CN101890503B - Method for preparing fine Mo-Ru solder powder - Google Patents
Method for preparing fine Mo-Ru solder powder Download PDFInfo
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- CN101890503B CN101890503B CN2010102094819A CN201010209481A CN101890503B CN 101890503 B CN101890503 B CN 101890503B CN 2010102094819 A CN2010102094819 A CN 2010102094819A CN 201010209481 A CN201010209481 A CN 201010209481A CN 101890503 B CN101890503 B CN 101890503B
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Abstract
The invention discloses a method for preparing minuteness Mo-Ru solder powder by using a chemical coprecipitation method. The method comprises the following steps of: preparing solution of ruthenium trichloride and solution of ammonium molybdate respectively; mixing the solution of ruthenium trichloride and the solution of ammonium molybdate and drying the mixed solution at a low temperature; heating the obtained product to remove ammonium chloride; reducing the product with hydrogen; and grinding and sieving the product to prepare the required ingredient, namely Mo-Ru solder powder, wherein the particle size of 90 percent of the solder powder is less than or equal to 6 microns, and the maximum particle size is less than or equal to 10 microns. The Mo-Ru solder powder prepared by the method has the characteristics of fine solder powder (the particle size of 90 percent of the particles is less than or equal to 6 microns) and uniform ingredients, so that the method can solve the problems of non-uniform ingredients, poor manufacturability and the like existing in the use of the Mo-Ru solder in the prior art.
Description
Technical field
The present invention relates to the Mo-Ru manufacturing method of power, particularly relate to the preparation technology that the chemical reaction coprecipitation is made the fine Mo-Ru solder powder.
Background technology
Make the field at electron tube, using a kind of high-temp solder Mo-Ru solder alloy, the composition of solder is positioned at Mo-Ru eutectic point composition Mo-43.27Ru, and the solder fusing point is 1920～1980 ℃.
Because this composition alloy melting point is very high; Adopt traditional aerosolization method preparation to be difficult to realize; Therefore in existing technology, all adopt pure Mo powder and pure Ru powder to carry out mechanical mixture, process the Mo-Ru solder powder of designing requirement composition or prepare the Mo-Ru solder powder with Mo-Ru alloy pig Mechanical Crushing-polishing in the required ratio of alloy.Because the solder composition is positioned at eutectic composition, under the brazing temperature effect, the solder powder of mixing connects the soldering of mother metal through eutectic reaction fusing, completion.
Mo-Ru solder powder preparation method's deficiency is in the prior art: the solder uneven components of mechanical mixing preparation causes solder fusing pre-arcing characterisitics not good; Its granularity of fragmentation-polishing is big (>=30 microns), can not satisfy the use technological requirement that fine member applies.
Summary of the invention
The present invention can solve the existence in using of Mo-Ru solder in the prior art uneven components, use deficiencies such as manufacturability is not good enough.Mo-Ru solder powder of the present invention is to adopt the preparation of chemical reaction coprecipitation, and solder is by being the mixture that main body and a small amount of pure Mo, Ru particle are formed with molybdenum ruthenium compound particle.
The Mo-Ru solder powder of the inventive method preparation, not only fine (90% granularity≤6 micron), and 90% particle is the Mo-Ru compound; Thereby given the high uniformity that Mo and Ru distribute in the mixture; The carrying out of favourable two elements eutectic reaction under brazing temperature, favourable solder fusing and raising brazing characteristics, 90% particle≤6 micron fine solder powder; Also help solder and on meticulous member, apply, improved the use processing performance of solder.
Mo-Ru powder brazing alloy preparation method key step of the present invention is following:
Press the composition of Mo-Ru solder design, weigh ruthenium trichloride and ammonium molybdate; Process solution with distilled water or ionized water respectively; Two solution are mixed, dry at following mixed solution of 100～150 ℃ of temperature, and through following chemical reaction: 2RuCl
3+ (NH
4)
6Mo
70
24→ (Ru)
2Mo
7O
24↓+6NH
4C1 generates molybdic acid ruthenium and ammonium chloride, and then 400～600 ℃ of heating, through following chemical reaction: NH
4C1 → NH
3↑+HCl ↑, remove the ammonium chloride in the mixture, remaining molybdic acid ruthenium; Last molybdic acid ruthenium reduces processing with hydrogen at 900～950 ℃, through following chemical reaction generation Mo-Ru compound and Mo, Ru simple substance:
Chemical reaction 1: (Ru)
2Mo
7O
24+ 24H
2→ (Mo
7Ru
2)+24H
2O
Chemical reaction 2:2RuCl
3+ 3H
2→ 2Ru+6HCl ↑
Chemical reaction 3: (NH
4)
6Mo
7O
24+ 21H
2→ 7Mo+24H
2O+6NH
3↑
After the mixture cooling, the mixture with bulk grinds, sieves again, processes the Mo-Ru attritive powder solder of design mix.
The characteristics of the Mo-Ru solder powder of preparation method's preparation that the present invention proposes are: solder powder fine (90% particle≤6 micron), composition are even, thus can solve the existence during the Mo-Ru solder uses in the prior art uneven components, use deficiencies such as manufacturability is not good enough.The main body that the inventive method prepares the Mo-Ru solder powder is that Mo-Ru compound particle and a small amount of pure Mo, pure Ru particle are formed.Therefore, the Mo-Ru solder powder of the present invention's preparation is much more even than the solder composition of pure Mo of prior art and the preparation of pure Ru powder mechanical mixture.
The specific embodiment
1 one kinds of solder compositions of embodiment (mass fraction): 58%Mo-42%Ru solder powder preparation method; By solder designing quality mark is the composition of 58%Mo-42%Ru; According to ruthenium trichloride molecular formula and ammonium molybdate molecular formula; Wherein each atoms of elements amount calculates the required weight of ruthenium trichloride and ammonium molybdate, processes solution respectively, mixes to be incorporated under 100 ℃ of conditions and dry with distilled water then.Then, the mixture of drying is heated, remove ammonium chloride, heating is carried out at 400 ℃; At last, under hot conditions, with hydrogen mixture is reduced processing, treatment temperature is 900 ℃, and time: 2h after the mixture cooling, through grinding, sieving, processes required composition and specification Mo-Ru solder powder.
Adopt the granularity of the Mo-Ru solder powder of method for preparing; 90% powder size≤6 micron, maximum particle size≤10 micron, wherein 88% powder particle is to be made up of the Mo-Ru compound.
The composition of solder powder (mass fraction) testing result is: 57.7%Mo-42.3%Ru, the fusion temperature of solder: 1960～1980 ℃.
Embodiment 2:
A kind of solder composition (mass fraction): 56%Mo-44%Ru solder powder preparation method
Solder composition by design 56%Mo-44%Ru calculates the required weight of ruthenium trichloride and ammonium molybdate, processes solution respectively, mixes to be incorporated under 150 ℃ of conditions and dry with ionized water then.Then, the mixture of drying is heated, remove ammonium chloride, heating is carried out at 500 ℃; At last, under hot conditions, with hydrogen mixture is reduced processing, treatment temperature is 950 ℃.After the mixture cooling,, process the Mo-Ru solder powder of required composition and specification requirement through grinding, sieving.
The Mo-Ru of employing method for preparing adopts the granularity of the Mo-Ru solder powder of method for preparing; 92% powder size≤6 micron, maximum particle size≤9.4 micron, wherein 90% powder particle is to be made up of the Mo-Ru compound.
The composition of solder powder (mass fraction) testing result is: 56.4%Mo-43.6%Ru; The fusion temperature of solder: 1940～1983 ℃.
Claims (2)
1. method for preparing fine Mo-Ru solder powder, it is characterized in that: composition is mass fraction 58～56%Mo, 42～44%Ru, concrete preparation process is following:
(1) according to the requirement of Mo-Ru powder brazing alloy design mix, prepares ruthenium trichloride solution and ammonium molybdate solution respectively;
(2) ruthenium trichloride solution and ammonium molybdate solution are mixed, dry for 100 ℃ times;
(3) add ammonium chloride in the heat abstraction mixture;
(4) under 900 ℃, mixture is reduced with hydrogen; Obtain pure block Mo-Ru powder brazing alloy;
(5) after the cooling, block Mo-Ru solder is ground, sieves, make the fine solder powder of required Mo-Ru.
2. method for preparing fine Mo-Ru solder powder according to claim 1 is characterized in that: the granularity of said fine solder powder: wherein: 90% is 1～6 micron, and maximum particle size is no more than 10 microns.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102094819A CN101890503B (en) | 2010-06-25 | 2010-06-25 | Method for preparing fine Mo-Ru solder powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102094819A CN101890503B (en) | 2010-06-25 | 2010-06-25 | Method for preparing fine Mo-Ru solder powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101890503A CN101890503A (en) | 2010-11-24 |
| CN101890503B true CN101890503B (en) | 2012-05-30 |
Family
ID=43099934
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010102094819A Expired - Fee Related CN101890503B (en) | 2010-06-25 | 2010-06-25 | Method for preparing fine Mo-Ru solder powder |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103170764B (en) * | 2011-12-26 | 2015-02-18 | 北京有色金属研究总院 | Brazing filler alloy powder and preparation method thereof |
| CN103862190B (en) * | 2012-12-17 | 2016-04-27 | 北京有色金属研究总院 | A kind of negative electrode high-temperature brazing material and preparation method thereof |
| CN104014803B (en) * | 2014-05-26 | 2016-05-18 | 贵研铂业股份有限公司 | A kind of fine Mo-Ru-B solder powder and preparation method thereof |
| CN105834457B (en) * | 2016-05-27 | 2018-09-18 | 贵研铂业股份有限公司 | A kind of micron-size spherical Mo-Ru solder raw powder's production technologies |
| CN106624471B (en) * | 2016-12-29 | 2021-10-15 | 广东威特真空电子制造有限公司 | Mo-Ru solder, preparation method thereof and magnetron |
| CN112170858B (en) * | 2020-09-03 | 2023-04-07 | 重庆材料研究院有限公司 | Preparation method of Mo-Ru brazing filler metal powder |
| CN113025839B (en) * | 2021-03-03 | 2021-11-26 | 西北有色金属研究院 | Preparation method of microalloyed molybdenum-ruthenium alloy |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4859236A (en) * | 1988-04-25 | 1989-08-22 | Gte Products Corporation | Process for producing molybdenum-ruthenium metal powder |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS599278B2 (en) * | 1976-10-08 | 1984-03-01 | 株式会社日立製作所 | Manufacturing method for high temperature brazing materials |
| JPH0677874B2 (en) * | 1986-11-06 | 1994-10-05 | 田中貴金属工業株式会社 | Manufacturing method of brazing filler metal for magnetron |
-
2010
- 2010-06-25 CN CN2010102094819A patent/CN101890503B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4859236A (en) * | 1988-04-25 | 1989-08-22 | Gte Products Corporation | Process for producing molybdenum-ruthenium metal powder |
Non-Patent Citations (3)
| Title |
|---|
| JP昭53-45647A 1978.04.24 |
| JP特开昭63-119999A 1988.05.24 |
| 戴红.Mo和Ru纳米粉末的生长机制及热稳定性.《有色金属》.2002,第54卷57-60. * |
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|---|---|
| CN101890503A (en) | 2010-11-24 |
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