CN101766983B - Non-evaporable fiber silk type getter and preparation method thereof - Google Patents
Non-evaporable fiber silk type getter and preparation method thereof Download PDFInfo
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- CN101766983B CN101766983B CN2010100137364A CN201010013736A CN101766983B CN 101766983 B CN101766983 B CN 101766983B CN 2010100137364 A CN2010100137364 A CN 2010100137364A CN 201010013736 A CN201010013736 A CN 201010013736A CN 101766983 B CN101766983 B CN 101766983B
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Abstract
The invention discloses a non-evaporable fiber silk type getter, which comprises the following components by weight percent: 80%-92% of Ti, 5%-12% of Ni and 3%-8% of V, and the sum of the weight percents of the components is 100%, wherein the Ti is high-purity sponge titanium with the purity of 99.1%-99.7%, impurity elements of Al and O in the getter respectively account for below 80ppm of the total weight of the getter by weight, and the impurity elements of C, Fe, Si and N respectively account for below 20ppm of the total weight of the getter by weight. The invention further discloses a preparation method of the getter, which comprises the following steps: carrying out smelting thrice on three types of metal, then forging, obtaining a finished alloy ingot, further carrying out working procedure of refining fiber silk, obtaining a pre-formed black, and finally adopting vacuum sintering for preparing the getter. The getter can solve the powder shedding problem of the non-evaporable getter during the using process and has high gettering rate of H2 and sufficient gettering capacity.
Description
Technical field
The present invention relates to powder metallurgical technology, relate to a kind of non-evaporable fiber silk type getter that is used for fields such as atomic clock, proton precessional magnetometer, heat insulation vessel and cathode-ray tube, the invention still further relates to the preparation method of this getter.
Background technology
Getter is meant the effectively common name of material, reagent or the device of some gas molecule of sorption.It mainly acts on is to store and duration of work at electron tube; Improve and keep vacuum certain in the device; Sudden venting when absorbing electron tube startup and what it perceives as anomalous operation, for device provides good vacuum environment, thus the service life of prolongation device.Compared to evaporable air-absorbing agent, nonevaporable getter has and does not pollute device, can reuse, and also can not cause advantages such as vacuum device after the use is not reworkable.Nonevaporable getter is known in the vacuum technique field; And successfully in the various devices that need high vacuum condition, using for four more than ten years for the supply of condition of high vacuum degree and maintenance, these need the device of high vacuum environments to comprise fields such as atomic clock, proton precessional magnetometer, heat insulation vessel and cathode-ray tube.Nonevaporable getter also often is applied in the purification field of inert gas.Nonevaporable getter commonly used has: ternary alloy three-partalloy Zr-V-Fe; The Zr-Al alloy; Quaternary alloy Zr-V-Fe-Ti.These getter elements are mainly processed from several microns powder to the hundreds of micron by granularity.In most cases, these powder are pressed into difform goods (like sheet, ring-type, plate-like etc.) or are rolled into band shape, and are different according to instructions for use, can take sintering process, perhaps just can use behind the straight forming.
Nonevaporable getters such as zirconium aluminium commonly used at present, zirconium vanadium iron all prepare through powder extrusion forming sintering technology or similar techniques, and this type getter material intensity is low.Thermal stress in use and mechanical load all possibly make getter element fracture or loose, and the situation of shedding takes place, and this can have a strong impact on vacuum system equipment, are not allow situation about occurring; And existing nonevaporable getter is to H
2Gettering rate low, gulp capacity is not enough.Adopt moulding, the sintering process of existing getter alloys powder, can not prepare and not only have than higher intensity, but also have the air suction element of good pumping property.
Summary of the invention
The purpose of this invention is to provide a kind of non-evaporable fiber silk type getter, solve the shedding problem that occurs in the nonevaporable getter use, and to H
2High, the gulp capacity foot of gettering rate.
Another object of the present invention provides the preparation method of above-mentioned non-evaporable fiber silk type getter.
The technical scheme that the present invention adopted is, non-evaporable fiber silk type getter, by mass percentage; Its component is Ti 80%-92%, Ni 5%-12%; V 3%-8%, the mass percent sum of said components is 100%, wherein; Ti is high-purity titanium sponge of purity 99.1%-99.7%, and impurity elements Al, O element quality account for respectively below the 80ppm of getter gross mass in the getter, and impurity element C, Fe, Si, N element quality account for respectively below the 20ppm of getter gross mass.
Another technical scheme that the present invention adopted is, the preparation method of non-evaporable fiber silk type getter specifically carries out according to following steps:
Step 1,
By mass percentage, take by weighing the metal Ti of 80%-92%, the metal Ni of 5%-12%, the metal V of 3%-8%, the mass percent sum of said components is 100%,
Wherein, Ti is high-purity titanium sponge of purity 99.1%-99.7%, and impurity elements Al, O element quality account for respectively below the 80ppm of getter gross mass in the getter, and impurity element C, Fe, Si, N element quality account for respectively below the 20ppm of getter gross mass;
Step 2,
Three kinds of metals of titanium, nickel, vanadium that step 1 is taken by weighing place water jacketed copper crucible, and carry out the melting first time: the forvacuum degree is lower than 8 * 10
-3Behind the Pa, send electrical heating; Send electrical power and time relationship to be: 0-2min, power are 60-80kw; 2-6min, power are 100-150kw; 6-10min, power are 200-220kw; 10-15min, power are 250-270kw; In the fusion process, the working vacuum degree is not less than 3 * 10
-2Pa; Behind the alloy molten, the applying argon gas protection is cooled off; Adopt identical step then, melting is 3 times altogether, obtains complete alloying ingot casting;
Step 3,
The complete alloying ingot casting that step 2 is made; Forge at 950-1200 ℃, make the ingot casting cross-sectional diameter be former diameter of section 0.5-0.75 doubly, the ingot casting after the forging carries out annealing in process at 700-850 ℃; Then the ingot casting after the annealing is carried out finishing and handle, obtain the finishing alloy pig;
Step 4,
The finishing alloy pig that step 3 obtains is removed surface contamination; Carry out the refined fiber wire process: the finishing alloy pig is fixed on the wire producing machine, regulates the wire producing machine rotating speed at 300-750 rev/min, the filametntary cross section that processes is for oval; Long axis of ellipse length is 0.30-0.80mm; Minor axis length is 0.03-0.10mm, and through compacting preformed, briquetting pressure is 0.8T/cm then
2, obtain preform;
Step 5,
The preform that step 4 is obtained adopts vacuum drying oven to carry out sintering, and sintering temperature is 900-1250 ℃, is incubated 2 hours, cools to applying argon gas below 400 ℃ with the furnace, is cooled to normal temperature and comes out of the stove, and promptly gets.
The non-evaporable fiber silk type getter that the present invention prepares is the alloy of host element with the titanium, because titanium elements is an active element, is prone to and reaction bonded such as hydrogen, carbon dioxide, nitrogen, steam, and metal Ni can form intermetallic compound T with titanium
2Ni, TiNi, Ti
3Ni etc., these compounds have better adsorption capability to active gases, wherein to H
2Suction-operated particularly outstanding; Metal V can form multiple intermetallic compound with Ni, like Ni
3V, Ni
2V, NiV
3Deng, these compounds all have good absorbability to active gases, are prone to and reaction bonded such as hydrogen, carbon dioxide, nitrogen, steam.The Ni, the V intermediate alloy that add make this filament have higher intensity, not easy fracture shedding in use.
The specific embodiment
Through the specific embodiment the present invention is elaborated below.
Non-evaporable fiber silk type getter of the present invention, by mass percentage, its component does,
Ti 80%-92%, Ni 5%-12%, V 3%-8%, the mass percent sum of said components is 100%.
Wherein, Ti is high-purity titanium sponge of purity 99.1%-99.7%, and impurity elements Al, O element quality account for respectively below the 80ppm of getter gross mass in the getter, and impurity element C, Fe, Si, N element quality account for respectively below the 20ppm of getter gross mass.
In the getter of the present invention, titanium is a base element.Titanium itself is a kind of gettering material of excellence, and titanium is to various active gases, and especially hydrogen has stronger affinity, and forms all cpds.But generally all there is one deck passivating film on pure titanium surface, must after high temperature, high vacuum activate this layer passivating film processing elimination, pumping property be arranged, and this has retrained the direct application of pure titanium under some conditions.For the expanding application scope, improve the pumping property and the intensity of getter, in titanium, added Ni, V metallic element.The Ni that adds can form intermetallic compound with titanium: like T
2Ni, TiNi, Ti
3Ni etc., these compounds have better adsorption capability to active gases, wherein to H
2Suction-operated particularly outstanding; Metal V can form multiple intermetallic compound with Ni, like Ni
3V, Ni
2V, NiV
3Deng, these compounds all have good absorbability to active gases.In addition, the adding of Ni, V intermediate alloy can effectively improve the filametntary intensity of this getter, the use dry linting that can not rupture.
The preparation method of non-evaporable fiber silk type getter of the present invention, specifically carry out according to following steps:
Step 1,
By mass percentage, take by weighing the metal Ti of 80%-92%, the metal Ni of 5%-12%, the metal V of 3%-8%, the mass percent sum of each component is 100%,
Wherein, Ti is high-purity titanium sponge of purity 99.1%-99.7%, and impurity elements Al, O element quality account for respectively below the 80ppm of getter gross mass in the getter, and impurity element C, Fe, Si, N element quality account for respectively below the 20ppm of getter gross mass;
Step 2,
Three kinds of metals of high-purity titanium sponge, nickel, vanadium that step 1 is taken by weighing place water jacketed copper crucible, and carry out the melting first time: the forvacuum degree is lower than 8 * 10
-3Behind the Pa, send electrical heating; Send electrical power and time relationship to be: 0-2min, power are 60-80kw; 2-6min, power are 100-150kw; 6-10min, power are 200-220kw; 10-15min, power are 250-270kw; In the fusion process, the working vacuum degree is not less than 3 * 10
-2Pa; Behind the alloy molten, the applying argon gas protection is cooled off; Adopt identical step then, melting is 3 times altogether, obtains complete alloying ingot casting;
Step 3,
The complete alloying ingot casting that step 2 is made; Forge at 950-1200 ℃; Make the ingot casting cross-sectional diameter be former diameter of section 0.5-0.75 doubly, the ingot casting after the forging carries out annealing in process at 700-850 ℃, changes its tensile property; Then the ingot casting after the annealing is carried out finishing and handle, obtain the finishing alloy pig;
Step 4,
The finishing alloy pig that step 3 obtains is removed surface contamination; Carry out the refined fiber wire process: the finishing alloy pig is fixed on the wire producing machine, regulates the wire producing machine rotating speed at 300-750 rev/min, the filametntary cross section that processes is for oval; Long axis of ellipse length is 0.30-0.80mm; Minor axis length is 0.03-0.10mm, and through compacting preformed, briquetting pressure is 0.8T/cm then
2, obtain preform.
Step 5,
The preform that step 4 is obtained adopts vacuum drying oven to carry out sintering, and sintering temperature is 900-1250 ℃, is incubated 2 hours, cools to applying argon gas below 400 ℃ with the furnace, is cooled to normal temperature and comes out of the stove, and promptly gets.
Embodiment 1
Get high-purity titanium sponge of 92%, 5% Ni and 3% V by mass percentage; Wherein impurity elements Al, O element quality account for respectively below the 80ppm of getter gross mass, and impurity element C, Fe, Si, N element quality account for respectively below the 20ppm of getter gross mass; Titanium, nickel, three kinds of metals of vanadium are placed water jacketed copper crucible, and carry out the melting first time: the forvacuum degree is lower than 8 * 10
-3Behind the Pa, send electrical heating; Send electrical power and time relationship to be: 0-2min, power are 60kw; 2-6min, power are 100kw; 6-10min, power are 200kw; 10-15min, power are 250kw; In the fusion process, the working vacuum degree is not less than 3 * 10
-2Pa; Behind the alloy molten, the applying argon gas protection is cooled off; Adopt identical step then, melting is 3 times altogether, obtains complete alloying ingot casting; Continuation is forged at 950 ℃, and making the ingot casting cross-sectional diameter is 0.5 times of former diameter of section.Ingot casting after the forging carries out annealing in process at 700 ℃, obtains the finishing alloy pig; Again the finishing alloy pig is removed surface contamination; The finishing alloy pig is fixed on the wire producing machine, regulates the wire producing machine rotating speed at 300 rev/mins, the filametntary cross section that processes is for oval; Long axis of ellipse length is 0.30mm; Minor axis length is 0.03mm, and through compacting preformed, briquetting pressure is 0.8T/cm then
2Adopt vacuum-sintering then, sintering temperature is 900 ℃, is incubated 2 hours, cools to applying argon gas below 400 ℃ with the furnace, is cooled to normal temperature and comes out of the stove, and promptly gets.
Embodiment 2
Get high-purity titanium sponge of 80%, 12% Ni and 8% V by mass percentage; Wherein impurity elements Al, O element quality account for respectively below the 80ppm of getter gross mass, and impurity element C, Fe, Si, N element quality account for respectively below the 20ppm of getter gross mass; Titanium, nickel, three kinds of metals of vanadium are placed water jacketed copper crucible, and carry out the melting first time: the forvacuum degree is lower than 8 * 10
-3Behind the Pa, send electrical heating; Send electrical power and time relationship to be: 0-2min, power are 80kw; 2-6min, power are 150kw; 6-10min, power are 220kw; 10-15min, power are 270kw; In the fusion process, the working vacuum degree is not less than 3 * 10
-2Pa; Behind the alloy molten, the applying argon gas protection is cooled off; Adopt identical step then, melting is 3 times altogether, obtains complete alloying ingot casting; Forge at 1200 ℃, making the ingot casting cross-sectional diameter is 0.75 times of former diameter of section.Ingot casting after the forging carries out annealing in process at 850 ℃, obtains the finishing alloy pig; Again the finishing alloy pig is removed surface contamination; The finishing alloy pig is fixed on the wire producing machine, regulates the wire producing machine rotating speed at 750 rev/mins, the filametntary cross section that processes is for oval; Long axis of ellipse length is 0.80mm; Minor axis length is 0.10mm, and through compacting preformed, briquetting pressure is 0.8T/cm then
2Adopt vacuum-sintering then, sintering temperature is 1250 ℃, is incubated 2 hours, cools to applying argon gas below 400 ℃ with the furnace, is cooled to normal temperature and comes out of the stove, and promptly gets.
Embodiment 3
Get high-purity titanium sponge of 87%, 7.8% Ni and 5.2% V by mass percentage; Wherein impurity elements Al, O element quality account for respectively below the 80ppm of getter gross mass, and impurity element C, Fe, Si, N element quality account for respectively below the 20ppm of getter gross mass; Titanium, nickel, three kinds of metals of vanadium are placed water jacketed copper crucible, and carry out the melting first time: the forvacuum degree is lower than 8 * 10
-3Behind the Pa, send electrical heating; Send electrical power and time relationship to be: 0-2min, power are 70kw; 2-6min, power are 120kw; 6-10min, power are 210kw; 10-15min, power are 260kw; In the fusion process, the working vacuum degree is not less than 3 * 10
-2Pa; Behind the alloy molten, the applying argon gas protection is cooled off; Adopt identical step then, melting is 3 times altogether, obtains complete alloying ingot casting; Forge at 1100 ℃, making the ingot casting cross-sectional diameter is 0.6 times of former diameter of section.Ingot casting after the forging carries out annealing in process at 780 ℃, obtains the finishing alloy pig; Again the finishing alloy pig is removed surface contamination; The finishing alloy pig is fixed on the wire producing machine, regulates the wire producing machine rotating speed at 520 rev/mins, the filametntary cross section that processes is for oval; Long axis of ellipse length is 0.50mm; Minor axis length is 0.05mm, and through compacting preformed, briquetting pressure is 0.8T/cm then
2Adopt vacuum-sintering then, sintering temperature is 1100 ℃, is incubated 2 hours, cools to applying argon gas below 400 ℃ with the furnace, is cooled to normal temperature and comes out of the stove, and promptly gets.
Get the getter that embodiment 1-embodiment 3 makes respectively, test it gettering rate of the tenth minute of hydrogen is respectively 2103cm
3/ gs, 2315cm
3/ gs, 2395cm
3/ gs.Under common same condition, with ZrAl
16Nonevaporable getter carries out the performance test contrast.ZrAl
16The tenth minute hydrogen-absorption speed is 1142cm
3/ gs, and the tenth minute hydrogen-absorption speed of getter of the present invention is all greater than 2100cm
3/ gs.Getter is after 900 ℃ of activation, and the gettering rate to hydrogen was respectively 3365.47cm in the tenth minute
3/ gs, 3390.52cm
3/ gs, 3398.41cm
3/ gs.
The getter that makes through embodiment 1-embodiment 3 is after 900 ℃ of activation, and hydrogen absorption capacity was respectively 3532.24cm in the 60th minute
3Pa/g, 3583.52cm
3Pa/g, 3601.70cm
3Pa/g.And ZrAl
16The 60th minute hydrogen absorption capacity of nonevaporable getter is 2421cm
3Pa/g.
Get 5 the 10 filament getter samples that restrain that embodiment 1-embodiment 3 prepares respectively, get the ZrAl of 5 10 grams again
16The nonevaporable getter powdered sample makes a strength test, and it is highly fallen from 3 meters, and filament getter sample weight has no loss, and ZrAl
16Powdered sample all has fracture, shedding situation in various degree, and the loss in weight is between the 0.43-1.6 gram.
In sum, the filament getter of the inventive method preparation has effectively improved the pumping property of getter; Gettering rate is high; Especially hydrogen is had the good adsorption binding ability, and gulp capacity is big, intensity is good; Can not rupture, the dry linting phenomenon, can reliably be applied to vacuum and require severe rugged environment.
Claims (1)
1. the preparation method of a non-evaporable fiber silk type getter, specifically carry out according to following steps:
Step 1,
By mass percentage, take by weighing the metal Ti of 80%-92%, the metal Ni of 5%-12%, the metal V of 3%-8%, the mass percent sum of said components is 100%,
Wherein, Ti is high-purity titanium sponge of purity 99.1%-99.7%, and impurity elements Al, O element quality account for respectively below the 80ppm of getter gross mass in the getter, and impurity element C, Fe, Si, N element quality account for respectively below the 20ppm of getter gross mass;
Step 2,
Three kinds of metals of titanium, nickel, vanadium that step 1 is taken by weighing place water jacketed copper crucible, and carry out the melting first time: the forvacuum degree is lower than 8 * 10
-3Behind the Pa, send electrical heating; Send electrical power and time relationship to be: 0-2min, power are 60-80kw; 2-6min, power are 100-150kw; 6-10min, power are 200-220kw; 10-15min, power are 250-270kw; In the fusion process, the working vacuum degree is not less than 3 * 10
-2Pa; Behind the alloy molten, the applying argon gas protection is cooled off; Adopt identical step then, melting is 3 times altogether, obtains complete alloying ingot casting;
Step 3,
The complete alloying ingot casting that step 2 is made; Forge at 950-1200 ℃, make the ingot casting cross-sectional diameter be former diameter of section 0.5-0.75 doubly, the ingot casting after the forging carries out annealing in process at 700-850 ℃; Then the ingot casting after the annealing is carried out finishing and handle, obtain the finishing alloy pig;
Step 4,
The finishing alloy pig that step 3 obtains is removed surface contamination; Carry out the refined fiber wire process: the finishing alloy pig is fixed on the wire producing machine, regulates the wire producing machine rotating speed at 300-750 rev/min, the filametntary cross section that processes is for oval; Long axis of ellipse length is 0.30-0.80mm; Minor axis length is 0.03-0.10mm, and through compacting preformed, briquetting pressure is 0.8T/cm then
2, obtain preform; Step 5,
The preform that step 4 is obtained adopts vacuum drying oven to carry out sintering, and sintering temperature is 900-1250 ℃, is incubated 2 hours, cools to applying argon gas below 400 ℃ with the furnace, is cooled to normal temperature and comes out of the stove, and promptly gets.
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CN104181655A (en) * | 2014-03-11 | 2014-12-03 | 黄燕生 | Fiber filling paste and preparation method thereof |
CN110614361B (en) * | 2019-10-16 | 2022-10-14 | 上海晶维材料科技有限公司 | Method for preparing block getter by microwave sintering |
CN115672254A (en) * | 2022-11-17 | 2023-02-03 | 北京锦正茂科技有限公司 | Activation-free gas adsorbent used in cryostat and preparation method thereof |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1312395A (en) * | 2000-12-26 | 2001-09-12 | 西北有色金属研究院 | Zr-Ni alloy powder producing method |
US6398980B1 (en) * | 1997-03-28 | 2002-06-04 | Tovarischestvo S Ogranichennoi Otvetstvennest Ju “Tekhnovak+ ” | Method for producing a nonevaporable getter |
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Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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US6398980B1 (en) * | 1997-03-28 | 2002-06-04 | Tovarischestvo S Ogranichennoi Otvetstvennest Ju “Tekhnovak+ ” | Method for producing a nonevaporable getter |
CN1312395A (en) * | 2000-12-26 | 2001-09-12 | 西北有色金属研究院 | Zr-Ni alloy powder producing method |
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Address after: The northern section of the economic and Technological Development Zone Jingwei Town Road 710201 Shaanxi city of Xi'an province Weihua No. 12 Patentee after: Western Baode Technologies Co., Ltd. Address before: 710016 Shaanxi province Xi'an Weiyang Weiyang Road No. 96 Patentee before: Xi'an Baode Powder Metallurgy Co., Ltd. |