CN103801252A - Degassing agent with protective layer as well as preparation method thereof - Google Patents

Degassing agent with protective layer as well as preparation method thereof Download PDF

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Publication number
CN103801252A
CN103801252A CN201210461386.7A CN201210461386A CN103801252A CN 103801252 A CN103801252 A CN 103801252A CN 201210461386 A CN201210461386 A CN 201210461386A CN 103801252 A CN103801252 A CN 103801252A
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getter
particles
protective layer
getter particles
core
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杜军
崔航
张心强
朱君
田士法
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Beijing General Research Institute for Non Ferrous Metals
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Beijing General Research Institute for Non Ferrous Metals
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Abstract

The invention relates to a degassing agent with a protective layer as well as a preparation method thereof. The degassing agent provided by the invention is composed of degassing agent particles of dual-layer structures; the core comprises the main components of Zr, V and Fe; the protective layer comprises the main component of Ni. According to the invention, the degassing agent particles with the protective layer are prepared by chemical coating, and the degassing agent with the protective layer is prepared by compressing and sintering; the surfaces of the degassing agent particles are coated with a Ni protective layer; Ni has a dissociation function to a hydrogen molecule and can improve the absorbing capacity of hydrogen, and moreover, the protective layer can prevent oxygen adsorption and reduce the activation temperature. The degassing agent provided by the invention can be activated in the process of baking at 180-350 DEG C, has a favorable degassing function after baking at room temperature, and can be used for absorbing and removing internal residual gases in high-vacuum devices.

Description

A kind of getter with matcoveredn and preparation method thereof
Technical field
The present invention relates to a kind of getter with matcoveredn and preparation method thereof, getter of the present invention is a kind of high-performance low-temp activation nonevaporable getter.
Background technology
Getter is one of effective means of gas clean-up.Getter can be reacted or adsorb with active gases molecule by physics or chemical action, thereby effectively improves the vacuum in device.
Conventional gettering material has alloy or the compound of barium, strontium, magnesium, calcium, titanium, zirconium, hafnium, vanadium, barium aluminium alloy or transition metal and aluminium or rare earth element, wherein bianry alloy is as Ba-Al, Ti-V, Zr-Al etc., and ternary alloy three-partalloy is as Ba-Al-Ni, Zr-V-Fe, Ti-Zr-V etc.This class material generally has very high activity, low saturated vapor pressure and bigger serface, to the residual activity gas in electrovacuum as H 2, O 2, N 2, CO and C mh ndeng, the absorption that tool is very strong or absorbability.
Application at present more widely getter is mainly Zr-Al getter, Zr-C getter etc.These getters mainly have the following disadvantages: (1) getter activationary temperature is higher, and temperature range, at 500 ~ 900 ℃, has certain limitation for the use of high accuracy microelectronic component; (2) getter is very easily oxidized under the state that exposes atmosphere, and the life-span of getter is short.
Summary of the invention
The object of this invention is to provide a kind of nonevaporable getter, is to be formed by getter particles compacting, the sintering with protective layer, has the feature of low-temp activation and has high pumping property.
In the present invention, adopt Zr-V-Fe alloy as getter particles core, hydrogen atom rich V in alloy has higher diffusion velocity in mutually, and Zr-V-Fe alloy has lower activationary temperature, 350 ~ 450 ℃.Improve getter activity, strengthened gettering ability.Method by chemical plating is prepared layer of Ni layer in getter particles core, because Ni layer can reduce the dissociation energy of hydrogen molecule on getter surface, improves the chemisorbed rate on getter surface, has improved gettering rate and the inspiratory capacity of getter.Meanwhile, Ni layer has effectively stoped the oxidation of oxygen isoreactivity gas to getter particles core, thereby has reduced the activationary temperature of getter, and has extended the service life of getter.This getter is to adopt the method for compacting and sintering to be prepared from, and is in getter body, to form loose structure, effectively raises the specific area of getter, has improved air-breathing active area and gettering rate.
The invention provides a kind of getter with matcoveredn, be made up of getter particles, described getter particles has double-decker, and the main component of the core of gettering layer particle is Zr, V and Fe, and the main component of the protective layer of getter particles is Ni.
In the absorption core of described getter particles, the mass content that the mass content that the mass content of Zr is 60 ~ 80%, V is 10 ~ 35%, Fe is 1% ~ 10%.The mass percent sum of said components is 100%.
In the protective layer of described getter particles, the mass content of Ni is more than or equal to 99.5%.
The particle size range of the core of described getter particles is 20 ~ 200 μ m, preferably 50 ~ 100 μ m.The thickness of the protective layer of described getter particles is 10 ~ 80nm.
In the present invention, gettering layer is to the H except inert gas 2, O 2, N 2, CO, CO 2and C mh nthere is good absorption ability Deng gas.And the protective layer above gettering layer, to the selective adsorption function of hydrogen atom, can play a protective role to gettering layer, greatly reduces O 2to the oxidation of gettering layer.
The activationary temperature of getter of the present invention is low, directly realizes afterwards surface activation 180 ~ 350 ℃ of bakings, and activationary time is 60 ~ 180min, has good pumping property, to H 2, CO, O 2, N 2, CO 2isoreactivity gas has high gettering rate and inspiratory capacity.
The present invention provides a kind of preparation method of above-mentioned getter simultaneously.The air-breathing core of getter particles of the present invention becomes ingot by alloy melting; and be prepared from through pulverizing; adopt again the method for chemical plating to prepare layer protective layer in getter particles core surfaces; then surface is there is to getter particles compacting (ring or piece) base substrate in flakes of protective layer; and through oversintering, preparation has double-deck getter.
The preparation method of the getter of band matcoveredn of the present invention, comprises the steps:
(1) meet the alloy cast ingot of getter particles core proportioning with vacuum arc furnace melting, under the atmosphere protection of argon gas, broken alloy cast ingot to diameter is 20 ~ 200 μ m, obtains getter particles core;
(2), by washed with de-ionized water getter particles core, corrode getter particles with HF, then use washed with de-ionized water;
(3) prepare chemical nickel-plating solution, chemical nickel-plating solution is NiCl 26H 2o, Na 3c 6h 5o 72H 2o, H 3bO 3and NaH 2pO 2h 2the aqueous solution of O, pH is 7 ~ 11;
(4) chemical nickel-plating solution constant water bath box step (3) being obtained is heated to 45 ~ 85 ℃; Stirring under the state of plating solution, add getter particles core, plating 5 ~ 25min(temperature remains on 45 ~ 85 ℃);
(5) after plating finishes, remove plating solution, use washed with de-ionized water getter particles; The getter particles of preparation is dry in vacuum drying chamber;
(6) by the compacting of dried getter particles in flakes, ring or block base substrate;
(7) the getter base substrate of preparation in step (6) is put into vacuum sintering furnace and carry out sintering.
In step (2), the concentration of described HF is 0.1 ~ 1.3wt.%, and the time of corrosion getter particles is 60 ~ 300s.
In step (3), NiCl in chemical nickel-plating solution 26H 2the concentration of O is 15 ~ 35g/L, Na 3c 6h 5o 72H 2the concentration of O is 30 ~ 50g/L, H 3bO 3concentration be 30 ~ 50g/L, NaH 2pO 2h 2the concentration of O is 10 ~ 30g/L; The step of preparing chemical nickel-plating solution comprises: as coating bath, use 1/3rd water yield heating for dissolving NiCl of coating bath volume with stainless steel 26H 2o, the water yield with other 1/3rd is dissolved Na 3c 6h 5o 72H 2o and H 3bO 3, then by NiCl 26H 2o solution is under agitation poured Na into 3c 6h 5o 72H 2o and H 3bO 3in solution, clarification filtration; With remaining 1/3rd water yields dissolving NaH 2pO 2h 2o, filters, and under agitation pours in above-mentioned mixed liquor, be diluted to cumulative volume, use 1:10(volume ratio) sulfuric acid or 1:4(volume ratio) ammoniacal liquor adjusting pH value to 7 ~ 11.
In step (5), described dry temperature is 40 ℃, and be 4 ~ 6h drying time.
In step (7), the temperature of described sintering is 450 ~ 1000 ℃, and sintering time is 10 ~ 20min.
In the present invention, adopt the preparation technology of compacting and sintering, improved the specific area of getter, formed larger effective air-breathing area, improved the gettering rate of getter.
The getter of band matcoveredn of the present invention can be applied in microelectromechanical systems (MEMS), flat-panel monitor (OLED/FED/LCD), solar energy heat-insulating shield equal vacuum degree require high, activation condition is required in strict environment.
Getter advantage prepared by the present invention is: preparing getter particles by the means of chemical plating is double-decker; at getter particles surface deposition Ni protective layer; Ni layer can reduce the dissociation energy of hydrogen molecule on getter surface; improve the chemisorbed rate on getter surface, improved gettering rate and the inspiratory capacity of getter.Meanwhile, Ni layer has effectively stoped the oxidation of oxygen isoreactivity gas to getter particles core, thereby has reduced the activationary temperature of getter, and has extended the service life of getter.The present invention can realize activation in 180 ~ 350 ℃ of bake process, can be good at avoiding the damage to device in activation.The present invention adopts Zr-V-Fe alloy as getter particles core, and hydrogen atom rich V in alloy has higher diffusion velocity in mutually, and Zr-V-Fe alloy has lower activationary temperature, and 350 ~ 450 ℃, activationary time is 60 ~ 120min.Improve getter activity, strengthened gettering ability.
Below by the drawings and specific embodiments, the present invention will be further described, but and do not mean that limiting the scope of the invention.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the getter of band matcoveredn of the present invention.
Fig. 2 is the schematic diagram without the getter of protective layer.
Fig. 3 is the pumping property comparison diagram of comparative example and embodiment 1,2,3 gained getters.
The specific embodiment
The getter (as embodiment 1-3) of band matcoveredn of the present invention as shown in Figure 1, is coated with Ni protective layer 2 in Zr-V-Fe getter particles core 1.Fig. 2 is the schematic diagram without protective layer getter (as comparative example), in Zr-V-Fe getter particles 3, there is no protective layer.
Comparative example
Use vacuum arc furnace melting Zr-V-Fe alloy; wherein each constituent mass mark is (Zr:70%; V24.6%; Fe:5.4%); under argon shield, be crushed to particle diameter at 50 ~ 100 μ m, getter particles is compressing, then put into vacuum sintering furnace and carry out sintering; sintering temperature is 870 ℃, and sintering time is 10min.The getter that obtains under this technological parameter presents loose structure, and activationary temperature is 350 ~ 450 ℃.
Embodiment 1
Use vacuum arc furnace melting Zr-V-Fe alloy, wherein each constituent mass mark is (Zr:80%, V:10%, Fe:10%), is crushed to particle diameter at 50 ~ 100 μ m under argon shield, obtains getter particles core.
Adopt the method for chemical plating in getter particles core, to deposit layer of Ni protective layer.The processing step of deposition Ni protective layer: use washed with de-ionized water getter particles, with HF (0.1wt.%) corrosion getter particles 300s, then use washed with de-ionized water.Prepare chemical nickel-plating solution, as coating bath, use 1/3rd water yield heating for dissolving NiCl of coating bath volume with stainless steel 26H 2o (15g/L), the water yield with other 1/3rd is dissolved Na 3c 6h 5o 72H 2o (30g/L) and H 3bO 3(30g/L), then by NiCl 26H 2o solution is under agitation poured into wherein, and clarification filtration, with remaining 1/3rd water yields dissolving NaH 2pO 2h 2o (20g/L), filters, and under stirring, pours in above-mentioned mixed liquor, is diluted to cumulative volume, with the sulfuric acid of 1:10 or the ammoniacal liquor of 1:4 adjusting pH to 7.Plating solution is heated to 45 ℃, stirring under the state of plating solution, adds getter particles, plating 25min.After plating finishes, remove plating solution, use washed with de-ionized water getter particles.The getter particles of preparation is dry in vacuum drying chamber, and temperature is 40 ℃, and be 4h drying time.Then the getter particles with protective layer of preparation is suppressed and sintering 20min at 450 ℃.
Under this technological parameter, the getter obtaining is loose structure, and getter particles protective layer thickness is 40 ~ 80nm, and the mass content of Ni is 99.7%.Getter particles core diameter is 60 ~ 80 μ m, and getter activationary temperature is 350 ℃, activationary time 60min.
Embodiment 2
Use vacuum arc furnace melting Zr-V-Fe alloy, wherein each constituent mass mark is (Zr:60%, V:35%, Fe:5%), is crushed to particle diameter at 50 ~ 100 μ m under argon shield, obtains getter particles core.
Adopt the method for chemical plating in getter particles core, to deposit layer of Ni protective layer.The processing step of deposition Ni protective layer: use washed with de-ionized water getter particles, with HF (1.3wt.%) corrosion getter particles 60s, then use washed with de-ionized water.Prepare chemical nickel-plating solution, as coating bath, use 1/3rd water yield heating for dissolving NiCl of coating bath volume with stainless steel 26H 2o (25g/L), the water yield with other 1/3rd is dissolved Na 3c 6h 5o 72H 2o (50g/L) and H 3bO 3(36g/L), then by NiCl 26H 2o solution is under agitation poured into wherein, and clarification filtration, with remaining 1/3rd water yields dissolving NaH 2pO 2h 2o (10g/L), filters, and under stirring, pours in above-mentioned mixed liquor, is diluted to cumulative volume, with the sulfuric acid of 1:10 or the ammoniacal liquor of 1:4 adjusting pH to 11.Plating solution is heated to 50 ℃, stirring under the state of plating solution, adds getter particles, plating 10min.After plating finishes, remove plating solution, use washed with de-ionized water getter particles.The getter particles of preparation is dry in vacuum drying chamber, and temperature is 40 ℃, and be 6h drying time.Then the getter particles with protective layer of preparation is suppressed and sintering 10min at 1000 ℃.
Under this technological parameter, the getter obtaining is loose structure, and getter particles protective layer thickness is 10 ~ 50nm, and the mass content of Ni is 99.5%.Getter particles core diameter is 70 ~ 100 μ m, and getter activationary temperature is 180 ℃, activationary time 120min.
Embodiment 3
Use vacuum arc furnace melting Zr-V-Fe alloy, wherein each constituent mass mark is (Zr:79%, V:20%, Fe:1%), is crushed to particle diameter at 50 ~ 100 μ m under argon shield, obtains getter particles core.
Adopt the method for chemical plating in getter particles core, to deposit layer of Ni protective layer.The processing step of deposition Ni protective layer: use washed with de-ionized water getter particles, with HF (1.0wt.%) corrosion getter particles 200s, then use washed with de-ionized water.Prepare chemical nickel-plating solution, as coating bath, use 1/3rd water yield heating for dissolving NiCl of coating bath volume with stainless steel 26H 2o (35g/L), the water yield with other 1/3rd is dissolved Na 3c 6h 5o 72H 2o (45g/L) and H 3bO 3(50g/L), then by NiCl 26H 2o solution is under agitation poured into wherein, and clarification filtration, with remaining 1/3rd water yields dissolving NaH 2pO 2h 2o (30g/L), filters, and under stirring, pours in above-mentioned mixed liquor, is diluted to cumulative volume, with the sulfuric acid of 1:10 or the ammoniacal liquor of 1:4 adjusting pH to 10.Plating solution is heated to 85 ℃, stirring under the state of plating solution, adds getter particles, plating 5min.After plating finishes, remove plating solution, use washed with de-ionized water getter particles.The getter particles of preparation is dry in vacuum drying chamber, and temperature is 40 ℃, and be 4h drying time.Then the getter particles with protective layer of preparation is suppressed and sintering 15min at 870 ℃.
Under this technological parameter, the getter obtaining is loose structure, and getter particles protective layer thickness is 30 ~ 70nm, and the mass content of Ni is 99.8%.Getter particles core diameter is 50 ~ 90 μ m, and getter activationary temperature is 250 ℃, activationary time 80min.
As shown in Figure 3; for comparative example and embodiment 1; 2; pumping property contrast under 3 techniques after the activation of gained getter; wherein be respectively embodiment 1,2 from top to bottom, 3 and the pumping property curve of comparative example; this shows, the pumping property of the getter of band matcoveredn of the present invention is significantly better than the getter with protective layer not.
The present invention is by the get everything ready getter particles of matcoveredn of chemically plating, and prepares the getter with protective layer by compacting and sintering.Getter particles surface is coated with Ni protective layer, and Ni has to hydrogen molecule the function of dissociating, and can improve the adsorbance of hydrogen, and protective layer can hinder the absorption of oxygen, reduction activationary temperature.The present invention can realize activation in the process of 180 ~ 350 ℃ of bakings, and after baking, getter has good pumping property at ambient temperature.The getter of band matcoveredn of the present invention can be used for, in high vacuum device, absorbing inner residual gas.

Claims (10)

1. the getter with matcoveredn, is made up of getter particles, it is characterized in that: described getter particles has double-decker, and the main component of core is Zr, V and Fe, and the main component of protective layer is Ni.
2. the getter with matcoveredn according to claim 1, is characterized in that: in the core of described getter particles, the mass content that the mass content that the mass content of Zr is 60 ~ 80%, V is 10 ~ 35%, Fe is 1% ~ 10%; In the protective layer of described getter particles, the mass content of Ni is more than or equal to 99.5%.
3. the getter with matcoveredn according to claim 1, is characterized in that: the particle diameter of the core of described getter particles is 20 ~ 200 μ m, and the thickness of the protective layer of described getter particles is 10 ~ 80nm.
4. the getter with matcoveredn according to claim 3, is characterized in that: the particle diameter of the core of described getter particles is 50 ~ 100 μ m.
5. the getter with matcoveredn according to claim 1, is characterized in that: the activationary temperature of described getter is 180 ~ 350 ℃, and activationary time is 60 ~ 180min.
6. the preparation method of the getter with matcoveredn described in any one in claim 1-5, comprises the steps:
(1) meet the alloy cast ingot of getter particles core proportioning with vacuum arc furnace melting, under the atmosphere protection of argon gas, broken alloy cast ingot to diameter is 20 ~ 200 μ m, obtains getter particles core;
(2), by washed with de-ionized water getter particles core, corrode getter particles with HF, then use washed with de-ionized water;
(3) prepare chemical nickel-plating solution, chemical nickel-plating solution is NiCl 26H 2o, Na 3c 6h 5o 72H 2o, H 3bO 3and NaH 2pO 2h 2the aqueous solution of O, pH is 7 ~ 11;
(4) chemical nickel-plating solution constant water bath box step (3) being obtained is heated to 45 ~ 85 ℃; Stirring under the state of plating solution, add getter particles core, plating 5 ~ 25min;
(5) after plating finishes, remove plating solution, use washed with de-ionized water getter particles; The getter particles of preparation is dry in vacuum drying chamber;
(6) by the compacting of dried getter particles in flakes, ring or block base substrate;
(7) the getter base substrate of preparation in step (6) is put into vacuum sintering furnace and carry out sintering.
7. the preparation method of the getter with matcoveredn according to claim 6, is characterized in that: in described chemical nickel-plating solution, and NiCl 26H 2the concentration of O is 15 ~ 35g/L, Na 3c 6h 5o 72H 2the concentration of O is 30 ~ 50g/L, H 3bO 3concentration be 30 ~ 50g/L, NaH 2pO 2h 2the concentration of O is 10 ~ 30g/L.
8. the preparation method of the getter with matcoveredn according to claim 7, is characterized in that: the step of preparing chemical nickel-plating solution comprises: as coating bath, use 1/3rd water yield heating for dissolving NiCl of coating bath volume with stainless steel 26H 2o, the water yield with other 1/3rd is dissolved Na 3c 6h 5o 72H 2o and H 3bO 3, then by NiCl 26H 2o solution is under agitation poured Na into 3c 6h 5o 72H 2o and H 3bO 3in solution, clarification filtration; With remaining 1/3rd water yields dissolving NaH 2pO 2h 2o, filters, and under agitation pours in above-mentioned mixed liquor, is diluted to cumulative volume, with the sulfuric acid of 1:10 or the ammoniacal liquor of 1:4 adjusting pH value to 7 ~ 11.
9. the preparation method of the getter with matcoveredn according to claim 6, is characterized in that: the concentration of described HF is 0.1 ~ 1.3wt.%, and the time of corrosion getter particles is 60 ~ 300s; Described dry temperature is 40 ℃, and be 4 ~ 6h drying time; The temperature of described sintering is 450 ~ 1000 ℃, and sintering time is 10 ~ 20min.
10. the application of the getter with matcoveredn described in any one in microelectromechanical systems, flat-panel monitor, solar energy heat-insulating shield in claim 1-5.
CN201210461386.7A 2012-11-15 2012-11-15 Degassing agent with protective layer as well as preparation method thereof Pending CN103801252A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104307461A (en) * 2014-10-24 2015-01-28 武汉钢铁(集团)公司 Getter for purifying krypton and xenon, and preparation method of getter
CN109834263A (en) * 2017-11-29 2019-06-04 北京有色金属研究总院 A kind of preparation method of high intensity high pumping property Zr-V system gettering material
CN110819849A (en) * 2019-10-16 2020-02-21 上海晶维材料科技有限公司 Preparation method of nano nickel protective layer getter material
CN114318233A (en) * 2021-12-10 2022-04-12 兰州空间技术物理研究所 Getter with thin film coating and preparation method and application thereof
CN114574721A (en) * 2022-03-01 2022-06-03 秦皇岛江龙吸气材料有限公司 Multi-element non-evaporable low-temp activated getter and its preparing process
CN115341120A (en) * 2022-07-06 2022-11-15 上海大学 Non-evaporable low-temperature activated zirconium-based getter alloy and preparation method thereof
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

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104307461A (en) * 2014-10-24 2015-01-28 武汉钢铁(集团)公司 Getter for purifying krypton and xenon, and preparation method of getter
CN109834263A (en) * 2017-11-29 2019-06-04 北京有色金属研究总院 A kind of preparation method of high intensity high pumping property Zr-V system gettering material
CN110819849A (en) * 2019-10-16 2020-02-21 上海晶维材料科技有限公司 Preparation method of nano nickel protective layer getter material
CN114318233A (en) * 2021-12-10 2022-04-12 兰州空间技术物理研究所 Getter with thin film coating and preparation method and application thereof
CN114574721A (en) * 2022-03-01 2022-06-03 秦皇岛江龙吸气材料有限公司 Multi-element non-evaporable low-temp activated getter and its preparing process
CN114574721B (en) * 2022-03-01 2022-12-13 秦皇岛江龙吸气材料有限公司 Multi-element non-evaporable low-temp activated getter and its preparing process
CN115341120A (en) * 2022-07-06 2022-11-15 上海大学 Non-evaporable low-temperature activated zirconium-based getter alloy and preparation method thereof
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

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Application publication date: 20140521