CN115786768B - Gas adsorption material with ultralow-temperature vacuum Dewar structure and preparation method thereof - Google Patents
Gas adsorption material with ultralow-temperature vacuum Dewar structure and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 50
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000956 alloy Substances 0.000 claims abstract description 37
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 36
- 229910000990 Ni alloy Inorganic materials 0.000 claims abstract description 28
- IKBUJAGPKSFLPB-UHFFFAOYSA-N nickel yttrium Chemical compound [Ni].[Y] IKBUJAGPKSFLPB-UHFFFAOYSA-N 0.000 claims abstract description 27
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 17
- 239000010936 titanium Substances 0.000 claims abstract description 17
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 16
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000002844 melting Methods 0.000 claims abstract description 8
- 230000008018 melting Effects 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 28
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 27
- 239000002245 particle Substances 0.000 claims description 25
- 230000004913 activation Effects 0.000 claims description 20
- 239000003463 adsorbent Substances 0.000 claims description 20
- 238000003723 Smelting Methods 0.000 claims description 18
- 239000012535 impurity Substances 0.000 claims description 12
- 229910052759 nickel Inorganic materials 0.000 claims description 12
- 229910052727 yttrium Inorganic materials 0.000 claims description 12
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 abstract 3
- 239000002184 metal Substances 0.000 abstract 3
- 150000002739 metals Chemical class 0.000 abstract 3
- 238000002474 experimental method Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 30
- 239000000047 product Substances 0.000 description 17
- 238000012360 testing method Methods 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000005247 gettering Methods 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000004806 packaging method and process Methods 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910011214 Ti—Mo Inorganic materials 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910001325 element alloy Inorganic materials 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical class [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 229910020706 Co—Re Inorganic materials 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000009461 vacuum packaging Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910001868 water Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a gas adsorption material with ultralow temperature Dewar structure and a preparation method thereof, wherein various metals are used for preparing a getter alloy, the main components of the getter alloy are titanium, vanadium and yttrium nickel alloy, the getter alloy is formed after the metals are melted into liquid state through a medium-frequency vacuum melting furnace and are cooled and solidified, the mass ratio of the metals is changed, the getter effect of the getter product and other getter products is compared according to experiments, and according to the experimental results, the getter alloy provided by the invention has the advantages of simple use condition and stable getter amount.
Description
Technical Field
The invention relates to the technical field of gas adsorption materials, in particular to a gas adsorption material with an ultralow-temperature vacuum Dewar structure and a preparation method thereof.
Background
The gas adsorbing material is a generic term for a material capable of efficiently adsorbing a specific gas molecule. The gas adsorbing material can generally reversibly adsorb hydrogen gas and irreversibly adsorb hydrocarbon gas, water, oxygen, nitrogen gas, carbon oxides, and the like. The vacuum-maintaining device is mainly used for vacuum maintenance in vacuum containers or devices, such as heat preservation and insulation, photoelectric vacuum and other related products in the industries, wherein the products are used for maintaining the stability of work and prolonging the service life, and the internal cavity is required to maintain a certain vacuum degree, so that the gas adsorption material products are placed in the internal cavity. After vacuum packaging, the residual gas or external gas inside the vacuum chamber, especially hydrogen, can slowly permeate into the pipe fitting along the grain boundary or defect of the material even through the crystal lattice because of small molecular radius of the hydrogen, and can cause the air pressure in the pipe fitting to rise, so that the heat insulation or electric insulation function of the pipe fitting is disabled. The gas adsorbent in the tube or Du Waga layer is an effective solution to this problem. Particularly in modern physical research, more and more ultralow temperature tests are used for researching the superconducting or magnetic properties of materials, and more effective and reliable vacuum Dewar heat insulation structures are needed to ensure the construction and maintenance of ultralow temperature environments.
The material of the common gas adsorbent is mainly binary or multi-element alloy composed of titanium, zirconium, hafnium, vanadium, aluminum, transition metal and rare earth elements, wherein binary alloy such as Zr-Al, ti-Mo and the like, multi-element alloy such as Zr-V-Fe, zr-Co-Re and the like are commonly used for preparing the gas adsorbent. Such materials are generally highly reactive towards residual reactive gases in vacuum, such as H 2 、0 2 、N 2 CO, hydrocarbon and the like have strong adsorption or absorption capacity. However, these adsorbent products have a small and single activation temperature range, which is in the range of 350-500 ℃ or 650-850 ℃, and thus, a gas adsorbent material having a wide range of activation temperatures and excellent gettering properties is required.
Disclosure of Invention
The invention aims to provide a gas adsorption material with an ultralow-temperature vacuum Dewar structure and a preparation method thereof, and the prepared gas adsorption material can have excellent air suction characteristics on the premise of ensuring a larger activation temperature range.
The gas adsorption material with the ultralow-temperature Dewar structure is characterized by comprising the following components in percentage by mass: 65-70% of titanium, 20-25% of vanadium, 5-15% of yttrium-nickel alloy and 0-0.4% of impurities, wherein the yttrium-nickel alloy comprises 50% ± 5% of yttrium and 50% ± 3% of nickel by mass percent
Preferably, the components and mass percentages thereof are: titanium 65%, vanadium 22%, yttrium-nickel alloy 12.9%, impurity 0.1%, wherein the yttrium-nickel alloy comprises, by mass, yttrium 50% and nickel 50%.
Preferably, the components and mass percentages thereof are: 70% of titanium, 20% of vanadium, 9.9% of yttrium-nickel alloy and 0.1% of impurities, wherein the yttrium-nickel alloy comprises, by mass, 47% of yttrium and 53% of nickel
Preferably, the components and mass percentages thereof are: 69% of titanium, 24% of vanadium, 6.8% of yttrium-nickel alloy and 0.2% of impurities, wherein the yttrium-nickel alloy comprises, by mass, 52% of yttrium and 48% of nickel.
The preparation method of the gas adsorption material with the ultralow-temperature Dewar structure comprises the following steps:
s1, weighing titanium, vanadium and yttrium-nickel alloy serving as materials according to mass percentage;
s2, feeding all materials into a medium-frequency vacuum melting furnace for melting, heating and melting when the air pressure is reduced to a certain degree, and cooling to form a getter alloy after the materials are completely melted into a liquid state;
s3, crushing the cooled getter alloy to a certain size, crushing the getter alloy by a jaw crusher, grinding the getter alloy into powder by a ball mill, and filtering the powder by a screen to ensure that the diameter of the powder is within a certain range;
and S4, pressing the powder to form or preparing slurry to coat the powder on other media to prepare the adsorbent product.
Preferably, the air pressure in the step S2 is reduced to a vacuum air pressure value of less than 4×10 -1 pa。
Preferably, in the step S2, the smelting is performed by heating, and the smelting temperature is 1950-2200 ℃.
Preferably, in the step S3, the getter alloy is crushed into particles having a particle diameter of less than 30 mm.
Preferably, in the step S3, the ball mill grinds the crushed particles into powder having a particle diameter of 20 μm to 75 μm.
Preferably, in step S4, the activation temperature of the adsorbent alloy is in the range of 350 ℃ to 700 ℃.
Therefore, the gas adsorption material with the ultralow-temperature vacuum Dewar structure and the preparation method thereof are adopted, so that the manufactured getter alloy can have a larger activation temperature range and good gettering performance.
The technical scheme of the invention is further described in detail through examples.
Drawings
FIG. 1 is a graph of the inspiration rate versus inspiration amount of a gas adsorbent of the present invention and a comparative gas adsorbent at an activation temperature of 650 ℃;
FIG. 2 is a graph of the inspiration rate versus inspiration amount for a gas adsorbent of the present invention and a comparative gas adsorbent at an activation temperature of 400 ℃.
Detailed Description
The technical scheme of the invention is further described below through examples and drawings.
The invention provides a preparation method of a gas adsorption material with an ultralow-temperature Dewar structure, which comprises the following steps:
s1, weighing the materials according to different schemes: titanium: 65-70%, vanadium: 20-25%; auxiliary additive components: yttrium nickel alloy: 5-15%; other unavoidable impurities: 0-0.4%; the yttrium-nickel alloy comprises the following components in percentage by mass: yttrium: 50% ± 5%, nickel: 50% ± 3%;
s2, feeding all materials into a medium-frequency vacuum melting furnace for melting, wherein when the real air pressure is not more than 4 multiplied by 10 -1 And (3) heating and smelting at 1950-2200 ℃ under Pa, and cooling to form the getter alloy after the material is completely melted into a liquid state.
S3, crushing the cooled air-suction alloy ingot into particles with the diameter of 30mm square, crushing the particles to the size which can be used by a ball mill through a jaw crusher, grinding the alloy particles into powder through the ball mill, filtering the powder through a screen to ensure that the diameter of the powder particles is distributed between 25 micrometers and 75 micrometers, and pressing the powder to form or preparing slurry to be coated on other media to form a product with adsorption capacity.
And S4, pressing the powder to form or preparing slurry to coat the powder on other media to prepare the adsorbent product.
The technical scheme of the invention is further described by the following examples
Example 1
The invention relates to an ultralow-temperature vacuum Dewar structure one embodiment of the gas adsorbing material of (2): the weight percentages of the weighed materials are as follows: titanium: 65%, vanadium: 22%, yttrium nickel alloy: 12.9%, other unavoidable impurities: 0.1%; the yttrium-nickel alloy comprises the following components in percentage by mass: yttrium: 50%, nickel: 50%.
The preparation method comprises the following steps: after the materials are proportioned, smelting in a medium-frequency vacuum smelting furnace, when the true air pressure is not more than 4 multiplied by 10 -1 And (3) heating and smelting at 1950 ℃ at Pa, pouring out and packaging after the materials are completely melted into liquid state after long-time smelting, and cooling to form the air-sucking alloy spindle. The getter alloy is crushed into particles with the square diameter of 30mm, the alloy particles are put into a jaw crusher, the crushed particles with the proper size are put into a ball mill, the ball mill is carried out to obtain powder, the powder is filtered by a screen to ensure that the particle size of the powder is distributed at about 40 microns, the powder is pressed and formed or coated on other media to form a getter product, and the activation temperature of the getter product is 400 ℃ according to the measurement.
Example 2
The invention relates to an ultralow-temperature vacuum Dewar structure one embodiment of the gas adsorbing material of (2): the weight percentages of the weighed materials are as follows: titanium: 70%, vanadium: 20%, yttrium nickel alloy: 9.9%, other unavoidable impurities: 0.1%; the yttrium-nickel alloy comprises the following components in percentage by mass: yttrium: 47%, nickel: 53%.
The preparation method comprises the following steps: after the materials are proportioned, smelting in a medium-frequency vacuum smelting furnace, when the true air pressure is not more than 4 multiplied by 10 -1 And (3) heating and smelting at the temperature of 2100 ℃ at Pa, pouring out and packaging after materials are completely melted into liquid state after long-time smelting, and cooling to form an alloy spindle. The getter alloy is crushed into particles with the square diameter of 30mm, the alloy particles are put into a jaw crusher, the crushed particles with the proper size are put into a ball mill, the ball mill is carried out to obtain powder, the powder is filtered by a screen to ensure that the particle size of the powder is distributed at about 75 microns, the powder is pressed and formed or coated on other media to form a getter product, and the activation temperature of the getter product is 400 ℃ according to the measurement.
Example 3
The invention relates to an ultralow-temperature vacuum Dewar structure one embodiment of the gas adsorbing material of (2): the weight percentages of the weighed materials are as follows: titanium: 69%, vanadium: 24%, yttrium nickel alloy: 6.8%, other unavoidable impurities: 0.2%; the yttrium-nickel alloy comprises the following components in percentage by mass: yttrium: 52%, nickel: 48%.
The preparation method comprises the following steps: after the materials are proportioned, smelting in a medium-frequency vacuum smelting furnace, when the true air pressure is not more than 4 multiplied by 10 -1 And (3) heating and smelting at 2200 ℃ at Pa, pouring out and packaging after the materials are completely melted into liquid state after long-time smelting, and cooling to form the alloy spindle. The getter alloy is crushed into particles with the square diameter of 30mm, the alloy particles are put into a jaw crusher, the crushed particles with the proper size are put into a ball mill, the ball mill is carried out to obtain powder, the powder is filtered by a screen to ensure that the particle size of the powder is distributed at about 60 microns, the powder is pressed and formed or coated on other media to form a getter product, and the activation temperature of the getter product is 650 ℃ according to the measurement.
As shown in figures 1 and 2, the Ti-V-Y-Ni adsorbing material alloy is smelted by the formula and the preparation method to prepare a 150mg adsorbing agent sheet type product, a constant pressure method is adopted to test the air suction characteristic of the adsorbing agent, an air suction performance graph is prepared, two traditional adsorbing materials Ti-Mo and Zr-V-Fe are prepared according to the same conditions, the components of the prepared adsorbing agent sheet are different, the weight and the appearance of the prepared adsorbing agent sheet are the same, the test is carried out on the same test bench, the activation temperature, the activation time, the air suction temperature and the test time are the same, the air suction performance graph corresponding to the air suction performance of the three adsorbing agent sheets is prepared, the trend of the graph is that the air suction rate is gradually reduced, the total air suction amount is gradually increased, the higher the air suction rate is, and the higher the air suction amount indicates that the air suction performance is better.
The limit condition is that the mass of the adsorbent tablets made of the three adsorption material alloys is 150mg, the activation time is 20 minutes in the same test system, the test gas is hydrogen with the purity not lower than 5N, and the constant pressure is 4.0x10 -4 Pa。
In FIG. 1, the three getter activation temperatures are 650 ℃, and the getter rates of the Ti-V-Y-Ni getter alloys, ti-Mo, zr-V-Fe getter alloys are respectively: 1100ml/s,500ml/s and 360ml/s, it can be shown that the gettering performance of the Ti-V-Y-Ni alloy of the present invention is superior to that of the other two conventional alloys under the condition of activation at a low temperature of 650 ℃.
In FIG. 2, again, the comparison curves show that when the activation temperature of the three getters is 400 ℃, the gettering rates of the Ti-V-Y-Ni getter alloy, the Ti-Mo, and the Zr-V-Fe getter alloy are respectively: 980ml/s,450ml/s and 600ml/s, it can be shown that the air suction performance of the TiVYNI alloy of the invention is better than that of the other two traditional alloys under the condition of low-temperature activation at 400 ℃.
The alloy material for absorbing gas in the invention takes titanium as a main element, the element has good air suction characteristic, is widely used in non-evaporable adsorbents, other doped elements and main elements can improve air suction performance after being smelted to form an alloy, and can change the activation temperature of the adsorbent.
The getter in the invention has a wide activation temperature of 350-700 ℃, the adsorbent product can be pressed and block-shaped and spot-welded on the inner wall of the Dewar structure or made into slurry to be directly coated on the inner wall, and the product can be conveniently activated by adopting a baking Du Wabi mode to heat, so that the adsorbent can be more conveniently used compared with the traditional adsorbent product, and has good air suction performance.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting it, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that: the technical scheme of the invention can be modified or replaced by the same, and the modified technical scheme cannot deviate from the spirit and scope of the technical scheme of the invention.
Claims (5)
1. The gas adsorption material with the ultralow-temperature Dewar structure is characterized by comprising the following components in percentage by mass: 65-70% of titanium, 20-25% of vanadium, 5-15% of yttrium-nickel alloy and 0-0.4% of impurities, wherein the yttrium-nickel alloy comprises 50% ± 5% of yttrium and 50% ± 3% of nickel by mass;
the preparation method of the gas adsorption material with the ultralow-temperature Dewar structure comprises the following steps:
s1, weighing titanium, vanadium and yttrium-nickel alloy serving as materials according to mass percentage;
s2, feeding all materials into a medium-frequency vacuum melting furnace for melting, and reducing the air pressure to a vacuum air pressure value smaller than 4 multiplied by 10 - 1 Pa, heating and smelting, and cooling to form a getter alloy after the material is completely melted into a liquid state;
s3, crushing the cooled getter alloy into particles with the particle diameter smaller than 30mm, crushing the particles by a jaw crusher, grinding the particles into powder by a ball mill, and filtering the powder by a screen to ensure that the particle diameter of the powder is 20-75 microns;
s4, pressing the powder to form or preparing slurry to coat on other media to prepare an adsorbent product, wherein the activation temperature of the adsorbent alloy is between 350 ℃ and 700 ℃.
2. The ultra-low temperature dewar structured gas adsorbing material according to claim 1, wherein: the components and mass percentages are as follows: titanium 65%, vanadium 22%, yttrium-nickel alloy 12.9%, impurity 0.1%, wherein the yttrium-nickel alloy comprises, by mass, yttrium 50% and nickel 50%.
3. The ultra-low temperature dewar structured gas adsorbing material according to claim 1, wherein: the components and mass percentages are as follows: 70% of titanium, 20% of vanadium, 9.9% of yttrium-nickel alloy and 0.1% of impurities, wherein the yttrium-nickel alloy comprises, by mass, 47% of yttrium and 53% of nickel.
4. The ultra-low temperature dewar structured gas adsorbing material according to claim 1, wherein: the components and mass percentages are as follows: 69% of titanium, 24% of vanadium, 6.8% of yttrium-nickel alloy and 0.2% of impurities, wherein the yttrium-nickel alloy comprises, by mass, 52% of yttrium and 48% of nickel.
5. The ultra-low temperature dewar structured gas adsorbing material according to claim 1, wherein: and in the step S2, heating and smelting are carried out, wherein the smelting temperature is 1950-2200 ℃.
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| JP2000311588A (en) * | 1999-02-26 | 2000-11-07 | Canon Inc | Getter, airtight container with getter, image forming device and manufacture of getter |
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| CN114749144A (en) * | 2022-04-27 | 2022-07-15 | 中山金石新材料科技有限公司 | Renewable composite getter for maintaining high vacuum environment and manufacturing method thereof |
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2022
- 2022-11-17 CN CN202211440264.XA patent/CN115786768B/en active Active
Patent Citations (7)
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| CN1094378A (en) * | 1993-04-29 | 1994-11-02 | 工程吸气公司 | Removal of gaseous impurities improves one's methods from hydrogen stream |
| JP2000311588A (en) * | 1999-02-26 | 2000-11-07 | Canon Inc | Getter, airtight container with getter, image forming device and manufacture of getter |
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