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EP0906635A1 - Pumping device by non-vaporisable getter and method for using this getter - Google Patents

Pumping device by non-vaporisable getter and method for using this getter

Info

Publication number
EP0906635A1
EP0906635A1 EP97929213A EP97929213A EP0906635A1 EP 0906635 A1 EP0906635 A1 EP 0906635A1 EP 97929213 A EP97929213 A EP 97929213A EP 97929213 A EP97929213 A EP 97929213A EP 0906635 A1 EP0906635 A1 EP 0906635A1
Authority
EP
European Patent Office
Prior art keywords
enclosure
getter
vacuum
evaporable getter
temperature
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.)
Granted
Application number
EP97929213A
Other languages
German (de)
French (fr)
Other versions
EP0906635B1 (en
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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Filing date
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/en
Application granted granted Critical
Publication of EP0906635B1 publication Critical patent/EP0906635B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

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

  • Non-evaporable getter pumping device and method for implementing this getter are described in detail below.
  • the present invention relates to improvements made to pumping by a non-evaporable getter (NEG) to create a very high vacuum in an enclosure defined by a metal wall capable of releasing gas on its surface.
  • NEG non-evaporable getter
  • 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 to the surface defining the enclosure.
  • the vacuum level obtained in one enclosure is therefore defined by the dynamic balance between the degassing at the surface defining the enclosure and the pumping speed of the pumps used. Obtaining a high vacuum implies both great cleanliness of the surface of the enclosure reducing the emission of gas and a high pumping speed. For vacuum systems of particle accelerators whose chambers are generally of small section, the pumps must be brought close to each other or else a continuous pumping must be implemented, in order to overcome the limitation of conductance.
  • this material is capable of producing chemically stable compounds by reaction with the gases present in a vacuum enclosure (in particular H 2 , 0 2 , CO, C0 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, that is to say free from any passivation layer formed during the exposure of the getter 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 therefrom.
  • the level of vacuum that can be obtained in the enclosure remains defined by the dynamic balance between the pumping speed (whatever the means used) and the degassing speed of the metallic surface of 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.
  • the object of the invention is therefore to propose an improved solution which makes it possible to solve this problem and which, because of the degassing rate occurring in the enclosure, significantly increases the efficiency of the pumping means used and leads to a improvement of several orders of magnitude of the vacuum level likely to be created in the enclosure.
  • a getter layer according to the invention does not occupy any sensitive space, and offers the advantage of providing a pumping effect under zero bulk, 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 which has become unnecessary.
  • the material used has certain characteristics isolated or combined in whole or in part.
  • the material must of course have a high adsorption capacity for the chemically reactive gases present in the enclosure despite the barrier effect provided by the thin layer.
  • the material must also have great power absorption and 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 an activation temperature as low as possible, compatible with the drying temperatures of the vacuum systems (approximately 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 approximately 20 ° C; in these conditions, in general the activation temperature must be at most equal to 400 ° C.
  • the material must have a high solubility, greater than 2%, for oxygen in order to allow the 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 concentration of 2% in the getter would be reached after approximately 10 cycles, without count the other gases pumped during the vacuum operation; thicker layers could be considered, but they would take longer to deposit and their adhesion could become less good.
  • titanium and / or zirconium and / or hafnium and / or vanadium and scandium which have a solubility limit, for oxygen, at ambient temperature, greater than 2% can constitute getter suitable for constituting a thin layer coating within the scope of the invention.
  • titanium, zirconium and hafnium have a solubility for oxygen close to 20%
  • vanadium and scandium have a high diffusivity for gases. It is of course also possible to retain, alone or in combination with at least one of the aforementioned bodies, any alloy comprising at least one of the bodies, so as to combine the effects obtained, or even to obtain new effects not directly resulting from the accumulation of individual effects.
  • 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 C0 2 of the order of 1 ls "1 per cm 2 of surface. It should be added as an additional advantage that the implementation of a getter in the form of a thin layer adhering to a metal substrate makes it play the role of thermal stabilizer capable of limiting the temperature. ⁇ ture in the thin layer.
  • This arrangement is very advantageous because it makes it possible to use, as a getter, materials with high pyrophoricity without any safety problems being posed because of the stabilizing effect conferred by the substrate with a high thermal capacity compared to the heat of combustion of the thin getter layer.
  • thermodynamically unstable materials which widens the field of choice of the optimum material as a getter. This possibility can be exploited in a simple manner by implementing a technique of simultaneous cathodic pulverization of several bodies, using a composite cathode which is discussed below.
  • the invention provides a method for implementing a non-evaporable getter in order to create a very high vacuum in an enclosure defined by a metal wall capable of releasing gas on its surface, which method includes the following steps: a) the enclosure is cleaned; the thin layer deposition device is introduced inside the enclosure; a relative vacuum is created in the enclosure; we perform a steaming the enclosure to remove as much of the water vapor as possible; then the getter is deposited in a thin layer on at least most of the surface of the wall defining the enclosure; b) the atmospheric pressure in the enclosure is restored; and the depositing device is extracted from the enclosure; c) the enclosure coated internally with the thin getter layer is assembled within the installation which it is to equip; we create a relative vacuum; steaming the installation at the desired temperature while maintaining the enclosure at a temperature below the activation temperature of the getter; d) stopping the steaming of the installation and simultaneously raising the temperature of the enclosure to the activation temperature of the getter which is maintained for a predetermined period (
  • the surface of the getter thin layer is clean and its thermal degassing or induced by bombardment of particles (ions, electrons, or synchrotron light) is greatly reduced.
  • a molecular pumping phenomenon appears due to the chemical reaction, on the surface of the getter layer, of the gases present in the enclosure.
  • a vacuum evaporation process To deposit the getter in a thin layer on the surface of the wall of the enclosure, it is certainly possible to use a vacuum evaporation process; However, such a process seems difficult to control effectively in order to constitute a uniform and homogeneous layer, in particular during the simultaneous deposition of several bodies, and it seems in practice more advantageous to have recourse to a sputtering process which allows much control. effective conditions for the formation of the thin layer.
  • a sputtering process makes it possible to deposit several materials simultaneously to form an alloy type getter combining materials having different optimal characteristics, the accumulation of which is sought, as indicated above.
  • a cathode is formed, intended to be placed centrally in the enclosure, which can be constituted by a twist of several (for example two or three) metallic wires of the respective materials of the alloy which are wish to train.
  • the use of a composite cathode thus constituted allows the simultaneous deposition of several metals and therefore artificially create an alloy of thermodynamically unstable materials which it would not be possible to obtain by other traditional routes.
  • 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 they are 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 particularly interesting field of application of the invention consists in obtaining and maintaining over a long period of time a high vacuum in the accelerators / accumulators of particles whose conditioning period by circula ⁇ tion of the particle beam would then be erased and in which the problems of vacuum instability would be eliminated.

Landscapes

  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (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)
  • Image-Pickup Tubes, Image-Amplification Tubes, And Storage Tubes (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Finger-Pressure Massage (AREA)
  • Thermal Insulation (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention discloses a pumping device by non-vaporisable getter to create a very high vacuum in a chamber defined by a metal wall capable of releasing gas at its surface, characterised in that it comprises a thin layer of non-vaporisable getter coated on at least almost the whole metal wall surface defining the chamber.

Description

Dispositif de pompage par getter non évaporable et procédé de mise en oeuyre de ce getter. Non-evaporable getter pumping device and method for implementing this getter.
La présente invention concerne des perfectionnements apportés au pompage par getter non évaporable (NEG) pour créer un vide très poussé dans une enceinte définie par une paroi métallique susceptible de relâcher du gaz à sa surface.The present invention relates to improvements made to pumping by a non-evaporable getter (NEG) to create a very high vacuum in an enclosure defined by a metal wall capable of releasing gas on its surface.
Dans un système métallique étuvable dans lequel doit être réalisé un vide très poussé (c'est-à-dire un vide d'au moins 10"10 Torr, voire d'un ordre de grandeur de 10"13 à 10"14 Torr), les parois métalliques de l'enceinte à vide consti¬ tuent une source inépuisable de gaz. L'hydrogène contenu dans le métal de construction (par exemple acier inoxydable, cuivre, alliage d'aluminium) diffuse librement dans l'épais- seur du métal et est relâché à la surface définissant l'enceinte. De même, lorsque les parois de la chambre à vide sont bombardées par des particules ( rayonnement de synchro- ton, électrons ou ions) -comme c'est la cas dans les accélérateurs de particules-, il en résulte l'expulsion aussi d'espèces moléculaires plus lourdes, telles que CO, C02, CH4, produites en surface après dissociation d'hydrocar¬ bures, carbures et oxydes.In a steamable metal system in which a very high vacuum must be produced (that is to say a vacuum of at least 10 "10 Torr, or even of an order of magnitude from 10 " 13 to 10 "14 Torr) , the metal walls of the vacuum enclosure constitute an inexhaustible source of gas. The hydrogen contained in the construction metal (for example stainless steel, copper, aluminum alloy) diffuses freely in the thickness of the metal and is released to the surface defining the enclosure. Similarly, when the walls of the vacuum chamber are bombarded with particles (synchrotron radiation, electrons or ions) - as is the case in accelerators of particles-, this also results in the expulsion of heavier molecular species, such as CO, C0 2 , CH 4 , produced on the surface after dissociation of hydrocarbons, carbides and oxides.
Le niveau de vide obtenu dans 1 ' enceinte est donc défini par l'équilibre dynamique entre le dégazage à la surface définissant l'enceinte et la vitesse de pompage des pompes utilisées. L'obtention d'un vide élevé implique à la fois une grande propreté de la surface de l'enceinte réduisant l'émission de gaz et une vitesse de pompage élevée. Pour les systèmes à vide des accélérateurs de particules dont les chambres sont généralement de petite section, les pompes doivent être rapprochées les unes des autres ou bien il faut mettre en oeuvre un pompage continu, afin de surmonter la limitation de conductance.The vacuum level obtained in one enclosure is therefore defined by the dynamic balance between the degassing at the surface defining the enclosure and the pumping speed of the pumps used. Obtaining a high vacuum implies both great cleanliness of the surface of the enclosure reducing the emission of gas and a high pumping speed. For vacuum systems of particle accelerators whose chambers are generally of small section, the pumps must be brought close to each other or else a continuous pumping must be implemented, in order to overcome the limitation of conductance.
Dans ces conditions, pour parvenir à obtenir un vide aussi poussé que possible, il est connu de compléter le vide produit par des pompes mécaniques en effectuant un pompage complémentaire à l'aide d'un getter disposé dans l'enceinte: ce matériau est capable de produire des composés chimique¬ ment stables par réaction avec les gaz présents dans une enceinte à vide (notamment H2, 02, CO, C02, N2) et cette réaction donne lieu à la disparition des espèces moléculai¬ res concernées, ce qui correspond à un effet de pompage.Under these conditions, in order to achieve as high a vacuum as possible, it is known to complete the vacuum produced by mechanical pumps by pumping complementary using a getter placed in the enclosure: this material is capable of producing chemically stable compounds by reaction with the gases present in a vacuum enclosure (in particular H 2 , 0 2 , CO, C0 2 , N 2 ) and this reaction gives rise to the disappearance of the molecular species concerned, which corresponds to a pumping effect.
Pour que la réaction chimique souhaitée puisse effectivement se produire, il est nécessaire que la surface du getter soit propre, c'est-à-dire exempte de toute couche de passivation formée lors de l'exposition du getter à l'air ambiant. Cette couche de passivation peut notamment être éliminée en diffusant les gaz de surface (02 principalement) à l'intérieur du getter par chauffage (processus d'activa- tion du getter qui est alors dénommé getter non évaporable: NEG). Les getters non évaporables présentent l'avantage de pouvoir être réalisés sous forme d'un ruban que l'on peut alors mettre en place tout le long de l'enceinte à vide de sorte qu'il en résulte un effet de pompage distribué.In order for the desired chemical reaction to actually occur, the surface of the getter must be clean, that is to say free from any passivation layer formed during the exposure of the getter 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 therefrom.
Toutefois, quel que soit le processus de pompage mis en oeuvre, et malgré l'efficacité du pompage réparti que permet d'effectuer la mise en oeuvre d'un getter non évaporable, le niveau de vide susceptible d'être obtenu dans l'enceinte reste défini par l'équilibre dynamique entre la vitesse de pompage (quels que soient les moyens mis en oeuvre) et la vitesse de dégazage de la surface métallique de l'enceinte (quelle qu'en soit la cause) ? autrement dit pour une vitesse de pompage donnée, le niveau de vide reste tributaire du taux de dégazage dans l'enceinte.However, whatever the pumping process implemented, and despite the efficiency of the distributed pumping that allows the implementation of a non-evaporable getter, the level of vacuum that can be obtained in the enclosure remains defined by the dynamic balance between the pumping speed (whatever the means used) and the degassing speed of the metallic surface of 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.
L'invention a donc pour but de proposer une solution perfectionnée qui permette de résoudre ce problème et qui, en raison du taux de dégazage se produisant dans l'enceinte, accroisse notablement l'efficacité des moyens de pompage mis en oeuvre et conduise à une amélioration de plusieurs ordres de grandeurs du niveau de vide susceptible d'être créé dans l'enceinte.The object of the invention is therefore to propose an improved solution which makes it possible to solve this problem and which, because of the degassing rate occurring in the enclosure, significantly increases the efficiency of the pumping means used and leads to a improvement of several orders of magnitude of the vacuum level likely to be created in the enclosure.
A ces fins, il est proposé conformément à l'inven- tion que au moins la quasi totalité de la surface de la paroi métallique définissant l'enceinte soit recouverte d'une couche mince de getter non évaporable déposée sous vide, notamment par pulvérisation cathodique. Cette couche de getter constitue un écran qui inhibe le dégazage du métal de la paroi de l'enceinte, sans en produire à son tour. En outre, dans les chambres des accélérateurs de particules, c'est cette couche qui subit les impacts des particules en mouvement et qui, formant écran, empêche la libération d'espèces moléculaires suscep¬ tible de polluer le vide dans l'enceinte. Il en résulte que, par ce moyen, on empêche, au moins dans une grande mesure, le dégazage, quelle qu'en soit la cause, dans l'enceinte. De plus, un getter mis en oeuvre sous la forme d'une telle couche conserve l'avantage d'un pompage réparti de façon uniforme et est moins susceptible qu'un dépôt par poudre pressée de relâcher des particules solides dont l'effet peut être néfaste pour certaines applications.For these purposes, it is proposed in accordance with the invention tion that at least almost the entire surface of the metal wall defining the enclosure is covered with a thin layer of non-evaporable getter deposited under vacuum, in particular by sputtering. This getter layer constitutes a screen which inhibits the degassing of the metal from the wall of the enclosure, without in turn producing it. In addition, in the particle accelerator chambers, it is this layer which is subjected to the impacts of moving particles and which, forming a screen, prevents the release of molecular species likely to pollute the vacuum in the enclosure. As a result, by this means, at least to a great extent, degassing, whatever the cause, is prevented in the enclosure. In addition, a getter implemented in the form of such a layer retains the advantage of uniformly distributed pumping and is less likely than a deposition by pressed powder to release solid particles whose effect can be harmful for certain applications.
Enfin, une couche de getter conforme à l'invention n'occupe aucun espace sensible, et offre l'avantage de procurer un effet de pompage sous un encombrement nul, ce qui permet sa mise en oeuvre même dans des cas où les contraintes géométriques interdiraient l'emploi d'un getter sous forme de ruban. De même, dans les machines à électrons, la conception de la chambre à vide pourrait être grandement simplifiée par l'élimination du canal latéral de pompage devenu inutile.Finally, a getter layer according to the invention does not occupy any sensitive space, and offers the advantage of providing a pumping effect under zero bulk, which allows its implementation even in cases where the geometric constraints would prohibit the use of a getter in the form of a ribbon. Similarly, in electron machines, the design of the vacuum chamber could be greatly simplified by eliminating the lateral pumping channel which has become unnecessary.
Pour que l'efficacité du getter en couche mince puisse conduire à l'effet de pompage optimum recherché, le matériau utilisé possède certaines caractéristiques isolées ou combinées en tout ou partie.So that the efficiency of the getter in a thin layer can lead to the optimum pumping effect sought, the material used has certain characteristics isolated or combined in whole or in part.
Le matériau doit bien entendu posséder un grand pouvoir d'adsorption pour les gaz chimiquement réactifs présents dans l'enceinte malgré l'effet de barrière procuré par la couche mince.The material must of course have a high adsorption capacity for the chemically reactive gases present in the enclosure despite the barrier effect provided by the thin layer.
Le matériau doit posséder également un grand pouvoir d'absorption et une grande diffusivité pour l'hydrogène, avec capacité à former une phase hydrure. Il doit, en outre, présenter une pression de dissociation de la phase hydrure inférieure à 10"13 Torr à environ 20°C. Le matériau doit également posséder une température d'activation aussi basse que possible, compatible avec les températures d'étuvage des systèmes à vide (environ 400°C pour les chambres en acier inoxydable, 200-250βC pour les chambres en cuivre et alliage d'aliminium) et compatible avec la stabilité du matériau à l'air, à environ 20°C ; dans ces conditions, d'une façon générale la température d'acti¬ vation doit être au plus égale à 400°C.The material must also have great power absorption and 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 an activation temperature as low as possible, compatible with the drying temperatures of the vacuum systems (approximately 400 ° C for stainless steel chambers, 200-250 β C for copper and aluminum alloy chambers) and compatible with the stability of the material in air, at approximately 20 ° C; in these conditions, in general the activation temperature must be at most equal to 400 ° C.
Le matériau doit enfin posséder une grande solubi¬ lité, supérieure à 2 %, pour l'oxygène afin de permettre l'absorption de la quantité d'oxygène pompée en surface lors d'un grand nombre de cycles d'activation et d'exposition à l'air. Par exemple, avec une couche de getter non évaporable de 1 μm d'épaisseur et une épaisseur de 20A d'oxyde formé en surface à chaque exposition, une concentration d'oxygène de 2 % dans le getter serait atteinte après environ 10 cycles, sans compter les autres gaz pompés pendant l'opération sous vide ; des couches plus épaisses pourraient être envisagées, mais elles seraient plus longues à déposer et leur adhésion pourrait devenir moins bonne. En définitive, le titane et/ou le zirconium et/ou le hafnium et/ou le vanadium et le scandium qui présentent une limite de solubilité,pour l'oxygène, à la température ambian¬ te, supérieure à 2 % peuvent constituer des getter non éva- porables appropriés pour constituer un revêtement en couche mince dans le cadre de l'invention. On notera que le titane, le zirconium et le hafnium ont une solubilité pour l'oxygène voisine de 20 %, tandis que le vanadium et le scandium présentent une grande diffusivité pour les gaz. On peut bien entendu retenir également, isolément ou en association avec au moins un des corps précités, tout alliage comprenant au moins un des corps, de manière à combiner les effets obtenus, voire à obtenir des effets nouveaux ne résultant pas directement du cumul des effets individuels.Finally, the material must have a high solubility, greater than 2%, for oxygen in order to allow the absorption of the quantity of oxygen pumped to the surface during a large number of activation and exposure cycles. to the air. For example, with a non-evaporable getter layer 1 μm thick and a thickness of 20 A of oxide formed on the surface at each exposure, an oxygen concentration of 2% in the getter would be reached after approximately 10 cycles, without count the other gases pumped during the vacuum operation; thicker layers could be considered, but they would take longer to deposit and their adhesion could become less good. Ultimately, titanium and / or zirconium and / or hafnium and / or vanadium and scandium which have a solubility limit, for oxygen, at ambient temperature, greater than 2% can constitute getter suitable for constituting a thin layer coating within the scope of the invention. It will be noted that titanium, zirconium and hafnium have a solubility for oxygen close to 20%, while vanadium and scandium have a high diffusivity for gases. It is of course also possible to retain, alone or in combination with at least one of the aforementioned bodies, any alloy comprising at least one of the bodies, so as to combine the effects obtained, or even to obtain new effects not directly resulting from the accumulation of individual effects.
A titre d'exemple, le titane est activable à 400°C, le zirconium à 300°C et l'alliage Ti 50 % - Zr 50 % à 250°C. Une activation à ces températures pendant deux heures réduit de quatre ordres de grandeur le taux de désorption induit par un bombardement d'électrons d'une énergie de 500 eV et produit des vitesses de pompage pour CO et C02 de l'ordre de 1 ls"1 par cm2 de surface. II faut ajouter comme avantage supplémentaire que la mise en oeuvre d'un getter sous forme d'une couche mince adhérant à un substrat métallique fait jouer à ce dernier le rôle de stabilisateur thermique apte à limiter la tempéra¬ ture dans la couche mince. Cette disposition est très avantageuse car elle permet d'utiliser, en tant que getter, des matériaux à pyrophoricite élevée sans qu'il se pose de problèmes de sécurité en raison de l'effet de stabilisation conféré par le substrat dont la capacité thermique est grande par rapport à la chaleur de combustion de la couche mince de getter.For example, 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 C0 2 of the order of 1 ls "1 per cm 2 of surface. It should be added as an additional advantage that the implementation of a getter in the form of a thin layer adhering to a metal substrate makes it play the role of thermal stabilizer capable of limiting the temperature. ¬ ture in the thin layer. This arrangement is very advantageous because it makes it possible to use, as a getter, materials with high pyrophoricity without any safety problems being posed because of the stabilizing effect conferred by the substrate with a high thermal capacity compared to the heat of combustion of the thin getter layer.
On peut enfin noter que l'utilisation d'un getter non évaporable sous forme de couche mince offre la possibi¬ lité de créer des matériaux thermodynamiquement instables, ce qui élargit le domaine du choix du matériau optimum en tant que getter. Cette possibilité peut être exploitée de façon simple en mettant en oeuvre une technique de pulvéri¬ sation cathodique simultanée de plusieurs corps, à l'aide d'une cathode composite dont il est question plus loin.Finally, it can be noted that the use of a non-evaporable getter in the form of a thin layer offers the possibility of creating thermodynamically unstable materials, which widens the field of choice of the optimum material as a getter. This possibility can be exploited in a simple manner by implementing a technique of simultaneous cathodic pulverization of several bodies, using a composite cathode which is discussed below.
Selon un second de ses aspects, l'invention propose un procédé pour la mise en oeuvre d'un getter non évaporable afin de créer un vide très poussé dans une enceinte définie par une paroi métallique susceptible de relâcher du gaz à sa surface, lequel procédé comprend les étapes qui suivent : a) on nettoie l'enceinte ; on introduit le dispositif de dépôt en couche mince à l'intérieur de l'enceinte ; on crée un vide relatif dans l'enceinte ; on effectue un étuvage de l'enceinte afin d'évacuer la plus grande partie possible de la vapeur d'eau ; puis on effectue le dépôt du getter en une couche mince sur au moins la plus grande partie de la surface de la paroi définissant 1 'enceinte ; b) on rétablit la pression atmosphérique dans l'enceinte ; et on extrait le dispositif de dépôt hors de l'enceinte; c) on assemble l'enceinte revêtue intérieurement de la couche mince de getter au sein de l'installation qu'elle doit équiper ; on crée un vide relatif ; on réalise un étuvage de l'installation à la température voulue tout en maintenant l'enceinte à une température inférieure à la température d'activation du getter ; d) on arrête 1 'étuvage de l'installation et simultanément on élève la température de l'enceinte jusqu'à la température d'activation du getter que l'on maintient pendant une durée prédéterminée (par exemple 1 à 2 heures ) ; et enfin on ramène la température de l'enceinte à la température ambiante. A la fin de cette procédure, la surface de la couche mince de getter est propre et son dégazage thermique ou induit par bombardement de particules (ions, électrons, ou lumière de synchrotron) est fortement réduit. En même temps apparaît un phénomène de pompage moléculaire dû à la réaction chimique, sur la surface de la couche de getter, des gaz présents dans l'enceinte.According to a second of its aspects, the invention provides a method for implementing a non-evaporable getter in order to create a very high vacuum in an enclosure defined by a metal wall capable of releasing gas on its surface, which method includes the following steps: a) the enclosure is cleaned; the thin layer deposition device is introduced inside the enclosure; a relative vacuum is created in the enclosure; we perform a steaming the enclosure to remove as much of the water vapor as possible; then the getter is deposited in a thin layer on at least most of the surface of the wall defining the enclosure; b) the atmospheric pressure in the enclosure is restored; and the depositing device is extracted from the enclosure; c) the enclosure coated internally with the thin getter layer is assembled within the installation which it is to equip; we create a relative vacuum; steaming the installation at the desired temperature while maintaining the enclosure at a temperature below the activation temperature of the getter; d) stopping the steaming of the installation and simultaneously raising the temperature of the enclosure to the activation temperature of the getter which is maintained for a predetermined period (for example 1 to 2 hours); and finally the temperature of the enclosure is brought down to ambient temperature. At the end of this procedure, the surface of the getter thin layer is clean and its thermal degassing or induced by bombardment of particles (ions, electrons, or synchrotron light) is greatly reduced. At the same time, a molecular pumping phenomenon appears due to the chemical reaction, on the surface of the getter layer, of the gases present in the enclosure.
Pour effectuer le dépôt du getter en couche mince sur la surface de la paroi de l'enceinte, on peut certes avoir recours à un processus d'évaporation sous vide ; toutefois un tel processus semble difficile à contrôler de façon efficace pour constituer une couche uniforme et homogène en particulier lors du dépôt simultané de plusieurs corps, et il semble en pratique plus avantageux d'avoir recours à un processus de pulvérisation cathodique qui autorise un contrôle beaucoup efficace des conditions de formation de la couche mince. De plus, un processus de pulvérisation cathodique permet de déposer simultanément plusieurs matériaux pour former un getter de type alliage combinant des matériaux ayant des caractéristiques optimales différentes dont on recherche le cumul, comme indiqué plus haut. Pour ce faire, on constitue une cathode, destinée à être disposée centrale- ment dans l'enceinte, qui peut être constituée par une torsade de plusieurs ( par exemple deux ou trois ) fils métalliques des matériaux respectifs de l'alliage que l'on souhaite former. Le recours à une cathode composite ainsi constituée permet le dépôt simultané de plusieurs métaux et donc de créer artificiellement un alliage de matériaux thermodynamiquement instables qu'il ne serait pas possible d'obtenir par d'autres voies traditionnelles. Les moyens proposés par l'invention offrent la possibilité inégalée de produire des vides poussés de 10"10 à 10~14 Torr pour des applications de laboratoire, pour l'isolation thermique et/ou phonique et pour les systèmes d'analyse de surface, surtout lorsqu'ils sont utilisés pour des matériaux réactifs. Toutefois, il faut noter que la mise en oeuvre de 1 ' invention dans des systèmes à vide souvent exposés à 1 'atmosphère ou opérant sous des vides peu poussés conduirait très rapidement à la saturation de la surface du getter en couche mince et que les avantages mentionnés plus haut ne pourraient pas être atteints.To deposit the getter in a thin layer on the surface of the wall of the enclosure, it is certainly possible to use a vacuum evaporation process; However, such a process seems difficult to control effectively in order to constitute a uniform and homogeneous layer, in particular during the simultaneous deposition of several bodies, and it seems in practice more advantageous to have recourse to a sputtering process which allows much control. effective conditions for the formation of the thin layer. In addition, a sputtering process makes it possible to deposit several materials simultaneously to form an alloy type getter combining materials having different optimal characteristics, the accumulation of which is sought, as indicated above. To do this, a cathode is formed, intended to be placed centrally in the enclosure, which can be constituted by a twist of several (for example two or three) metallic wires of the respective materials of the alloy which are wish to train. The use of a composite cathode thus constituted allows the simultaneous deposition of several metals and therefore artificially create an alloy of thermodynamically unstable materials which it would not be possible to obtain by other traditional routes. 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 they are used for reactive materials. However, it should be noted that 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.
Plus spécifiquement, un domaine d'application particulièrement intéressant de l'invention est constitué par l'obtention et l'entretien sur une longue durée de temps d'un vide poussé dans les accélérateurs/accumulateurs de particules dont la période de conditionnement par circula¬ tion de faisceau de particules serait alors effacée et dans lesquels les problèmes d'instabilité du vide seraient éliminés. More specifically, a particularly interesting field of application of the invention consists in obtaining and maintaining over a long period of time a high vacuum in the accelerators / accumulators of particles whose conditioning period by circula¬ tion of the particle beam would then be erased and in which the problems of vacuum instability would be eliminated.

Claims

REVENDICATIONS
1. Dispositif de pompage par getter non évaporable pour créer un vide très poussé dans une enceinte définie par une paroi métallique susceptible de relâcher du gaz à sa surface, caractérisé en ce qu'au moins la quasi totalité de la surface de la paroi métallique définissant l'enceinte est recouverte d'une couche mince de getter non évaporable déposée sous vide, notamment par pulvérisation cathodique. 1. Non-evaporable getter pumping device to create a very high vacuum in an enclosure defined by a metal wall capable of releasing gas on its surface, characterized in that at least almost the entire surface of the metal wall defining the enclosure is covered with a thin layer of non-evaporable getter deposited under vacuum, in particular by sputtering.
2. Dispositif de pompage selon la revendication 1, caractérisé en ce que le getter non évaporable possède :2. Pumping device according to claim 1, characterized in that the non-evaporable getter has:
- un grand pouvoir d'adsorption pour les gaz présents dans l'enceinte, et/ou- a high adsorption capacity for the gases present in the enclosure, and / or
- une grande solubilité pour l'oxygène d'au moins 2 %, et/ou - un grand pouvoir d'absorption et une grande diffusivité pour l'hydrogène, et/ou- a high solubility for oxygen of at least 2%, and / or - a high absorption power and a high diffusivity for hydrogen, and / or
- une capacité à former une phase hydrure, et/ou- an ability to form a hydride phase, and / or
- une pression de dissociation de la phase hydrure qui est inférieure à 10"13 Torr à environ 20°C, et/ou - une température d'activation au plus égale à 400°C et aussi basse que possible en compatibilité avec sa stabi¬ lité à l'air à environ 20°C.- a dissociation pressure of the hydride phase which is less than 10 "13 Torr at about 20 ° C, and / or - an activation temperature at most equal to 400 ° C and as low as possible in compatibility with its stabilization lity in air at about 20 ° C.
3. Dispositif de pompage selon la revendication 1 ou 2, caractérisé en ce que le getter non évaporable est choisi parmi le titane et/ou le zirconium et/ou le hafnium et/ou le vanadium et/ou le scandium et/ou un alliage comprenant au moins un de ces derniers.3. Pumping device according to claim 1 or 2, characterized in that the non-evaporable getter is chosen from titanium and / or zirconium and / or hafnium and / or vanadium and / or scandium and / or an alloy comprising at least one of these.
4. Procédé pour la mise en oeuvre d'un getter non évaporable afin de créer un vide très poussé dans une enceinte définie par une paroi métallique susceptible de relâcher du gaz à sa surface, caractérisé par la succession des étapes qui suivent : a) on effectue un dépôt d'une couche mince de getter non évaporable sur au moins la plus grande partie de la surface de la paroi de l'enceinte, b) on assemble l'enceinte avec un système à vide, on fait le vide à l'aide du système à vide, on effectue un étuvage du système à vide à une température donnée tout en maintenant l'enceinte à une température inférieure à la température d'activation du getter non évaporable, c) on arrête l'étuvage du système à vide, et simultanément on élève la température de l'enceinte jusqu'à la tempéra¬ ture d'activation, on maintient cette température pendant une durée prédéterminée appropriée pour rendre propre la couche de getter non évaporable, puis on abaisse la température jusqu'à la température ambiante.4. Method for implementing a non-evaporable getter in order to create a very high vacuum in an enclosure defined by a metal wall capable of releasing gas on its surface, characterized by the succession of the following steps: a) deposits a thin layer of non-evaporable getter on at least most of the surface of the wall of the enclosure, b) the enclosure is assembled with a vacuum system, the vacuum using the vacuum system, steaming of the vacuum system is carried out at a given temperature while maintaining the enclosure at a temperature below the activation temperature of the non-evaporable getter, c) stopping the steaming of the vacuum system, and simultaneously raising the temperature of the enclosure to the activation temperature, maintaining this temperature for a predetermined period suitable for making the getter layer non-evaporable clean, then lowering the temperature up to room temperature.
5. Procédé selon la revendication 4, caractérisé en ce qu'à l'étape a/, le dépôt de la couche de getter non évaporable est effectué par pulvérisation cathodique.5. Method according to claim 4, characterized in that in step a /, the deposition of the non-evaporable getter layer is carried out by sputtering.
6. Procédé selon la revendication 5 pour déposer une couche de getter non évaporable constitué par un alliage de plusieurs matériaux, caractérisé en ce qu'on utilise une cathode, disposée centralement dans l'enceinte, qui peut être constituée par plusieurs fils des matériaux respectifs de l'alliage torsadés les uns autour des autres. 6. Method according to claim 5 for depositing a non-evaporable getter layer consisting of an alloy of several materials, characterized in that a cathode is used, placed centrally in the enclosure, which can be constituted by several wires of the respective materials. of the alloy twisted around each other.
EP97929213A 1996-06-19 1997-06-18 Method for using a non-vaporisable getter Expired - Lifetime EP0906635B1 (en)

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FR9607625 1996-06-19
FR9607625A FR2750248B1 (en) 1996-06-19 1996-06-19 NON-EVAPORABLE GETTER PUMPING DEVICE AND METHOD FOR IMPLEMENTING THE GETTER
PCT/EP1997/003180 WO1997049109A1 (en) 1996-06-19 1997-06-18 Pumping device by non-vaporisable getter and method for using this getter

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EP0906635A1 true EP0906635A1 (en) 1999-04-07
EP0906635B1 EP0906635B1 (en) 2003-03-05

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DE (1) DE69719507T2 (en)
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RU2193254C2 (en) 2002-11-20
EP0906635B1 (en) 2003-03-05
DK0906635T3 (en) 2003-06-23
CA2258118C (en) 2010-08-17
AU3340497A (en) 1998-01-07
CA2258118A1 (en) 1997-12-24
FR2750248B1 (en) 1998-08-28
WO1997049109A1 (en) 1997-12-24
NO317454B1 (en) 2004-11-01
JP4620187B2 (en) 2011-01-26
ES2193382T3 (en) 2003-11-01
JP2001503830A (en) 2001-03-21
US6468043B1 (en) 2002-10-22
FR2750248A1 (en) 1997-12-26
ATE233946T1 (en) 2003-03-15
DE69719507T2 (en) 2004-02-19
NO985927L (en) 1998-12-17
PT906635E (en) 2003-07-31
NO985927D0 (en) 1998-12-17
DE69719507D1 (en) 2003-04-10

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