CN1429658A - Material for removing impurity in inert gas and its use method - Google Patents

Material for removing impurity in inert gas and its use method Download PDF

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Publication number
CN1429658A
CN1429658A CN01145123A CN01145123A CN1429658A CN 1429658 A CN1429658 A CN 1429658A CN 01145123 A CN01145123 A CN 01145123A CN 01145123 A CN01145123 A CN 01145123A CN 1429658 A CN1429658 A CN 1429658A
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China
Prior art keywords
inert gas
gas
impurity
content
zirconium
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CN01145123A
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CN1190262C (en
Inventor
胡小敏
陈雨田
熊贤信
陈文宇
杨江喜
田明勇
路家兵
陈光明
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Beijing Tejin Vacuum Electronic Technology Co Ltd
Oxygen Co Ltd Wuhan Iron & Steel Group
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Beijing Tejin Vacuum Electronic Technology Co Ltd
Oxygen Co Ltd Wuhan Iron & Steel Group
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Priority to CNB011451238A priority Critical patent/CN1190262C/en
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/151Reduction of greenhouse gas [GHG] emissions, e.g. CO2

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  • Drying Of Semiconductors (AREA)
  • Separation Of Gases By Adsorption (AREA)

Abstract

An alloy material for removing carbon fluoride compound (CF4 and C2F4) from inertial gas (Xe and Kr) contains Al (10-25 wt.%), Hf (1-2), La-series RE (0.1-5), Ni (1-3) and Zr (the rest). It is applied through activating at 700-960 deg.C for 2-3 hr, and adsorbing the impurities (CF4 and C2F4) at 400-960 deg.c and under 0.3-1.5 MPa, while gas flow-is controlled at 0.5-10 cu.m/hr. Its advantages are high effect (making purity of inertial gas greater than 99.9999%), and no absorption of inertial gas.

Description

A kind of material and using method thereof of removing impurity in the inert gas
(1) technical field
A kind of material and using method thereof of removing impurity in the inert gas, relate to a kind of removal and be used for the inert gas xenon that is filled with in semiconductor, high pure metal industry, chemical analysis analysis and various particular electrical light source, Laser Devices, the electro-optical device, particularly high-power illumination lamp, the material and the using method thereof of the fluorocarbons impurities in the krypton.
(2) background technology
High purity inert gas is carrier and protective atmosphere and the important source material that semiconductor, high pure metal industry, chemical analysis analysis, various particular electrical light source, Laser Devices and multiple high pure raw material and technical process must adopt, and occupies important status in modern science and technology and industrial development.The method that is used for high purity inert gas production at present has multiple, and the purification process of gas has air separating method, absorption process and absorption method etc.Can remove the O of active gases in this way effectively 2, N 2, CO, H 2Impurity such as O satisfy certain industrial use.But usually not really desirable for containing the fluorocarbons removal effect in the gas, the fluorocarbons content in the inert gas after the processing is higher than 50ppm, is difficult to satisfy the industrial use high to the indifferent gas purity requirement, as particular electrical light source etc. to the inert gas requirement.Because the influence of purity inert gas, present vaporificly in high-power illumination lamp inside, the filament blackout has influenced product quality.To the inert gas of specific use, the height of purity is unusual important index.In present existing gas purification technology, in inert gas, the CF in krypton gas, the xenon particularly 4With C 2F 6The removal method does not also have highly effective method.
(3) summary of the invention
The objective of the invention is the deficiency that exists at above-mentioned prior art, provide a kind of in the removal inert gas that can effectively remove fluorocarbons the material and the using method thereof of impurity.
The objective of the invention is to be achieved through the following technical solutions.
A kind of material of removing impurity in the inert gas, it is characterized in that this material is a kind of zircaloy, the percentage by weight of this alloy consists of: contain aluminium 10%-25%, contain hafnium 1%-2%, lanthanide rare 0.4%-5%, nickel 1%-3%, surplus is zirconium and unavoidable impurities, its material is the 0.05mm-2.5mm particle.
A kind of material of removing impurity in the inert gas of the present invention also can be the voluminous powder sintered body.
Contain the Titanium element that percentage by weight is 1%-4% in a kind of zircaloy of removing the material of impurity in the inert gas of the present invention.
A kind of using method of removing the material of impurity in the inert gas is characterized in that its use is:
The material that a. will be used for removing inert gas impurity is packed in the rustless steel container of the Purge gas that has the gateway, and vacuumizing and exhausting to vacuum is 10 -3Behind the Pa, charge into inert gas, 700 ℃ of-960 ℃ of temperature of intensification, be incubated 2-3 hour, will carry out activation processing;
B. the inert gas that desire is purified feeds and is equipped with in the degasification container of material, carries out the gas purification process of absorbing gaseous impurities under 400 ℃ of-960 ℃ of temperature, and the control gas flow is 0.5m 3/ h-10m 3/ h, operating pressure is 0.3MPa-1.5MPa.
Inert gas purge material of the present invention does not absorb inert gas.This material has can remove fluorocarbons (CF effectively 4, C 2F 4) etc. special nature.Purity inert gas is greater than 99.9999% behind the purifying, and fluorocarbons content is less than 3ppm.When purifying krypton, xenon-133 gas through method of the present invention, the C in krypton, the xenon-133 gas 2F and C 2F 4Content is all reduced to 0.5ppm from 10ppm, and the gas loss rate is being lower than 5%, and effect is extremely remarkable.
(4) specific embodiment
A kind of material of removing impurity in the inert gas, this material are a kind of zirconium alloy, and its percentage by weight consists of: contain aluminium 10%-25%, contain hafnium 1%-2%, lanthanide rare 0.4%-5%, nickel 1%-3%, surplus is zirconium and unavoidable impurities, and its material is the particle of 0.05mm-2.5mm.
A kind of material of removing impurity in the inert gas of the present invention also can be the voluminous powder sintered body.
Also contain the Titanium element that percentage by weight is 1%-4% in a kind of zircaloy of removing the material of impurity in the inert gas of the present invention.
A kind of using method of removing the material of impurity in the inert gas at first will be removed the material of impurity in the inert gas, and in the rustless steel container of the Purge gas that has the gateway of packing into, vacuumizing and exhausting to vacuum is 10 -3Behind the Pa, charge into inert gas, 700 ℃ of-960 ℃ of temperature of intensification, be incubated 2-3 hour, carry out activation processing; The inert gas feeding that desire purifies is equipped with in the degasification container of material, carries out the gas purification of absorbing gaseous impurities under 400 ℃ of-960 ℃ of temperature, the control gas flow is 0.5m/h, and operating pressure is 0.3MPa-1.5MPa.Usually zirconium-base alloy and fluorocarbon gases impurity have the enough reaction time to take place under certain pressure and temperature, fluorocarbon gases impurity in the inert gas is absorbed, air-breathing reaction takes place, generate stable zirconium carbon compound and zirconium fluorine compounds, originally these compounds are created in the zirconium-base alloy particle surface, along with the carrying out of air-breathing reaction constantly spread to granule interior.Because this compound does not decompose under the temperature that air-breathing reaction takes place, remove the stable reaction of fluorocarbons in the inert gas such as xenon krypton and continue thereby make.
The material of impurity has added elements such as aluminium, hafnium, lanthanide rare, titanium in the removal inert gas of the present invention in zirconium-base alloy, these elements also can react with the impurity in the inert gas under certain condition, generate stable compound, and because the degasification performance of the alloy that these elements and zirconium form is more remarkable, improve the reaction speed of zirconium and gaseous impurity, removed the gaseous impurity of fluorocarbons.
The present invention is further illustrated below in conjunction with example.
Embodiment 1
The composition of inert gas purge material contains hafnium 2% for containing aluminium 11%, lanthanide rare 5%, nickel 2%, surplus were zirconium and unavoidable impurities, 720 ℃ of following activation processing 2.5 hours, the operating temperature of Purge gas process is 450 ℃, and operating pressure is 0.5MPa, gas flow 0.5m 3/ h is for purifying the active gaseous impurities content 35ppm in the gas of back, C in the gas 2F 6, CF 4Impurity content≤3ppm.
Embodiment 2
The composition of inert gas purge material contains hafnium 1.5% for containing aluminium 15%, lanthanide rare 3%, nickel 1%, surplus were zirconium and unavoidable impurities, 950 ℃ of following activation processing 2 hours, the operating temperature of Purge gas process is 600 ℃, and operating pressure is 1MPa, gas flow 5m 3/ h is for purifying the active gaseous impurities content 45ppm in the gas of back, C in the gas 2F 6, CF 4Impurity content≤3ppm.
Embodiment 3
The composition of inert gas purge material contains hafnium 2% for containing aluminium 12%, lanthanide rare 4%, 21%, titaniferous 4%, surplus were zirconium and unavoidable impurities, 800 ℃ of following activation processing 1.5 hours, the operating temperature of Purge gas process is 680 ℃, and operating pressure is 1.5MPa, gas flow 9m 3/ h is for purifying the active gaseous impurities content 47ppm in the gas of back, C in the gas 2F 6, CF 4Impurity content≤3ppm.
Embodiment 4
The composition of inert gas purge material contains hafnium 1% for containing aluminium 25%, lanthanide rare 0.5%, nickel 1%, surplus were zirconium and unavoidable impurities, 700 ℃ of following activation processing 3 hours, the operating temperature of Purge gas process is 720 ℃, and operating pressure is 1.5MPa, gas flow 7m 3/ h is for purifying the active gaseous impurities content 38ppm in the gas of back, C in the gas 2F 6, CF 4Impurity content≤3ppm.
Embodiment 5
The composition of inert gas purge material contains hafnium 1% for containing aluminium 10%, lanthanide rare 4%, nickel 2%, Ti content 1%, surplus were zirconium and unavoidable impurities, 880 ℃ of following activation processing 2.5 hours, the operating temperature of Purge gas process is 720 ℃, and operating pressure is 1.5MPa, gas flow 7m 3/ h is for purifying the active gaseous impurities content 36ppm in the gas of back, C in the gas 2F 6, CF 4Impurity content≤3ppm.
Embodiment 6
The composition of inert gas purge material contains hafnium 1% for containing aluminium 13%, lanthanide rare 3%, nickel 2%, Ti content 1%, surplus were zirconium and unavoidable impurities, 880 ℃ of following activation processing 2.5 hours, the operating temperature of Purge gas process is 470 ℃, and operating pressure is 1.5MPa, gas flow 7m 3/ h is for purifying the active gaseous impurities content 42ppm in the gas of back, C2F in the gas 6, CF 4Impurity content≤3ppm.
Embodiment 7
The composition of inert gas purge material contains hafnium 1% for containing aluminium 16%, lanthanide rare 0.5%, nickel 2%, Ti content 1%, surplus were zirconium and unavoidable impurities, 880 ℃ of following activation processing 2.5 hours, the operating temperature of Purge gas process is 700 ℃, and operating pressure is 1.0MPa, gas flow 6m 3/ h is for purifying the active gaseous impurities content 38ppm in the gas of back, C in the gas 2F 6, CF 4Impurity content≤3ppm.
Embodiment 8
The composition of inert gas purge material is for containing aluminium 20%, contain hafnium 1%, lanthanide rare 0.4%, nickel 2%, Ti content 1%, surplus is zirconium and unavoidable impurities, 880 ℃ of following activation processing 2.5 hours, the operating temperature of Purge gas process is 930 ℃, and operating pressure is 0.9MPa, gas flow 1.2m 3/ h is for purifying the active gaseous impurities content 38ppm in the gas of back, C in the gas 2F 6, CF 4Impurity content≤3ppm.
Embodiment 9
The composition of inert gas purge material contains hafnium 1% for containing aluminium 10%, lanthanide rare 5%, nickel 3%, Ti content 3%, surplus were zirconium and unavoidable impurities, 880 ℃ of following activation processing 2.5 hours, the operating temperature of Purge gas process is 520 ℃, and operating pressure is 1.5MPa, gas flow 0.6m 3/ h is for purifying the active gaseous impurities content 38ppm in the gas of back, C in the gas 2F 6, CF 4Impurity content≤3ppm.
Embodiment 10
The composition of inert gas purge material contains hafnium 1.5% for containing aluminium 13%, lanthanide rare 4%, nickel 2%, Ti content 2%, surplus were zirconium and unavoidable impurities, 880 ℃ of following activation processing 2.5 hours, the operating temperature of Purge gas process is 720 ℃, and operating pressure is 1.3MPa, gas flow 7m 3/ h is for purifying the active gaseous impurities content 48ppm in the gas of back, C in the gas 2F 6, CF 4Impurity content≤3ppm.
Embodiment 11
The composition of inert gas purge material contains hafnium 1% for containing aluminium 17%, lanthanide rare 2%, nickel 1%, Ti content 1%, surplus were zirconium and unavoidable impurities, 880 ℃ of following activation processing 2.5 hours, the operating temperature of Purge gas process is 720 ℃, and operating pressure is 1.5MPa, gas flow 10m 3/ h is for purifying the active gaseous impurities content 48ppm in the gas of back, C in the gas 2F 6, CF 4Impurity content≤3ppm.
Embodiment 12
The composition of inert gas purge material contains hafnium 1% for containing aluminium 19%, lanthanide rare 5%, nickel 1%, Ti content 4%, surplus were zirconium and unavoidable impurities, 880 ℃ of following activation processing 2.5 hours, the operating temperature of Purge gas process is 860 ℃, and operating pressure is 1.5MPa, gas flow 14m 3/ h is for purifying the active gaseous impurities content 41ppm in the gas of back, C in the gas 2F 6, CF 4Impurity content≤3ppm.

Claims (4)

1. material of removing impurity in the inert gas, it is characterized in that this material is a kind of zircaloy, the percentage by weight of this alloy consists of: contain aluminium 10%-25%, contain hafnium 1%-2%, lanthanide rare 0.4%-5%, nickel 1%-3%, surplus is zirconium and unavoidable impurities, its material is the particle of 0.05mm-2.5mm.
2. a kind of material of removing impurity in the inert gas according to claim 1 is characterized in that its material is the voluminous powder sintered body.
3. a kind of material of removing impurity in the inert gas according to claim 1 is characterized in that containing in its zircaloy the Titanium element that percentage by weight is 1%-4%.
4. the described a kind of using method of removing the material of impurity in the inert gas of claim 1 is characterized in that its use is:
The material that a. will be used for removing inert gas impurity is packed in the rustless steel container of the Purge gas that has the gateway, and vacuumizing and exhausting to vacuum is 10 -3Behind the Pa, charge into inert gas, 700 ℃ of-960 ℃ of temperature of intensification, be incubated 2-3 hour, will carry out activation processing;
B. the inert gas that desire is purified feeds and is equipped with in the degasification container of material, carries out the gas purification process of absorbing gaseous impurities under 400 ℃ of-960 ℃ of temperature, and the control gas flow is 0.5m 3/ h-10m 3/ h, operating pressure is 0.3MPa-1.5MPa.
CNB011451238A 2001-12-30 2001-12-30 Material for removing impurity in inert gas and its use method Expired - Fee Related CN1190262C (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1990380B (en) * 2005-12-30 2010-10-13 天津环煜电子材料科技有限公司 Technique for purifying and recovering argon gas by rare earth lanthanide series radical alloy degasser in single-crystal silicon preparation
CN101880796A (en) * 2010-07-15 2010-11-10 南京信息工程大学 Zirconium-nickel alloy and preparation method thereof
CN102100999A (en) * 2009-12-16 2011-06-22 贵阳铝镁设计研究院 Method for purifying inert gases and purifying device
CN101547857B (en) * 2006-12-01 2012-03-21 乔治洛德方法研究和开发液化空气有限公司 Xenon retrieval system and retrieval device
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
CN106512702A (en) * 2016-12-08 2017-03-22 天津工业大学 Online purification method for inert gases based on titanium metallic chemical properties

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5002230B2 (en) * 2006-10-05 2012-08-15 日本パイオニクス株式会社 Inert gas purification method

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1990380B (en) * 2005-12-30 2010-10-13 天津环煜电子材料科技有限公司 Technique for purifying and recovering argon gas by rare earth lanthanide series radical alloy degasser in single-crystal silicon preparation
CN101547857B (en) * 2006-12-01 2012-03-21 乔治洛德方法研究和开发液化空气有限公司 Xenon retrieval system and retrieval device
US8153091B2 (en) 2006-12-01 2012-04-10 L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Xenon retrieval system and retrieval device
CN102100999A (en) * 2009-12-16 2011-06-22 贵阳铝镁设计研究院 Method for purifying inert gases and purifying device
CN102100999B (en) * 2009-12-16 2013-05-15 贵阳铝镁设计研究院有限公司 Method for purifying inert gases and purifying device
CN101880796A (en) * 2010-07-15 2010-11-10 南京信息工程大学 Zirconium-nickel alloy and preparation method thereof
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
CN106512702A (en) * 2016-12-08 2017-03-22 天津工业大学 Online purification method for inert gases based on titanium metallic chemical properties

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