CN1796580B - Technique for preparing new type getter containing zirconium - Google Patents
Technique for preparing new type getter containing zirconium Download PDFInfo
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- CN1796580B CN1796580B CN 200410081543 CN200410081543A CN1796580B CN 1796580 B CN1796580 B CN 1796580B CN 200410081543 CN200410081543 CN 200410081543 CN 200410081543 A CN200410081543 A CN 200410081543A CN 1796580 B CN1796580 B CN 1796580B
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- getter
- zirconium
- zrh
- preparation
- hydrogen
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Abstract
This invention relates to a preparation process of new efficient getters which are made of zirconium and zirconium-contained alloy or nonmetallic composites. First, spongy zirconium is processed intoZrHx by means of hydrogen absorption and then ZrHx is mixed with zirconium alloy powders or nonmetals and molded. Finally, the consequent matter is directly made into getters with different shapes after dehydrogenation or repeated hydrogen adsorption-desorption.
Description
What the present invention relates to is a kind of new preparation process of efficient getter, and this getter is made up of zirconium powder and Zirconium alloy material or nonmetal (graphite) matrix material.Can be used for vacuum heat insulation material, vacuum electron device, high purity inert gas preparation and is essential and removes N
2, O
2, H
2, CO, CO
2, CH
4, H
2The place of O steam and metallic insulator etc.
Traditional preparation method who contains zirconium getter be adopt the powder metallurgical method with high-purity zirconium powder and other metal or nonmetally be mixed in proportion, moulding through the high temperature high vacuum and under the filling with inert gas protection melting be smelt alloy or sintering forms, and then broken, grind and make varigrained powder and make air suction element again.Traditional operational path is seen accompanying drawing 1.
The shortcoming of traditional preparation process route is active high because of zirconium powder, in process such as pulverizings be subject to obnoxious flavour in storing and stain, also is difficult to its high purity of assurance in the organic reagent even be kept at.Traditional in addition nonmetal composition that contains in the zirconium getter is a graphite, and graphite is a kind of thinner, does not play getter action.
What the present invention relates to is another kind of novel technical route, efficient getter.Adopt the method for absorption hydrogen that zirconium sponge is made ZrH earlier
x, again with zirconium alloy getters such as Zr-V-Fe or nonmetally mix aftershaping as aerogel carbon dust, activated carbon powder, graphite etc., dehydrogenation and make the difform air suction element that contains activated zr in a vacuum.Take by weighing a certain amount of zirconium sponge during operation earlier, be evacuated down to 10
-2Handkerchief keeps stopping to vacuumize after 0.5 hour, put into hydrogen and inhale H-H reaction promptly at hydrogen pressure 0.1MPa, flow 0.5-1.0 liter/minute, kept under the 600-1200 ℃ of condition 1-4 hour, after hydrogen pressure remains unchanged, slowly be cooled to 100 ℃, come out of the stove ZrH
xFinish suction hydrogen, make ZrH
xAfter, take by weighing ZrH by predetermined proportion
xWith alloy powder or non-metal powder, being blended in the 100-300MPa forming under the pressure through screening is green compact.Green compact are inserted alloy crucible be evacuated to 10 in vacuum oven
-2-10
-4Handkerchief is warming up to 500-900 ℃ of dehydrogenation.Because dehydrogenation, vacuum tightness begin to descend, and continue to vacuumize until returning to 10
-2-10
-4Handkerchief is stablized after 0.5-1 hour and is reduced to room temperature, ZrH in the green compact
xBe that the dehydrogenation fragmentation is a high reactivity Zr powder.Do not reach requirement as Zr powder degree, again blank is inserted alloy crucible and in vacuum oven, inhale hydrogen and promptly be evacuated to 10
-2Handkerchief stops to bleed, and feeding high-purity hydrogen (99.99%) to pressure is 0.1MPa, is warming up to 600-1200 ℃ and keeps 1-4 hour, generates ZrH this moment again
xAfter, be cooled to the 500-900 degree again, stop logical hydrogen, be evacuated to 10 simultaneously
-2-10
-4Handkerchief rises to 10 again again through breaking of vacuum
-2-10
-4Handkerchief and be stabilized in the certain embodiments of this vacuum tightness certain hour after, be chilled to room temperature.So inhale hydrogen-dehydrogenation, repeat 2-5 back granularity and promptly reach requirement.The zirconium powder median size is 200-300nm.The bulk porosity is greater than 50%.
Operational path of the present invention is seen accompanying drawing 2.
Characteristics of the present invention:
1. adopt the active zirconium powder of suction-desorption hydrogen flow preparation, inhale hydrogen earlier and prepare intermediate product ZrH
x
2.ZrH
xPowder is in the early stage process, and stable chemical performance is difficult for polluting, so needn't be stored in the organic reagent.
3. contain ZrH
xGreen compact be dehydrogenated to newborn zirconium powder in a vacuum, surface-area is big, and is active big, easy-formation, mold temperature is low, and is energy-conservation.
4. one of its important feature is the Graphite Powder 99 of employing carbon aerogels replacement traditional product employing etc.This carbon aerogels not only plays diluting effect and itself is that a kind of specific surface area is greater than 500m
2/ g forms the special carbon material getter of network structure by the pore of nano aperture, and it is active big, and inspiratory capacity is big.
5. the air suction element product performance that adopt this composition and processing method to prepare are better than the product of traditional product and traditional method preparation, itself are a kind of porous inseries, and its overall porosity is greater than 50%, and the surface is much larger than 1m
2/ g.High reactivity zirconium, zirconium alloy and carbon aerogels are can dual stack air-breathing.Because of its activity is higher, diffusion activation energy is lower, and the room temperature pumping property is better, the air-breathing speed height of tool, characteristic such as gulp capacity is big.
One embodiment of the present of invention: earlier zirconium sponge is made the ZrHx powder by inhaling hydrogen, makes the green compact of specified shape again with 1: 2 by volume mixed moulding of carbon-gas gel powder, put into the vacuum oven dehydrogenation then, the cooling back finished product.
Claims (5)
1. the preparation technology of a getter, the compound getter material that this getter is made up of zirconium and carbon aerogels powder is used for vacuum heat insulation material, vacuum electron device, high purity inert gas preparation or other need remove N
2, O
2, H
2, CO, CO
2, CH
4, H
2The place of O steam and metallic insulator is characterized in that adopting the method for absorption hydrogen that zirconium sponge is made ZrH
x, again with carbon aerogels powder mixing aftershaping, the process preparation of repeatedly inhaling hydrogen-dehydrogenation in a vacuum after a dehydrogenation or a dehydrogenation repeatedly contains the difform getter of activated zr.
2. the preparation technology of getter as claimed in claim 1 is characterized by preparation ZrH
xThe time be that zirconium sponge is vacuumized the back at hydrogen pressure 0.1MPa, flow 0.5-1.0 liter/minute, kept under the 600-1200 ℃ of condition 1-4 hour, after hydrogen pressure remained unchanged, slowly cooling was come out of the stove and is formed ZrH again
x
3. the preparation technology of getter as claimed in claim 2 is characterized by preparation ZrH
xThe time zirconium sponge requirement that vacuumizes for will reach vacuum tightness 10
-2Handkerchief, and kept 0.5 hour.
4. the preparation technology of getter as claimed in claim 1 is characterized by ZrH
xBe meant a ZrH with carbon aerogels powder mixing aftershaping
xIs green compact at the 100-300MPa forming under the pressure with the carbon aerogels powder after screening mixes, and green compact is inserted alloy crucible again and be evacuated to 10 in vacuum oven
-2-10
-4Handkerchief is stablized 0.5-1 hour maintenance vacuum tightness 10
-2-10
-4Reduce to room temperature behind the handkerchief and moulding.
5. as the preparation technology of claim 1 or 4 described getters, it is characterized by and repeat to inhale hydrogen-certain embodiments 2-5 time, the median size of zirconium powder is 200-300nm in the getter, and getter bulk porosity is greater than 50%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410081543 CN1796580B (en) | 2004-12-21 | 2004-12-21 | Technique for preparing new type getter containing zirconium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410081543 CN1796580B (en) | 2004-12-21 | 2004-12-21 | Technique for preparing new type getter containing zirconium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1796580A CN1796580A (en) | 2006-07-05 |
| CN1796580B true CN1796580B (en) | 2010-05-26 |
Family
ID=36817895
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410081543 Expired - Fee Related CN1796580B (en) | 2004-12-21 | 2004-12-21 | Technique for preparing new type getter containing zirconium |
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|---|---|
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103205603B (en) * | 2013-04-23 | 2015-04-08 | 北京科技大学 | Preparation process of crack-free zirconium alloys |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4839085A (en) * | 1987-11-30 | 1989-06-13 | Ergenics, Inc. | Method of manufacturing tough and porous getters by means of hydrogen pulverization and getters produced thereby |
| CN1131596A (en) * | 1995-03-20 | 1996-09-25 | 中国核动力研究设计院 | Preparation technology for production of Zr and Zr-2 alloy powder with hydrogenization method |
-
2004
- 2004-12-21 CN CN 200410081543 patent/CN1796580B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4839085A (en) * | 1987-11-30 | 1989-06-13 | Ergenics, Inc. | Method of manufacturing tough and porous getters by means of hydrogen pulverization and getters produced thereby |
| CN1131596A (en) * | 1995-03-20 | 1996-09-25 | 中国核动力研究设计院 | Preparation technology for production of Zr and Zr-2 alloy powder with hydrogenization method |
Non-Patent Citations (3)
| Title |
|---|
| JP特开2001-50160A 2001.02.23 |
| 景怀宇等.大吸气量新型吸氢材料的研究.稀有金属26 4.2002,26(4),307-309. |
| 景怀宇等.大吸气量新型吸氢材料的研究.稀有金属26 4.2002,26(4),307-309. * |
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|---|---|
| CN1796580A (en) | 2006-07-05 |
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Granted publication date: 20100526 Termination date: 20121221 |