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TiZrMnFe quaternary getter alloy material and preparation method and application thereof

A technology of alloy materials and quaternary alloys, which is applied in the field of intermetallic compound getter materials, can solve the problems of single enhancement of getter performance such as stability, difficulty in determining the change of alloy structure composition, and long time of getter saturation. Achieve the effect of improving the adsorption rate and adsorption capacity, uniform alloy microstructure and high vacuum degree

Inactive Publication Date: 2020-12-04
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] But the ZrMnFe ternary getter also has the following deficiencies: one is that the reaction temperature of ZrMnFe reacts with various impurity gases is relatively high, while the reaction temperature for the adsorption of nitrogen is higher (above 700°C); Under the condition of pressure and pressure, ZrMnFe has a relatively low adsorption rate for nitrogen, and it takes a long time to reach saturation. Research data shows that the adsorption saturation time of ZrMnFe-type getter materials for nitrogen needs nearly 72 hours, and the adsorption efficiency is very low; the third is the cost high and expensive
In the prior art, elements with similar atomic structures to the original elements of the getter material are generally used as replacements, or metal elements that have greater reactivity with the gas to be adsorbed by the getter material are added, but the composition of the alloy structure caused by different doping It is difficult to determine the change of the getter alloy. The phase structure and phase distribution of the getter alloy after doping are affected by many factors such as doping amount, preparation process, heat treatment process, etc. It is difficult to determine the various technical factors used to achieve the best getter performance of the getter material. Determined by theoretical methods, it can only be explored and summarized through a large number of repeated experiments; and the improvement trends of various getter performances brought about by the doping of various elements are not consistent, and the same method will enhance a certain adsorption performance of the getter material. However, it may have a weakening effect on other adsorption properties. Often, the gas-absorbing properties of the getter alloy, such as the total amount of gas adsorption, the adsorption rate, and the stability after adsorption, cannot be enhanced by a single element substitution, and assistance is needed. Other modification methods to obtain getter products with the best getter performance in all aspects

Method used

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  • TiZrMnFe quaternary getter alloy material and preparation method and application thereof
  • TiZrMnFe quaternary getter alloy material and preparation method and application thereof
  • TiZrMnFe quaternary getter alloy material and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Weigh 12.1 g of high-purity titanium, 207.7 g of nuclear-grade pure zirconium, 164.0 g of electrolytic manganese, and 141.3 g of high-purity iron, polish the scale, ultrasonically clean and dry them, and seal them for future use. The sample is placed in a water-cooled copper crucible in a non-consumable vacuum arc melting furnace, ready for melting.

[0042] Pump the vacuum in the melting furnace to 5×10 -3 Pa, stop vacuuming, fill with 99.9% high-purity argon to 0.05MPa, and prepare for arc melting. During the arc melting process, the position of the arc torch is constantly adjusted to ensure uniform melting, and the alloy ingot is turned over 6 times to ensure the melting quality. After the smelting is completed, the sample is cooled and taken out to obtain a TiZrMnFe quaternary alloy ingot.

[0043] Put the alloy ingot into a high-temperature furnace, vacuumize and fill with argon, and anneal at 1000°C for 15h. After the annealing is completed, the alloy ingot is ...

Embodiment 2

[0048] 24.75 grams of high-purity titanium, 188.75 grams of nuclear-grade pure zirconium, 167.1 grams of electrolytic manganese, and 144.4 grams of high-purity iron were weighed, polished to scale, ultrasonically cleaned and dried, and sealed for future use. The sample is placed in a water-cooled copper crucible in a non-consumable vacuum arc melting furnace, ready for melting.

[0049] Pump the vacuum in the melting furnace to 5×10 -3 Pa, stop vacuuming, fill with 99.9% high-purity argon to 0.05MPa, and prepare for arc melting. During the arc melting process, the position of the arc torch is constantly adjusted to ensure uniform melting, and the alloy ingot is turned over 6 times to ensure the melting quality. After smelting, cool for about 1 hour, open the lid and take out the sample.

[0050] After the sample is broken, select the flat side, grind it flat on the pre-grinder at a low speed with alumina sandpaper, put it into the hot mounting machine to heat mount the sampl...

Embodiment 3

[0052] 38.0 grams of high-purity titanium, 168.95 grams of nuclear-grade zirconium, 170.35 grams of electrolytic manganese, and 147.7 grams of high-purity iron were weighed, polished to scale, ultrasonically cleaned and dried, and sealed for future use. The sample is placed in a water-cooled copper crucible in a non-consumable vacuum arc melting furnace, ready for melting.

[0053] Pump the vacuum in the melting furnace to 5×10 -3 Pa, stop vacuuming and fill with 99.9% high-purity argon to 0.05MPa, ready for arc melting. During the arc melting process, the position of the arc torch is constantly adjusted to ensure uniform melting, and the alloy ingot is turned over 6 times to ensure the melting quality. After smelting, cool for about 1 hour, open the lid and take out the sample.

[0054] After the sample was taken out, it was annealed at 1000°C for 18h under the protection of argon. After the annealing is completed, the sample is taken out, put into a vibrating crusher, and...

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Abstract

The invention discloses a TiZrMnFe quaternary getter alloy material and a preparation method and application thereof. The chemical formula of the TiZrMnFe quaternary getter alloy material is TixZr1-xMnFe (x is equal to 0-0.4), and the TiZrMnFe quaternary getter alloy material is specifically composed of, by mass, 2.3 wt%-10.4 wt% of titanium, 29.6 wt% to 41.6 wt% of zirconium; 27.8 wt% to 29.8 wt%of manganese; and 28.0 wt% to 30.3 wt% of iron. The crystal form of the TiZrMnFe quaternary getter alloy material is a C14 type laves crystal structure, and the grain size of the TiZrMnFe quaternarygetter alloy material is 20 microns to 50 microns. The preparation method comprises the steps that Ti, Zr, Mn and Fe pure metal with a certain stoichiometric ratio is weighed, proportioned and smeltedto obtain an alloy ingot, heat treatment is conducted, and the alloy ingot obtained after heat treatment is subjected to crushing, ball milling and sieving to be prepared into TiZrMnFe air suction alloy powder with different particle sizes. The alloy powder is pressed into getter products in various shapes through a cold press, or alloy powder adsorption slurry is brushed on the surface of a device through an adhesive. The preparation process is simple and feasible, the nitrogen adsorption capacity of the getter per unit mass is high and is superior to that of a ternary ZrMnFe alloy, and thepreparation cost is low.

Description

technical field [0001] The invention relates to a TiZrMnFe quaternary getter alloy material and its preparation method and application, belonging to the technical field of intermetallic compound getter materials. Background technique [0002] The getter material is a kind of active gas (H 2 , CO, O 2 、H 2 O.CO 2 etc.), different from the traditional vacuum acquisition technology, the getter material can maintain the active state for a long time during the storage and use of the vacuum device, continuously absorb various physical and chemical products, and maintain the residual gas in the device. The amount is less than the maximum expected gas load, ensuring high reliability and long-term use of vacuum devices. [0003] ZrMnFe ternary getter material has a good purification and removal effect on gases containing hydrogen isotopes, can effectively crack methane, water vapor, ammonia and other gases, and can also absorb gases such as nitrogen, carbon monoxide and carbon di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22C30/00C22C1/02C22F1/02B01J20/02B01J20/28B01J20/30B01D53/02B01D53/54B01D53/81
CPCB01D53/02B01D53/54B01D53/81B01D2257/102B01J20/02B01J20/28004B01J20/28016C22C1/02C22C30/00C22F1/02
Inventor 曾凡浩李磊
Owner CENT SOUTH UNIV
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