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Paste used for ceramic low-temperature activity metallization, ceramic metallization method and vacuum electronic device prepared according to method

A technology of ceramic metallization and active metal, applied in the field of metallization treatment, can solve the problems of thermal stress concentration at the brazing interface, cracking of the brazing interface, high material cost, achieve strong bonding force, improve ceramic welding performance, and simple method. Effect

Active Publication Date: 2019-02-26
BEIJING INST OF NONFERROUS METALS & RARE EARTH
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  • 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, which is 2 to 5 times higher than the linear expansion coefficient of ceramics, and it is easy to cause cracking of the brazing interface during the brazing process

Method used

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  • Paste used for ceramic low-temperature activity metallization, ceramic metallization method and vacuum electronic device prepared according to method
  • Paste used for ceramic low-temperature activity metallization, ceramic metallization method and vacuum electronic device prepared according to method
  • Paste used for ceramic low-temperature activity metallization, ceramic metallization method and vacuum electronic device prepared according to method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Example 1 Preparation of low-temperature active metallized alumina ceramics (1)

[0037] 1. Prepare materials

[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) Raw material selection purity is 99.99% Ag, Cu, In, Ti, Li elemental metal;

[0041] (2) Preparation of InLi master alloy: according to the ratio of Li 5wt.%, In balance, using a non-vacuum melting method in an intermediate frequency induction furnace, the melting temperature is 400 ° C;

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

Embodiment 2

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

[0051] 1. Prepare materials

[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) Raw material selection purity is 99.99% Ag, Cu, In, Ti, Li elemental metal;

[0055] (2) Preparation of InLi master alloy: according to the ratio 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 the InLi master alloy;

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

Embodiment 3

[0064] Example 3 Preparation of Low Temperature Active Metallized Alumina Ceramics (3)

[0065] 1. Prepare materials

[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 ratio of Li 8wt.%, and the balance of In, the non-vacuum smelting method of intermediate frequency induction furnace is adopted, and the melting temperature is 500 ° C to prepare the InLi master alloy;

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

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Abstract

The invention discloses a paste used for ceramic low-temperature activity metallization, a ceramic metallization method and a vacuum electronic device prepared according to the method. The paste consists of 3.0wt% to 5.0wt% of a Mo powder, 8.0wt% to 15.0wt% of a binder and the balance of an AgCuInTiLi alloy powder. The preparation method comprises the following steps: preparing the paste used forceramic low-temperature activity metallization, enabling ceramic surface to be coated with the paste, drying ceramic to remove the binder, and carrying out vacuum sintering. After ceramic activity metallization treatment, a metal transition layer with the thickness of 40 to 60 microns can be generated on the surface, the weldability is improved, and the welding rate and welding strength are improved obviously. The treatment method is applicable to the metallization of various ceramics such as aluminum oxide, zirconium oxide, beryllium oxide and boron nitride, the method is simple, the operational process is short, the cost is low, and the volume production is facilitated.

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 Applications(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
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