CN114749144A - Renewable composite getter for maintaining high vacuum environment and manufacturing method thereof - Google Patents
Renewable composite getter for maintaining high vacuum environment and manufacturing method thereof Download PDFInfo
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- CN114749144A CN114749144A CN202210453716.1A CN202210453716A CN114749144A CN 114749144 A CN114749144 A CN 114749144A CN 202210453716 A CN202210453716 A CN 202210453716A CN 114749144 A CN114749144 A CN 114749144A
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- 239000002131 composite material Substances 0.000 title claims abstract description 58
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 98
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 30
- 239000000956 alloy Substances 0.000 claims abstract description 30
- 239000002808 molecular sieve Substances 0.000 claims abstract description 19
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 9
- 238000003825 pressing Methods 0.000 claims abstract description 8
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims description 66
- 238000001179 sorption measurement Methods 0.000 claims description 37
- 229910044991 metal oxide Inorganic materials 0.000 claims description 23
- 150000004706 metal oxides Chemical class 0.000 claims description 23
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 238000005485 electric heating Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052802 copper Inorganic materials 0.000 claims description 7
- 239000010949 copper Substances 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 229910052763 palladium Inorganic materials 0.000 claims description 7
- 229910000640 Fe alloy Inorganic materials 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- ZGTNJINJRMRGNV-UHFFFAOYSA-N [V].[Fe].[Zr] Chemical compound [V].[Fe].[Zr] ZGTNJINJRMRGNV-UHFFFAOYSA-N 0.000 claims description 6
- 229910052735 hafnium Inorganic materials 0.000 claims description 6
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 239000011575 calcium Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- 239000011701 zinc Substances 0.000 claims description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- 229910052747 lanthanoid Inorganic materials 0.000 claims description 3
- 150000002602 lanthanoids Chemical class 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052758 niobium Inorganic materials 0.000 claims description 3
- 239000010955 niobium Substances 0.000 claims description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052702 rhenium Inorganic materials 0.000 claims description 3
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 claims description 3
- 239000000741 silica gel Substances 0.000 claims description 3
- 229910002027 silica gel Inorganic materials 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- 238000003466 welding Methods 0.000 claims description 3
- 229910052727 yttrium Inorganic materials 0.000 claims description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 238000000748 compression moulding Methods 0.000 claims description 2
- 238000007711 solidification Methods 0.000 claims 2
- 230000008023 solidification Effects 0.000 claims 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 6
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000003463 adsorbent Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000008929 regeneration Effects 0.000 description 5
- 238000011069 regeneration method Methods 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 238000012423 maintenance Methods 0.000 description 3
- 229910000986 non-evaporable getter Inorganic materials 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910000314 transition metal oxide Inorganic materials 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 229910001069 Ti alloy Inorganic materials 0.000 description 2
- 239000011358 absorbing material Substances 0.000 description 2
- 238000001994 activation Methods 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 229910000733 Li alloy Inorganic materials 0.000 description 1
- 229910001093 Zr alloy Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- YSZKOFNTXPLTCU-UHFFFAOYSA-N barium lithium Chemical compound [Li].[Ba] YSZKOFNTXPLTCU-UHFFFAOYSA-N 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000001989 lithium alloy Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- PMTRSEDNJGMXLN-UHFFFAOYSA-N titanium zirconium Chemical compound [Ti].[Zr] PMTRSEDNJGMXLN-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3408—Regenerating or reactivating of aluminosilicate molecular sieves
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3483—Regenerating or reactivating by thermal treatment not covered by groups B01J20/3441 - B01J20/3475, e.g. by heating or cooling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/006—Processes utilising sub-atmospheric pressure; Apparatus therefor
Abstract
The invention discloses a renewable composite getter for maintaining a high vacuum environment and a manufacturing method thereof. The method for preparing the getter comprises adding sintered spherical 5A molecular sieve into powdery non-evaporable alloy getter, press-forming to obtain thin cylindrical gas adsorbing material,3g of ferric oxide powder and 20 to 35 mass percent of NH4HCO3Mixing the powders, stirring completely with anhydrous ethanol as solvent, adding spherical 5A molecular sieve with diameter of 2mm, and pressing to obtain gas-cured material. The invention compounds a plurality of getter materials with different functions together to obtain excellent comprehensive getter performance.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to a renewable composite getter for maintaining a high-vacuum environment and a manufacturing method thereof.
[ background of the invention ]
At present, zirconium alloy getters, titanium alloy getters, barium-lithium alloy getters, zirconium-titanium alloy getters and the like are widely applied to devices such as special lamps, traveling wave tubes, electronic picture tubes, vacuum contactors, micro-electromechanical systems (MEMS), solar heat collecting tubes, vacuum heat insulation containers, vacuum heat insulation plates and the like, and the alloy getters can adsorb various gases escaping from a vacuum closed cavity to enable the vacuum cavity to be maintained at a high vacuum degree level for a long time, so that the alloy getters play a role in guaranteeing functions of the devices which rely on vacuum environment to obtain good working performance.
However, these getters suffer from several common disadvantages: for example, (1) for the main gas H in high vacuum environment2The amount of adsorption of (a) is insufficient, particularly for devices with limited use space and difficulty in increasing the amount of gas adsorption by increasing the loading amount of the getter, and is particularly significant; (2) the getter has poor water vapor adsorption effect, and the getter has remarkably deteriorated air suction performance after trace water vapor is adhered to the surface of the getter; (3) is not suitable for adsorbing long molecular chain gas; (4) the manufacturing cost of the material is high.
In the prior art, for example, the composite getter described in patent CN 202942886U, CN 202921323U adopts a desiccant-coated non-evaporable getter and adopts a method of packaging after early high-temperature activation, which is only suitable for low-vacuum application of vacuum insulation panels, does not have the capability of maintaining a high-vacuum environment, and cannot realize getter regeneration. The combined getter disclosed in patent CN 105570618B is only suitable for adsorbing hydrogen and carbon monoxide gases that can chemically react with the oxide, but has no adsorption capability for gases such as nitrogen and carbon dioxide, and uses expensive metal elements such as Co and Ag, and for high vacuum environment, the gas molecules are very thin and normal temperature conditions, and these chemical reactions are not determined to be normally performed, and are only suitable for maintaining use in medium and low vacuum environment, and it also has no reproducible function. The composite getter material mentioned in US 8961817B 2 comprises getter material, cerium oxide, copper oxide and metallic palladium for removing hydrogen and carbon monoxide, and emphasizes the composite form of adding getter to transition metal oxide and drier material in powder state to effectively maintain vacuum environment, this technology is only suitable for activating once, using once getter product, without regeneration function, and it is difficult to guarantee gas absorption performance of these oxides under high vacuum.
The above information disclosed in this background section is only for enhancement of understanding of the background of the invention and therefore it may contain information that does not constitute prior art that is already known to a person of ordinary skill in the art.
[ summary of the invention ]
The invention aims to overcome the defects of the prior art and provides a composite getter for vacuum maintenance and a manufacturing method thereof, which can greatly improve the H ratio2And other specific gas adsorption amount, and the getter can exhaust the adsorbed gas for regeneration, and the manufacture is simple and convenient.
The invention is realized by the following technical scheme:
a renewable, composite getter for maintaining a high vacuum environment, characterized by: the gas-absorbing material comprises a non-evaporable alloy getter and a gas-solidified material, wherein the gas-solidified material is a composition of a metal oxide material and a porous absorbing material.
Renewable composite getter for maintaining a high vacuum environment as described above, characterized in that: the renewable composite getter has an electrical heating component.
Renewable composite getter for maintaining a high vacuum environment as described above, characterized in that: the alloy composition of the non-evaporable alloy getter material consists of one or more of titanium, zirconium, vanadium, iron, molybdenum, nickel, hafnium, niobium, yttrium, rhenium, lanthanides, aluminum, copper, palladium, hafnium and cobalt.
Renewable composite getter for maintaining a high vacuum environment as described above, characterized in that: the non-evaporable alloy getter material is a zirconium vanadium iron alloy getter.
Renewable composite getter for maintaining a high vacuum environment as described above, characterized in that: the porous adsorption material comprises one or more of activated carbon, molecular sieve, activated alumina and silica gel.
Renewable composite getter for maintaining a high vacuum environment as described above, characterized in that: the metal oxide material can chemically react with hydrogen gas at a temperature below 520 ℃ to form non-gaseous species.
Renewable composite getter for maintaining a high vacuum environment as described above, characterized in that: the metal oxide material is an oxide containing iron, copper, zinc, palladium, potassium, calcium, aluminum, or a combination thereof.
Renewable composite getter for maintaining a high vacuum environment as described above, characterized in that: the composition ratio of the metal oxide material to the porous adsorption material is 5-90 wt.% of porous metal oxide, and the composition ratio of the porous adsorption material is 5-90 wt.%, wherein wt.% represents mass ratio.
Renewable composite getter for maintaining a high vacuum environment as described above, characterized in that: the proportion of the non-evaporable alloy getter to the porous adsorption material is as follows: the mass of the non-evaporable alloy getter accounts for 10-99%, and the mass of the porous adsorbing material accounts for 5-60%.
A method of making a renewable, composite getter as described above for maintaining a high vacuum environment, characterized in that:
A. preparation of the gas adsorption material: adding a sintered and molded spherical 5A molecular sieve into a powdery non-evaporable alloy getter, and performing compression molding to obtain a thin cylindrical gas adsorption material, wherein the volume of the spherical 5A molecular sieve accounts for 5-60% of the mass of the thin cylindrical gas adsorption material, and the non-evaporable alloy getter is a zirconium-vanadium-iron alloy getter;
B. preparing a gas curing material: 3g of ferric oxide powder and 20 to 35 mass percent of NH4HCO3Mixing the powders, stirring with anhydrous ethanol, and addingPressing one spherical 5A molecular sieve with the diameter of 2mm, wherein the pressing pressure is less than 100MPa, and obtaining an oxide composite getter thin cylindrical gas curing material green compact with the diameter of 6mm and the height of 2 mm;
C. baking the gas-cured material green body in a vacuum drying oven at 80 ℃ for 4h to obtain NH4HCO3And decomposing to completely remove the gas-adsorbing material to obtain a final gas-curing material piece, and fixedly connecting the gas-adsorbing material and the gas-curing material on two sides of the electric heating part respectively in a metal spot welding manner to form the renewable composite getter for maintaining a high-vacuum environment.
Compared with the prior art, the invention has the following advantages:
1. on the premise of meeting the getter activation process conditions, the getter composite material compounds a plurality of getter materials with different functions to obtain excellent comprehensive getter performance.
2. The invention introduces a gas solidified material, generally a metal oxide, which can not react with the gas in the cavity under the condition of lower air pressure and no heating, when the air suction amount of the gas adsorption material reaches or approaches to saturation and the air suction performance is reduced, the composite getter is heated, so that the gas atoms adsorbed by the gas adsorption material are quickly desorbed from the composite getter and are bonded to gas molecules again on the surface of the composite getter and released to a vacuum space, the gas concentration in the closed cavity is increased by discharging a large amount of gas, at the moment, the gas solidified material chemically reacts with the gas with high concentration at higher temperature, the gas released by the gas adsorption material is transferred and solidified in a reaction product of the gas solidified material through chemical reaction, water in the reaction product is absorbed by the porous adsorption material, and the gas adsorption material in the composite getter obtains the capacity of continuously adsorbing gas again, the regeneration of the composite getter is completed, and the purposes of continuing the working capacity of the getter and prolonging the service life of the device are achieved.
[ description of the drawings ]
Fig. 1 is a schematic structural view of the present invention.
Fig. 2 is a plan view of the gas adsorbent material a in the composite getter of the present invention.
Fig. 3 is a sectional view of the gas adsorbent a in the composite getter according to the present invention.
Fig. 4 is a plan view of the gas-solidified material b in the composite getter of the present invention.
Fig. 5 is a sectional view of the gas solidified material b in the composite getter of the present invention.
In the figure: 1 is a spherical 5A molecular sieve; 2 is a non-evaporable alloy getter; 3 is a metal oxide blank; and 4, an electric heating part.
[ detailed description ] embodiments
The technical features of the present invention will be described in further detail with reference to the accompanying drawings so that those skilled in the art can understand the technical features.
The technical basis of the invention is based on the following two facts:
(1) the non-evaporable getter can adsorb a large amount of H dissipated in a high-vacuum environment after being activated at high temperature2、CO、CO2、N2When the gas is used, the main gas hydrogen has reversible adsorption characteristic, and H atoms adsorbed by the gas can be desorbed again at higher temperature and can be recombined into hydrogen which returns to the vacuum space.
(2) Some metal oxides have strong oxidizability and can be fully reacted with H under the condition of heating2Oxidation-reduction reaction is carried out to generate non-gaseous substances, thereby absorbing and solidifying H2Preventing it from returning to the vacuum space again, thereby maintaining the function of a high vacuum environment.
(3) Inorganic non-metal adsorbing materials with relatively low price, such as molecular sieves, activated carbon and the like, have strong adsorption capacity on water vapor (gas), inert gas and long molecular chain gas.
In the prior art, the getters with the characteristics are often used independently, the synergistic effect among the getters cannot be well utilized, the using effect is not good, and the using field of the getter products is limited.
The invention therefore claims a renewable composite getter for maintaining a high vacuum environment, the body comprising a gas-adsorbing material, a gas-solidifying material and an electric heating means, said gas-adsorbing material being a non-evaporable getter 2, and preferably further a composite porous adsorbing material. The gas-solidified material includes a metal oxide material and a porous adsorbent material.
The alloy composition of the non-evaporable alloy getter 2 is composed of one or more of titanium, zirconium, vanadium, iron, molybdenum, nickel, hafnium, niobium, yttrium, rhenium, lanthanides, aluminum, copper, palladium, hafnium and cobalt, for example the non-evaporable alloy getter material may be a zirconium vanadium iron alloy getter.
The porous adsorption material is an inorganic nonmetal substance and comprises one or more of activated carbon, a molecular sieve, activated alumina and silica gel, and the molecular sieve is preferably a spherical 5A molecular sieve 1.
The metal oxide material can chemically react with hydrogen released by the getter in the vacuum cavity under a certain temperature condition (such as the temperature below 520 ℃), so as to generate a stable non-gaseous product, wherein the reaction product often contains water, and the water is absorbed by the porous adsorption material.
The metal oxide material is an oxide containing iron, copper, zinc, palladium, potassium, calcium, aluminum, or a combination thereof.
The composition ratio of the metal oxide to the porous adsorption material is 5-90 wt.% of the metal oxide, and the composition ratio of the porous adsorption material is 5-90 wt.%, wherein wt.% represents the mass ratio.
The proportion of the non-evaporable alloy getter to the porous adsorption material is as follows: the mass of the non-evaporable alloy getter accounts for 10-99%, and the mass of the porous adsorbing material accounts for 5-60%.
The renewable composite getter for maintaining high vacuum degree of the invention adopts different getter materials to realize the integral high-efficiency gas adsorption capacity according to different gas characteristics of the use environment, and combines a method that certain materials can generate chemical reaction with specific gas so as to irreversibly store the gas, thereby obtaining higher gas adsorption capacity and longer-term vacuum degree of the maintenance cavity, realizing the online regeneration of the getter and greatly prolonging the service life of devices.
The invention also claims a method for manufacturing the renewable composite getter for high vacuum maintenance, in particular a manufacturing method of one embodiment of the composite getter.
A. Preparation of gas adsorbent a: adding a sintered and molded spherical 5A molecular sieve 1 into a powdery non-evaporable alloy getter 2, and performing press molding to obtain a thin cylindrical composite gas adsorbing material, wherein the volume of the spherical 5A molecular sieve 1 accounts for 5-60% of the thin cylindrical composite gas adsorbing material, and the non-evaporable alloy getter 2 is a zirconium-vanadium-iron alloy getter.
B. Preparation of gas-curing Material b: 3g of ferric oxide powder and 20 to 35 mass percent of NH4HCO3Mixing the powders, fully stirring the mixture by taking absolute ethyl alcohol as a solvent, adding 1 spherical 5A molecular sieve with the diameter of 2mm, and pressing the mixture to prepare a metal oxide blank 3, wherein the pressing pressure is less than 100MPa, and the metal oxide blank 3 is an oxide composite getter thin cylindrical green blank with the diameter of 6mm and the height of 2mm and is a transition metal oxide.
C. Placing the oxide composite getter thin cylindrical gas curing material green body in a vacuum drying oven, and baking for 4 hours at 80 ℃ to enable NH4HCO3Decomposing to completely remove to obtain porous gas solidified material, and fixedly connecting the gas adsorption material a and the gas solidified material b on two sides of an electric heating part 4 respectively to form a renewable composite getter for maintaining vacuum degree, wherein the electric heating part 4 is a resistance heating plate on the outer surface of ceramic. As shown in fig. 1, the gas adsorbent a is disposed on the left side of the electric heating element 4; on the right is gas-cured material b.
The transition metal oxide refers to a metal oxide which can chemically react with the interlayer gas under certain conditions to generate a non-gaseous substance and has low saturated vapor pressure and high vacuum stability, such as oxides of iron, copper, zinc, palladium, potassium, calcium, aluminum, or a combination of the oxides.
The working process of the composite getter of the invention is as follows:
the getter is activated by introducing current through the vacuum electric plug to heat the electric heating part 4, and the temperature is 500 ℃ and is maintained for 10 min. When the gas suction capacity of the composite getter is weakened, the current of the heating electric heating part 4 is switched on again to heat the composite getter, at the moment, the hydrogen absorbed in the non-evaporable alloy getter 2 can be desorbed from the getter and released again, and meanwhile, the metal oxide pressing piece 3 and the hydrogen generate chemical reaction for reducing iron oxide under the heating condition, so that a large amount of H is consumed2And the water produced in the reaction is absorbed by the 5A molecular sieve 1. Until the non-evaporable alloy getter 2 finishes the 'emptying' of the adsorbed gas, the fresh metal surface is exposed again, and the heating is stopped. At this time, the non-evaporable alloy getter 2 is activated again to be "empty" and begin to absorb various gases, and the metal oxide blank pressing member 3 synchronously completes a hydrogen curing action, and the above processes can be performed for multiple times as required.
The examples described herein are merely illustrative of preferred embodiments of the invention, for example, the composite of materials may also be present in a laminated, or clad, form, and the gas adsorbing material and gas solidified material may be combined with the electrical heating element by cold pressing, welding, high temperature glue bonding, or by other means of fastening. The above embodiments do not limit the concept and scope of the present invention, and various modifications and improvements made to the technical solutions of the present invention by those skilled in the art without departing from the design concept of the present invention should fall within the protection scope of the present invention.
Claims (10)
1. A renewable, composite getter for maintaining a high vacuum environment, characterized by: the getter comprises a gas adsorption material and a gas solidification material, wherein the gas adsorption material comprises a non-evaporable alloy getter, and the gas solidification material is a composition of a metal oxide material and a porous adsorption material.
2. Renewable composite getter for maintaining a high vacuum environment according to claim 1, characterized in that: the renewable composite getter has an electrical heating component.
3. Renewable composite getter for maintaining a high vacuum environment according to claim 1, characterized in that: the alloy composition of the non-evaporable alloy getter material consists of one or more of titanium, zirconium, vanadium, iron, molybdenum, nickel, hafnium, niobium, yttrium, rhenium, lanthanides, aluminum, copper, palladium, hafnium and cobalt.
4. Renewable composite getter according to claim 3, characterized in that: the non-evaporable alloy getter material is a zirconium vanadium iron alloy getter.
5. Renewable composite getter for maintaining a high vacuum environment according to claim 1, characterized in that: the porous adsorption material comprises one or more of activated carbon, molecular sieve, activated alumina and silica gel.
6. Renewable composite getter according to claim 1, characterized in that: the metal oxide material can chemically react with hydrogen gas at a temperature below 520 ℃ to form non-gaseous species.
7. Renewable composite getter according to claim 6, characterized in that: the metal oxide material is an oxide containing iron, copper, zinc, palladium, potassium, calcium, aluminum, or a combination thereof.
8. Renewable composite getter according to claim 7, characterized in that: the composition ratio of the metal oxide material to the porous adsorption material is 5-90 wt.% of porous metal oxide, and the composition ratio of the porous adsorption material is 5-90 wt.%, wherein wt.% represents mass ratio.
9. Renewable composite getter according to claim 1, characterized in that: the non-evaporable alloy getter and the porous adsorption material have the following ratio: the mass of the non-evaporable alloy getter accounts for 10-99%, and the mass of the porous adsorbing material accounts for 5-60%.
10. A method of making a renewable composite getter according to any of claims 1 to 9 for maintaining a high vacuum environment, characterized in that:
A. preparation of the gas adsorption material: adding a sintered and molded spherical 5A molecular sieve into a powdery non-evaporable alloy getter, and performing compression molding to obtain a thin cylindrical gas adsorption material, wherein the volume of the spherical 5A molecular sieve accounts for 5-60% of the mass of the thin cylindrical gas adsorption material, and the non-evaporable alloy getter is a zirconium-vanadium-iron alloy getter;
B. preparing a gas curing material: 3g of ferric oxide powder and 20 to 35 mass percent of NH4HCO3Mixing the powders, fully stirring the mixture by taking absolute ethyl alcohol as a solvent, adding a spherical 5A molecular sieve with the diameter of 2mm, and pressing the mixture under the pressure of less than 100MPa to obtain an oxide composite getter thin cylindrical gas curing material green compact with the diameter of 6mm and the height of 2 mm;
C. baking the gas-cured material green body in a vacuum drying oven at 80 ℃ for 4h to obtain NH4HCO3And decomposing to completely remove the gas-adsorbing material to obtain a final gas-curing material piece, and fixedly connecting the gas-adsorbing material and the gas-curing material on two sides of the electric heating part respectively in a metal spot welding manner to form the renewable composite getter for maintaining a high-vacuum environment.
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