g, cellulose nitrate: 13.05g; Mo powder particle size The particle size of AgCuInTiLi alloy powder is 25-45 μm.

[0053] The preparation method of AgCuInTiLi alloy powder is as follows:

[0054] (1) The raw materials are Ag, Cu, In, Ti, Li elemental metals with a purity of 99.99%;

[0055] (2) Preparation of InLi master alloy: According to the proportion of Li 9wt.%, and the balance of In, the non-vacuum melting method of intermediate frequency induction furnace is adopted, and the melting temperature is 500 ° C to prepare InLi master alloy;

[0056] (3) Preparation of AgCuInTiLi alloy powder: According to the ratio of Cu 20 wt.%, Ti 5.0wt.%, InLi 24wt.%, and the balance of Ag, the medium frequency induction furnace ...

Embodiment 3

[0064] Example 3 Preparation of low-temperature active metallized alumina ceramics (3)

[0065] 1. Material preparation

[0066] Weigh Mo powder in proportion: 3g, binder: 8g, AgCuInTiLi alloy powder: 89g; wherein, binder is acetone: 0.4g, triethanolamine: 0.08g, cellulose nitrate: 7.52g; Mo powder particle size The particle size of AgCuInTiLi alloy powder is 25-45 μm.

[0067] The preparation method of AgCuInTiLi alloy powder is as follows:

[0068] (1) The raw materials are Ag, Cu, In, Ti, Li elemental metals with a purity greater than 99.99%;

[0069] (2) Preparation of InLi master alloy: According to the proportion of Li 8wt.%, and the balance of In, the non-vacuum melting method of intermediate frequency induction furnace is adopted, and the melting temperature is 500 °C to prepare InLi master alloy;

[0070] (3) Preparation of AgCuInTiLi alloy powder: according to the ratio of Cu 22 wt.%, Ti 4.5.0wt.%, InLi 22wt.%, and the balance of Ag, the medium frequency induction...

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Abstract

A ceramic low-temperature active metallization paste, a ceramic metallization method and a vacuum electronic device prepared according to the method. The composition of the paste is: Mo powder 3.0-5.0wt.%, binder 8.0-15.0wt.%, and AgCuInTiLi alloy powder as the balance. The preparation method comprises: preparing a paste body for low-temperature active metallization of ceramics, coating the paste body on the surface of the ceramics, drying the ceramics to remove the binder and sintering in vacuum. After ceramic active metallization treatment, a metal transition layer with a thickness of 40 μm to 60 μm can be formed on the surface, the weldability is improved, and the welding rate and welding strength are significantly improved. The treatment method is suitable for the metallization of various ceramics such as alumina, zirconia, beryllium oxide, boron nitride, etc. The method is simple, the operation process is short, the cost is low, and it is beneficial to mass production.

Description

technical field [0001] The invention relates to a low-temperature active metallization method for ceramics, in particular to metallization treatment before vacuum sealing of ceramics for vacuum electronic devices. Background technique [0002] Ceramics have the characteristics of high strength, high temperature resistance, corrosion resistance, wear resistance, electrical insulation and other performance characteristics, and have gradually developed into high-performance structural materials for engineering applications. Alumina ceramics, as shell materials and insulator materials, are one of the key components of vacuum electronic devices, and are widely used in radar electronics, power transmission, industrial power devices, electrified railways, microwave communications, nuclear fusion devices and other fields. [0003] Most solders neither wet nor react with ceramics to form a strong bond. In order to make a reliable connection between ceramics and metals, it is usually...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B41/88
CPCC04B41/515C04B41/88C04B41/5133C04B41/5127C04B41/5116
Inventor 黄晓猛陈立建张国清韩鹏焦磊王冉王峰
Owner BEIJING INST OF NONFERROUS METALS & RARE EARTH