EP0906635B1 - Verfahren zur anwendung eines nicht verdampfbaren getters - Google Patents

Verfahren zur anwendung eines nicht verdampfbaren getters Download PDF

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Publication number
EP0906635B1
EP0906635B1 EP97929213A EP97929213A EP0906635B1 EP 0906635 B1 EP0906635 B1 EP 0906635B1 EP 97929213 A EP97929213 A EP 97929213A EP 97929213 A EP97929213 A EP 97929213A EP 0906635 B1 EP0906635 B1 EP 0906635B1
Authority
EP
European Patent Office
Prior art keywords
getter
temperature
vacuum
chamber
enclosure
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP97929213A
Other languages
English (en)
French (fr)
Other versions
EP0906635A1 (de
Inventor
Cristoforo Benvenuti
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
ORGANISATION EUROPEENNE POUR LA RECHERCHE NUCLEAIRE (CERN)
Original Assignee
ORGANISATION EUROPEENNE POUR LA RECHERCHE NUCLEAIRE (CERN)
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Publication date
Application filed by ORGANISATION EUROPEENNE POUR LA RECHERCHE NUCLEAIRE (CERN) filed Critical ORGANISATION EUROPEENNE POUR LA RECHERCHE NUCLEAIRE (CERN)
Publication of EP0906635A1 publication Critical patent/EP0906635A1/de
Application granted granted Critical
Publication of EP0906635B1 publication Critical patent/EP0906635B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J7/00—Details not provided for in the preceding groups and common to two or more basic types of discharge tubes or lamps
    • H01J7/14—Means for obtaining or maintaining the desired pressure within the vessel
    • H01J7/18—Means for absorbing or adsorbing gas, e.g. by gettering
    • H01J7/183—Composition or manufacture of getters
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J7/00—Details not provided for in the preceding groups and common to two or more basic types of discharge tubes or lamps
    • H01J7/14—Means for obtaining or maintaining the desired pressure within the vessel
    • H01J7/18—Means for absorbing or adsorbing gas, e.g. by gettering
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
    • H05H7/00—Details of devices of the types covered by groups H05H9/00, H05H11/00, H05H13/00
    • H05H7/14—Vacuum chambers

Definitions

  • the present invention relates to improvements brought in the field of non evaporable getter pumping (NEG) for create a very deep vacuum in an enclosure defined by a metal wall likely to release gas at its surface, said getter being deposited on at least the largest part from the surface of the enclosure wall.
  • NOG non evaporable getter pumping
  • the metal walls of the vacuum enclosure constitute an inexhaustible source of gas.
  • the hydrogen contained in the construction metal diffuses freely in the thickness of the metal and is released on the surface defining the enclosure.
  • the vacuum level obtained in the enclosure is therefore defined by the dynamic balance between degassing at surface defining the enclosure and the pumping speed of pumps used. Obtaining a high vacuum implies times a great cleanliness of the surface of the enclosure reducing gas emission and pumping speed high. For vacuum systems of accelerators particles whose chambers are usually small section, the pumps must be close to each other others or else a continuous pumping must be implemented, in order to overcome the conductance limitation.
  • this material is capable to produce chemically stable compounds by reaction with the gases present in a vacuum enclosure (in particular H 2 , O 2 , CO, CO 2 , N 2 ) and this reaction gives rise to the disappearance of the molecular species concerned, which corresponds to a pumping effect.
  • the surface of the getter must be clean, i.e. free from any passivation layer formed when the getter is exposed to ambient air.
  • This passivation layer can in particular be eliminated by diffusing the surface gases (mainly O 2 ) inside the getter by heating (activation process of the getter which is then called non-evaporable getter: NEG).
  • the non-evaporable getters have the advantage of being able to be produced in the form of a ribbon which can then be put in place all along the vacuum enclosure so that a distributed pumping effect results.
  • the vacuum level likely to be obtained in the enclosure remains defined by the dynamic balance between the pumping speed (whatever the means used work) and the degassing speed of the metal surface the enclosure (whatever the cause); in other words for a given pumping speed, the vacuum level remains dependent on the degassing rate in the enclosure.
  • Deposits on the walls of a vacuum enclosure have already been proposed in the past to improve the pressure of a vacuum system, for example as described in document DE-A-38 14 389.
  • the deposition of a boron and carbon layer obtained by radiofrequency plasma from a mixture of borane and of hydrocarbons, is proposed mainly to reduce the partial pressure of water vapor in the enclosure.
  • the object of the invention is therefore to propose a solution which solves this problem and which, due to the degassing rate occurring in the enclosure, significantly increases the efficiency of the pumping means used implement and lead to an improvement of several orders of magnitudes of the vacuum level likely to be created in the enclosure.
  • the non-evaporable getter layer forms a screen which inhibits the degassing of the metal from the wall of the enclosure, without produce in turn.
  • this layer is subjected to the impacts of moving particles and which, forming screen, prevents release of susceptible molecular species to pollute the vacuum in the enclosure. It follows that, by this means we prevent, at least to a great extent, degassing, whatever the cause, in the enclosure.
  • a getter implemented in the form of a such a layer retains the advantage of a distributed pumping of uniformly and. is less likely than a deposit by powder pressed to release solid particles including the effect may be harmful for certain applications.
  • a getter layer according to the invention does not occupy any sensitive space, and offers the advantage of provide a pumping effect under zero bulk, this which allows its implementation even in cases where the geometric constraints would prohibit the use of a getter in the form of a ribbon.
  • the design of the vacuum chamber could be greatly simplified by eliminating the lateral pumping channel become useless.
  • the material used has certain isolated characteristics or combined in whole or in part.
  • the material must of course have a large adsorption capacity for chemically reactive gases present in the enclosure despite the barrier effect provided by the thin layer.
  • the material must also have a high absorption power and a high diffusivity for hydrogen, with the capacity to form a hydride phase. It must, moreover, have a dissociation pressure of the hydride phase of less than 10 -13 Torr at approximately 20 ° C.
  • the material must also have a temperature as low as possible, compatible with steaming temperatures of vacuum systems (about 400 ° C for stainless steel chambers, 200-250 ° C for copper and aluminum alloy chambers) and compatible with the stability of the material in air, at about 20 ° C; in these conditions, generally the activation temperature must not be more than 400 ° C.
  • the material must finally have a high solubility, greater than 2%, for oxygen to allow absorption of the quantity of oxygen pumped to the surface during a large number of activation and exposure cycles to the air.
  • a high solubility greater than 2%
  • oxygen to allow absorption of the quantity of oxygen pumped to the surface during a large number of activation and exposure cycles to the air.
  • titanium and / or zirconium and / or hafnium and / or vanadium and scandium which have a solubility limit, for oxygen, at room temperature, greater than 2% may constitute non-evaporable getter suitable for forming a layered coating thin in the context of the invention.
  • titanium, zirconium and hafnium have a solubility for oxygen close to 20%, while vanadium and scandium have great diffusivity for gases.
  • titanium can be activated at 400 ° C, zirconium at 300 ° C and the alloy Ti 50% - Zr 50% at 250 ° C. Activation at these temperatures for two hours reduces the desorption rate induced by electron bombardment with an energy of 500 eV by four orders of magnitude and produces pumping speeds for CO and CO 2 of the order of 1 ls -1 per cm 2 of surface.
  • a getter in the form of a thin layer adhering to a metallic substrate makes it play the role of thermal stabilizer, able to limit the temperature in the thin layer.
  • This provision is very advantageous because it makes it possible to use, as a getter, materials with high pyrophoricity without any security issues due to the stabilizing effect conferred by the substrate whose thermal capacity is large compared to the heat of combustion of the layer thin getter.
  • a sputtering process allows multiple materials to be deposited simultaneously for form an alloy type getter combining materials having different optimal characteristics which one look for the cumulation, as indicated above.
  • a cathode is formed, intended to be disposed centrally in the enclosure, which can be constituted by a twist of several (for example two or three) wires metallic materials of the respective alloy which wish to train.
  • the use of a composite cathode as well constituted allows the simultaneous deposition of several metals and so to artificially create an alloy of materials thermodynamically unstable that it would not be possible to get by other traditional ways.
  • the means proposed by the invention offer the unequaled possibility of producing high voids from 10 -10 to 10 -14 Torr for laboratory applications, for thermal and / or phonic insulation and for surface analysis systems, especially when used for reactive materials.
  • the implementation of the invention in vacuum systems often exposed to the atmosphere or operating under low vacuum levels would very quickly lead to saturation of the surface of the getter in a thin layer and that the advantages mentioned above could not be achieved.
  • a field of application particularly interesting of the invention is constituted by obtaining and maintaining over a long period of time of a high vacuum in the accelerators / accumulators of particles whose conditioning period by circulation of particle beam would then be erased and in which vacuum instability problems would be eliminated.

Landscapes

  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Compressors, Vaccum Pumps And Other Relevant Systems (AREA)
  • Vessels, Lead-In Wires, Accessory Apparatuses For Cathode-Ray Tubes (AREA)
  • Common Detailed Techniques For Electron Tubes Or Discharge Tubes (AREA)
  • Fats And Perfumes (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Image-Pickup Tubes, Image-Amplification Tubes, And Storage Tubes (AREA)
  • Physical Vapour Deposition (AREA)
  • Finger-Pressure Massage (AREA)
  • Thermal Insulation (AREA)

Claims (3)

  1. Verfahren zur Anwendung eines nicht verdampfbaren Getters, um durch Getterwirkung in einem Raum einen sehr hohen Unterdruck zu erzeugen, der durch eine Metallwand begrenzt ist, die dazu ausgelegt ist, auf ihrer Oberfläche Gas frei zu geben, wobei der Getter auf zumindest dem größten Teil der Oberfläche der Wand des Raums abgeschieden ist, gekennzeichnet durch die Abfolge folgender Schritte:
    a) durch Kathodenzerstäubung wird auf zumindest dem größten Teil der Oberfläche der Wand des Raums die Abscheidung einer dünnen Getterschicht bewirkt,
    b) der Raum wird mit einem Unterdrucksystem erstellt, mit Hilfe des Unterdrucksystems wird der Unterdruck erzeugt, eine Heiztrocknung des Unterdrucksystems auf eine vorgegebene Temperatur wird bewirkt, während der Raum auf einer niedrigeren Temperatur als der Aktivierungstemperatur des nicht verdampfbaren Getters gehalten wird,
    c) die Heiztrocknung des Unterdrucksystems wird gestoppt und gleichzeitig wird die Temperatur des Raums bis auf die Aktivierungstemperatur erhöht, diese Temperatur wird während einer vorbestimmten Zeitdauer aufrechterhalten, die dazu geeignet ist, die Getterschicht nicht verdampfbar zu machen, woraufhin die Temperatur bis auf die Umgebungstemperatur absinken gelassen wird.
  2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass der nicht verdampfbare Getter aus Titan und/oder Zirkon und/oder Hafnium und/oder Vanadium und/oder Skandium und/oder einer Legierung ausgewählt ist, welche zumindest eines dieser Elemente enthält.
  3. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass zum Abscheiden einer nicht verdampfbaren Getterschicht, die aus einer Legierung von mehreren Materialien gebildet ist, eine Kathode verwendet wird, die im Zentrum des Raums angeordnet ist und die durch mehrere Drähte aus Legierungsmaterialien gebildet ist, die um einander verdreht bzw. verdrillt sind.
EP97929213A 1996-06-19 1997-06-18 Verfahren zur anwendung eines nicht verdampfbaren getters Expired - Lifetime EP0906635B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR9607625A FR2750248B1 (fr) 1996-06-19 1996-06-19 Dispositif de pompage par getter non evaporable et procede de mise en oeuvre de ce getter
FR9607625 1996-06-19
PCT/EP1997/003180 WO1997049109A1 (fr) 1996-06-19 1997-06-18 Dispositif de pompage par getter non evaporable et procede de mise en oeuvre de ce getter

Publications (2)

Publication Number Publication Date
EP0906635A1 EP0906635A1 (de) 1999-04-07
EP0906635B1 true EP0906635B1 (de) 2003-03-05

Family

ID=9493210

Family Applications (1)

Application Number Title Priority Date Filing Date
EP97929213A Expired - Lifetime EP0906635B1 (de) 1996-06-19 1997-06-18 Verfahren zur anwendung eines nicht verdampfbaren getters

Country Status (14)

Country Link
US (1) US6468043B1 (de)
EP (1) EP0906635B1 (de)
JP (1) JP4620187B2 (de)
AT (1) ATE233946T1 (de)
AU (1) AU3340497A (de)
CA (1) CA2258118C (de)
DE (1) DE69719507T2 (de)
DK (1) DK0906635T3 (de)
ES (1) ES2193382T3 (de)
FR (1) FR2750248B1 (de)
NO (1) NO317454B1 (de)
PT (1) PT906635E (de)
RU (1) RU2193254C2 (de)
WO (1) WO1997049109A1 (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2663813C2 (ru) * 2014-06-26 2018-08-10 Саес Геттерс С.П.А. Геттерная насосная система

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IT1312248B1 (it) * 1999-04-12 2002-04-09 Getters Spa Metodo per aumentare la produttivita' di processi di deposizione distrati sottili su un substrato e dispositivi getter per la
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IT1319141B1 (it) * 2000-11-28 2003-09-23 Getters Spa Unita' di accelerazione e focalizzazione, a vuoto migliorato, diimpiantatori ionici per la produzione di dispositivi a semiconduttore
ITMI20012389A1 (it) 2001-11-12 2003-05-12 Getters Spa Catodo cavo con getter integrato per lampade a scarica e metodi per la sua realizzazione
DE10209423A1 (de) * 2002-03-05 2003-09-18 Schwerionenforsch Gmbh Beschichtung aus einer Gettermetall-Legierung sowie Anordnung und Verfahren zur Herstellung derselben
ITMI20031178A1 (it) * 2003-06-11 2004-12-12 Getters Spa Depositi multistrato getter non evaporabili ottenuti per
DE602004008116T2 (de) 2004-01-22 2008-04-24 European Organisation For Nuclear Research Cern Evakuierbarer flachplattensonnenkollektor
US7888891B2 (en) * 2004-03-29 2011-02-15 National Cerebral And Cardiovascular Center Particle beam accelerator
RU2269838C1 (ru) * 2004-12-28 2006-02-10 Общество с ограниченной ответственностью "Ядерные технологии" Способ удаления активных газов и их смесей из замкнутого объема
GB0523838D0 (en) * 2005-11-23 2006-01-04 Oxford Instr Analytical Ltd X-Ray detector and method
ITMI20070301A1 (it) * 2007-02-16 2008-08-17 Getters Spa Supporti comprendenti materiali getter e sorgenti di metalli alcalini o alcalino-terrosi per sistemi di termoregolazione basati su effetto tunnel
EP1983548A1 (de) * 2007-04-20 2008-10-22 ICT Integrated Circuit Testing Gesellschaft für Halbleiterprüftechnik mbH Emitterkammer, Ladungsträgerteilchenstrahlvorrichtung und Bedienungsverfahren
EP2071188A1 (de) 2007-12-10 2009-06-17 VARIAN S.p.A. Vorrichtung zur Abscheidung von nicht-evaporierbaren Gettern (NEGs) und Abscheidungsverfahren mit einer solchen Vorrichtung
AU2008357548A1 (en) * 2008-06-11 2009-12-17 European Organization For Nuclear Research Cern High efficiency evacuated solar panel
CN102691640B (zh) * 2012-05-29 2015-12-02 储琦 一种抽气系统及工艺
RU2513563C2 (ru) * 2012-08-17 2014-04-20 Федеральное государственное унитарное предприятие "Научно-производственное предприятие "Исток" (ФГУП "НПП "Исток") Спеченный неиспаряющийся геттер
DE102016123146A1 (de) * 2016-06-03 2017-12-07 Movatec Gmbh Vakuumgerät und Verfahren zur Beschichtung von Bauteilen
JP6916537B2 (ja) * 2016-11-28 2021-08-11 大学共同利用機関法人 高エネルギー加速器研究機構 非蒸発型ゲッタコーティング部品、容器、製法、装置
FR3072788B1 (fr) 2017-10-24 2020-05-29 Commissariat A L'energie Atomique Et Aux Energies Alternatives Source de rayonnement infrarouge modulable
JP7837011B2 (ja) 2021-05-20 2026-03-30 大学共同利用機関法人 高エネルギー加速器研究機構 非蒸発型ゲッタコーティング装置、非蒸発型ゲッタコーティング容器・配管の製造方法、非蒸発型ゲッタコーティング容器・配管
FR3128307A1 (fr) 2021-10-14 2023-04-21 Safran Electronics & Defense Getter non evaporable activable a faible temperature, dispositif de pompage et enceinte contenant un tel getter
CN116575005B (zh) * 2023-05-10 2024-01-16 中国科学院近代物理研究所 一种TiZrCo真空吸气剂薄膜及其制备方法与应用

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2663813C2 (ru) * 2014-06-26 2018-08-10 Саес Геттерс С.П.А. Геттерная насосная система

Also Published As

Publication number Publication date
DE69719507D1 (de) 2003-04-10
CA2258118A1 (fr) 1997-12-24
ES2193382T3 (es) 2003-11-01
JP4620187B2 (ja) 2011-01-26
PT906635E (pt) 2003-07-31
RU2193254C2 (ru) 2002-11-20
DK0906635T3 (da) 2003-06-23
NO985927D0 (no) 1998-12-17
ATE233946T1 (de) 2003-03-15
US6468043B1 (en) 2002-10-22
EP0906635A1 (de) 1999-04-07
DE69719507T2 (de) 2004-02-19
FR2750248A1 (fr) 1997-12-26
FR2750248B1 (fr) 1998-08-28
JP2001503830A (ja) 2001-03-21
WO1997049109A1 (fr) 1997-12-24
AU3340497A (en) 1998-01-07
NO317454B1 (no) 2004-11-01
NO985927L (no) 1998-12-17
CA2258118C (fr) 2010-08-17

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