CN115672254A - Activation-free gas adsorbent used in cryostat and preparation method thereof - Google Patents
Activation-free gas adsorbent used in cryostat and preparation method thereof Download PDFInfo
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- CN115672254A CN115672254A CN202211443048.0A CN202211443048A CN115672254A CN 115672254 A CN115672254 A CN 115672254A CN 202211443048 A CN202211443048 A CN 202211443048A CN 115672254 A CN115672254 A CN 115672254A
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- hafnium
- getter
- zirconium
- activation
- cryostat
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- 239000003463 adsorbent Substances 0.000 title abstract description 33
- 238000002360 preparation method Methods 0.000 title description 4
- INIGCWGJTZDVRY-UHFFFAOYSA-N hafnium zirconium Chemical compound [Zr].[Hf] INIGCWGJTZDVRY-UHFFFAOYSA-N 0.000 claims abstract description 46
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000007789 gas Substances 0.000 claims abstract description 29
- 229910052751 metal Inorganic materials 0.000 claims abstract description 17
- 239000002184 metal Substances 0.000 claims abstract description 17
- 230000007704 transition Effects 0.000 claims abstract description 17
- 239000002594 sorbent Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 238000004806 packaging method and process Methods 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 230000003213 activating effect Effects 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 229910001092 metal group alloy Inorganic materials 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 23
- 238000001179 sorption measurement Methods 0.000 abstract description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 8
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 229910052759 nickel Inorganic materials 0.000 abstract description 5
- 239000001569 carbon dioxide Substances 0.000 abstract description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 4
- 238000009434 installation Methods 0.000 abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- 239000010410 layer Substances 0.000 description 12
- 238000012360 testing method Methods 0.000 description 8
- 229910052786 argon Inorganic materials 0.000 description 6
- 238000000748 compression moulding Methods 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 230000004913 activation Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000009461 vacuum packaging Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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Abstract
The invention discloses an activation-free gas adsorbent used in a cryostat, which comprises a zirconium hafnium getter, a nickel powder transition layer and a metal carrier, wherein the zirconium hafnium getter is positioned at the bottom of the metal carrier, and the nickel powder transition layer is positioned above the zirconium hafnium getter. The activation-free gas adsorbent for the interior of the cryostat adopting the structure can absorb nitrogen, carbon dioxide, organic gas and other gases by the zirconium-hafnium adsorption material, and the nickel transition layer can protect the zirconium-hafnium adsorption material from contacting with a large number of air molecules during preactivation and installation so as to ensure the maximum air absorption performance of the interior adsorption material.
Description
Technical Field
The invention relates to the technical field of vacuum, in particular to an activation-free gas adsorbent used in a cryostat.
Background
The cryostat device is widely used in research departments such as petroleum, chemical engineering, electronic instruments, physics, chemistry, bioengineering, medical and health, life science, light industry food, physical property test and chemical analysis, etc., provides a field source with controlled heat and cold and uniform and constant temperature for users during working, performs constant temperature test or test on test samples or produced products, and can also be used as a heat source or cold source for direct heating or refrigeration and auxiliary heating or refrigeration. The ambient environment of the cryostat is higher than the temperature inside the cryostat, so that the external heat is always transferred to the cryostat by convection, conduction and radiation, one of the first problems of the cryostat is the heat transfer problem, so that the external heat input is reduced as much as possible at the beginning of the design, and other methods are also sought to counteract the input heat, such as dewar insulation, vacuum, silver plating, etc. Therefore, the effectiveness of a thermostat is often dependent on the following stray warm flows:
(1) When the vacuum degree is not good enough, the heat convection is conducted through the low-pressure gas;
(2) Radiant heat;
(3) Heat conduction along a pipe or electrical conductor;
(4) Joule or eddy current heat generation.
The most feared of a cryostat is a temperature rise, wherein the main temperature-influencing factor is thermal convection, through which external heat is transferred into the interior of the cryostat in the presence of air. The vacuum pumping is to pump air away, so that heat can not be transferred into the air. The currently adopted form is 'vacuum pump unit' + 'active carbon adsorbent', and because the active carbon adsorbent has poor gas suction capacity, the vacuum pump unit needs to be kept in a gas suction state all the time during the use of the cryostat, so that the whole system can be subjected to large energy consumption and mechanical vibration, and the influence on some working conditions with special environmental requirements cannot be used.
As a low-temperature activated adsorbent product, the zirconium hafnium adsorption material has the characteristics of low-temperature activation and room-temperature air suction, and is relatively stable in chemical property, safe and environment-friendly to use. The zirconium hafnium adsorbent can be subjected to pre-activation treatment at a lower temperature in a vacuum furnace, so that the condition that a higher temperature condition is required to be provided for activation in a later use process is avoided.
Metallic nickel has been widely used industrially as a catalyst. The porous membrane mainly has unique performances of adsorption, sieving, ion exchange, catalysis and the like due to the fact that a plurality of pore channels with uniform pore diameters and cavities on the inner surface are formed inside the porous membrane. In addition, nickel has selective filtering property to gas after being oxidized at normal temperature, and can be used as a transition layer to isolate excessive oxidation or pollution of a large amount of active substances such as oxygen, nitrogen, carbon dioxide, carbon monoxide and the like in the air to the internal zirconium-hafnium gas adsorption material layer.
Disclosure of Invention
The invention aims to provide an activation-free gas adsorbent for the interior of a cryostat, which is produced in vacuum by adding a domestic mature metal nickel catalyst on the basis of using a zirconium-hafnium low-temperature adsorption material, and can protect the zirconium-hafnium adsorption material from contacting with a large amount of air molecules due to the blocking of a nickel transition layer when the adsorbent is exposed to the air for a short time after being unsealed (within 40 minutes, which is the longest time required for unsealing the adsorbent and placing the adsorbent in the cryostat during normal production).
In order to achieve the above object, the present invention provides an activation-free gas adsorbent for use inside a cryostat, comprising a zirconium hafnium getter, a nickel powder transition layer and a metal carrier, wherein the zirconium hafnium getter is located at the bottom of the metal carrier, and the nickel powder transition layer is located above the zirconium hafnium getter.
Preferably, the adsorbing material of the zirconium hafnium getter is a binary metal alloy with the composition of 70wt% of Zr and 30wt% of Hf.
Preferably, the particle size of the nickel powder transition layer is between 40 and 80 microns.
A preparation method of an activation-free gas adsorbent used in a cryostat comprises the following specific steps:
step S1: pretreating the zirconium-hafnium getter in a vacuum furnace at high temperature, taking out the zirconium-hafnium getter, pressing the zirconium-hafnium getter in a vacuum operation box body to form at the bottom of a metal carrier, covering nickel powder on the upper part of the zirconium-hafnium getter, and then pressing and forming again;
step S2: and after the integral manufacture of the zirconium-hafnium getter is finished, baking and activating at low temperature in a vacuum environment, and storing or packaging the formed and activated product in the vacuum environment or in inert gas.
Preferably, in the step S2, the zirconium-hafnium getter is loaded into a vacuum furnace and vacuumized to 10 degrees -3 Pa is heated to 250 ℃ and the temperature is kept for 10 minutes.
Therefore, the invention adopts the above-mentioned structure of the activation-free gas adsorbent for the interior of the cryostat, the zirconium hafnium adsorption material can absorb nitrogen, carbon dioxide, organic gas and other gases, and the nickel transition layer can protect the zirconium hafnium adsorption material from contacting with a large amount of air molecules during preactivation and installation so as to ensure the maximum air absorption performance of the interior adsorption material.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is a schematic diagram of an embodiment of an activated-free gas sorbent for use in a cryostat interior according to the present invention;
reference numerals
1. A zirconium hafnium getter; 2. a nickel powder transition layer; 3. a metal support.
Detailed Description
The technical solution of the present invention is further illustrated by the accompanying drawings and examples.
The invention provides an activation-free gas adsorbent for the interior of a cryostat, which comprises a zirconium-hafnium getter, a nickel powder transition layer and a metal carrier, wherein the adsorbing material of the zirconium-hafnium getter is a binary metal alloy consisting of 70wt% of Zr and 30wt% of Hf, the powder particle size of the nickel powder transition layer is 40-80 micrometers, the zirconium-hafnium getter is positioned at the bottom of the metal carrier, and the nickel powder transition layer is positioned above the zirconium-hafnium getter.
A preparation method of an activation-free gas adsorbent used in a cryostat is characterized by comprising the following specific steps:
step S1: pretreating the zirconium-hafnium getter in a vacuum furnace at high temperature, taking out the zirconium-hafnium getter, pressing the zirconium-hafnium getter in a vacuum operation box body to form at the bottom of a metal carrier, covering nickel powder on the upper part of the zirconium-hafnium getter, and then pressing and forming again;
step S2: and after the integral manufacture of the zirconium hafnium getter is finished, baking and activating at low temperature in a vacuum environment, and storing or packaging the formed and activated product in the vacuum environment or in inert gas.
Step S2, loading the zirconium-hafnium getter into a vacuum furnace, and vacuumizing to 10 DEG -3 Pa is heated to 250 ℃ and the temperature is kept for 10 minutes.
The specific implementation method comprises the following steps:
example 1
As shown in figure 1, the getter material for preparing zirconium hafnium adsorbent is formed by compression molding at the bottom of metal carrier in vacuum argon-filled glove box, then nickel powder is filled above the getter material for compression molding again, and then the getter material is loaded into a vacuum heating furnace and vacuumized to 10 DEG -3 After Pa, the mixture was heated to 250 ℃ and kept at that temperature for 10 minutes. And (5) cooling to room temperature, filling argon, discharging from the furnace, cooling, taking out, and carrying out vacuum packaging on the adsorbent in a plastic packaging machine in a glove box.
The process is carried out by taking a piece of packed adsorbent, unsealing and then placing in the air for 40 minutes, which is the time for simulating the production process of placing in a cryostat, and the longest time for unsealing the adsorbent until it is placed in the interlayer space. The adsorbent was then placed in a test bed and tested for hydrogen absorption capacity of 194PaL/mg.
Example 2
As shown in figure 1, the getter material for preparing zirconium hafnium adsorbent is formed by compression molding at the bottom of metal carrier in vacuum argon-filled glove box, then nickel powder is filled above the getter material for compression molding again, and then the getter material is loaded into a vacuum heating furnace and vacuumized to 10 DEG -3 After Pa, the mixture was heated to 250 ℃ and kept at that temperature for 10 minutes. And (5) cooling to room temperature, filling argon, discharging from the furnace, cooling, taking out, and carrying out vacuum packaging on the adsorbent in a plastic packaging machine in a glove box.
And (3) taking an adsorbent just taken out of the furnace, putting the adsorbent into a test bench for activation, and testing the hydrogen absorption capacity to be 206PaL/mg.
Example 3
As shown in figure 1, the getter material for preparing zirconium hafnium adsorbent is formed by compression molding at the bottom of metal carrier in vacuum argon-filled glove box, then nickel powder is filled above the getter material for compression molding again, and then the getter material is loaded into a vacuum heating furnace and vacuumized to 10 DEG -3 After Pa, the mixture was heated to 250 ℃ and kept at that temperature for 10 minutes. And (5) cooling to room temperature, filling argon, discharging from the furnace, cooling, taking out, and carrying out vacuum packaging on the adsorbent in a plastic packaging machine in a glove box.
The production process of placing the adsorbent in a cryostat was simulated by taking one well-encapsulated adsorbent, unsealing it and placing it in the air for 20 minutes, and the time taken to unseal the getter and place it in the interlayer space. The adsorbent was then placed in a test bed and tested for hydrogen absorption capacity of 191PaL/mg.
Therefore, the activation-free gas adsorbent for the interior of the cryostat adopting the structure can absorb gases such as nitrogen, carbon dioxide, organic gas and the like, and the nickel transition layer can protect the zirconium hafnium adsorption material from contacting with a large amount of air molecules during preactivation and installation so as to ensure the maximum air absorption performance of the interior adsorption material.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the invention without departing from the spirit and scope of the invention.
Claims (5)
1. An activation-free gas sorbent for use inside a cryostat, the activation-free gas sorbent comprising: the metal carrier comprises a zirconium hafnium getter, a nickel powder transition layer and a metal carrier, wherein the zirconium hafnium getter is positioned at the bottom of the metal carrier, and the nickel powder transition layer is positioned above the zirconium hafnium getter.
2. An activation-free gas sorbent for the interior of a cryostat according to claim 1, wherein: the component of the Zr-Hf getter is a binary metal alloy consisting of 70wt% of Zr and 30wt% of Hf.
3. An activation-free gas sorbent for use in the interior of a cryostat according to claim 1, wherein: the powder particle size of the nickel powder transition layer is between 40 and 80 microns.
4. A method of preparing the non-activated gas sorbent for the interior of a cryostat according to any of claims 1 to 3, comprising the specific steps of:
step S1: pretreating the zirconium-hafnium getter in a vacuum furnace at high temperature, taking out the zirconium-hafnium getter, pressing the zirconium-hafnium getter in a vacuum operation box body to form at the bottom of a metal carrier, covering nickel powder on the upper part of the zirconium-hafnium getter, and then pressing and forming again;
step S2: and after the integral manufacture of the zirconium hafnium getter is finished, baking and activating at low temperature in a vacuum environment, and storing or packaging the formed and activated product in the vacuum environment or in inert gas.
5. The method of claim 4, wherein the step of forming the non-activated gas sorbent comprises: in the step S2, the zirconium-hafnium getter is put into a vacuum furnace and is vacuumized to 10 DEG -3 Pa is heated to 250 ℃ and the temperature is kept for 10 minutes.
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| CN202211443048.0A CN115672254A (en) | 2022-11-17 | 2022-11-17 | Activation-free gas adsorbent used in cryostat and preparation method thereof |
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