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Method for improving ceramic metallized layer microstructure

A technology of ceramic metallization and microstructure, which is applied in the field of improving the microstructure of ceramic metallization layer, can solve the problems that the molybdenum powder particles are difficult to reach the nanometer level, and the mixing of ceramic metallization powder is uneven, and the reaction process is simple and easy to control , the effect of avoiding environmental pollution

Inactive Publication Date: 2009-01-28
UNIV OF SCI & TECH BEIJING
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to solve the problem of uneven mixing of ceramic metallization powder and difficulty in reaching the nanometer level of molybdenum powder particles, and to provide a glass powder required for ceramic metallization in the process of preparing ultrafine molybdenum powder by uniform precipitation method, thereby A method for obtaining a ceramic metallization powder that is uniformly mixed and the particle size of the molybdenum powder reaches nanoscale, and the ideal microstructure of the ceramic metallization layer can be obtained by using the ceramic metallization powder for ceramic metallization sintering

Method used

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  • Method for improving ceramic metallized layer microstructure
  • Method for improving ceramic metallized layer microstructure
  • Method for improving ceramic metallized layer microstructure

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Experimental program
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Effect test

Embodiment 1

[0028] 1) take by weighing analytically pure ammonium paramolybdate, add deionized water, be made into the ammonium molybdate solution that concentration is 1.0mol / l;

[0029] 2) adding ammonia water to adjust the pH value to make the pH value 6;

[0030] 3) Add polyvinylpyrrolidone (PVP) and oxalic acid, wherein the mass ratio of ammonium paramolybdate to PVP and oxalic acid is 79:1:20 respectively; after making it completely dissolved, add a certain proportion of glass powder to make Mo: Mn: glass The mass ratio of powder is 70:9:21;

[0031] 4) inject nitric acid and stir to obtain a white gel;

[0032] 5) Put the white gel in an oven and bake it at 100°C for 2 hours to prepare the precursor;

[0033] 6) The precursor was reduced with dry hydrogen in a tube furnace, the hydrogen dew point was -10°C, the reduction time was 1 hour, and the reduction temperature was 700°C;

[0034] 7) Add Mn powder in proportion to the reduced powder for mixing, so that the mass ratio of Mo...

Embodiment 2

[0038] 1) take by weighing analytically pure ammonium paramolybdate, add deionized water, be made into the ammonium molybdate solution that concentration is 2.5mol / l;

[0039] 2) adding ammonia water to adjust the pH value to make the pH value 7;

[0040] 3) Add PVP and oxalic acid in proportion, wherein the mass ratio of ammonium paramolybdate to PVP and oxalic acid is 66: 2: 32 respectively; after making it completely dissolved, add a certain proportion of glass powder to make Mo: Mn: the quality of glass powder The ratio is 85:4.5:10.5;

[0041] 4) Inject hydrochloric acid and stir to obtain a white gel;

[0042] 5) Put the white gel in an oven and bake it at 200°C for 1 hour to prepare the precursor;

[0043] 6) The precursor was reduced with dry hydrogen in a tube furnace, the hydrogen dew point was -30°C, the reduction time was 0.45 hours, and the reduction temperature was 750°C;

[0044] 7) Adding Mn powder in proportion to the reducing powder for mixing, so that the...

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Abstract

The invention belongs to the technical field of ceramics and metals sealing, which particularly relates to a method for mixing ceramic metalizing powder by a liquid phase method. The method comprises the following steps: glass powder needed by the ceramic metallization is added in the course of preparing ultrafine molybdenum powder by homogeneous precipitation method so that the glass powder can be mixed in solution, thus obtaining evenly mixed ceramic metalizing powder with the particle size of the molybdenum powder being nano grade, and then a perfect microstructure of the ceramic metalizing layer can be obtained by carrying out ceramic metallization sintering on the ceramic metalizing powder. The method is characterized in that ammonium molybdate solution with certain concentration is made from analytically pure ammonium paramolybdate, the solution is added with ammonia water to regulate the PH of the solution, then added with PVP and oxalic acid in proportion, added with the glass powder needed by the ceramic metallization when the PVP and the oxalic acid are fully dissolved, and then injected with strong acid and stirred to obtain white gel; the white gel is baked and carries out low temperature reduction, then Mn powder is added and mixed into the ceramic metalizing powder, and then the ceramic metallization sintering is carried out, thus the perfect microstructure of the ceramic metalizing layer is obtained.

Description

technical field [0001] The invention belongs to the technical field of ceramic-metal sealing, and in particular relates to a method for mixing ceramic metallization powder by a liquid phase method, that is, adding glass powder required for ceramic metallization in the process of preparing ultrafine molybdenum powder by a uniform precipitation method, so that The metal and ceramic powders in the ceramic metallization powder are evenly mixed, and the particles of the molybdenum powder reach the nanoscale, thereby obviously improving the microstructure of the ceramic metallization layer. Background technique [0002] Ceramic-metal sealing technology is widely used in the manufacture of vacuum electronic devices such as electron tubes and vacuum switch tubes, among which the most critical technology is ceramic metallization. There are many kinds of ceramic metallization processes, such as metal powder sintering method, deposition method, etc., which can be roughly divided into t...

Claims

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Application Information

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IPC IPC(8): C04B37/02
Inventor 郝俊杰陈敏郭志猛李美霞其其格
Owner UNIV OF SCI & TECH BEIJING