EP0906635B1 - Method for using a non-vaporisable getter - Google Patents

Method for using a non-vaporisable getter 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
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Prior art keywords
getter
temperature
vacuum
chamber
enclosure
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German (de)
French (fr)
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EP0906635A1 (en
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Cristoforo Benvenuti
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ORGANISATION EUROPEENNE POUR LA RECHERCHE NUCLEAIRE (CERN)
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    • 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.

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  • 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)
  • Fats And Perfumes (AREA)
  • Common Detailed Techniques For Electron Tubes Or Discharge Tubes (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-vaporizable getter to create a very high vacuum in a chamber defined by a metal wall capable of releasing gas at its surface, characterized in that it comprises a thin layer of non-vaporizable getter coated on at least almost the whole metal wall surface defining the chamber.

Description

La présente invention concerne des perfectionnements apportés dans le domaine du 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, ledit getter étant déposé sur au moins la plus grande part de la surface de la paroi de l'enceinte.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.

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 (1 Torr = 1.333 mbar), voire d'un ordre de grandeur de 10-13 à 10-14 Torr), les parois métalliques de l'enceinte à vide constituent 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'épaisseur 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 synchroton, 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, CO2, CH4, produites en surface après dissociation d'hydrocarbures, carbures et oxydes.In a steamable metal system in which a very high vacuum must be produced (i.e. a vacuum of at least 10 -10 Torr (1 Torr = 1.333 mbar), or even of an order of magnitude of 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 on the surface defining the enclosure. Likewise, when the walls of the vacuum chamber are bombarded by particles (synchrotron radiation, electrons or ions) - as is the case in particle accelerators -, this also results in the expulsion of molecular species heavier, such as CO, CO 2 , CH 4 , produced on the surface after dissociation of hydrocarbons, carbides and oxides.

Le niveau de vide obtenu dans l'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 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.

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 chimiquement stables par réaction avec les gaz présents dans une enceinte à vide (notamment H2, O2, CO, CO2, N2) et cette réaction donne lieu à la disparition des espèces moléculaires 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 performing additional pumping using a getter placed in the enclosure: 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.

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 (O2 principalement) à l'intérieur du getter par chauffage (processus d'activation 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 take place, 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.

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, regardless of the pumping process and despite the efficiency of distributed pumping, allows the implementation of a non getter evaporable, 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.

Des dépôts sur les parois d'une enceinte à vide ont déjà été proposés dans le passé pour améliorer la pression d'un système à vide, par exemple comme décrit dans le document DE-A-38 14 389. Dans ce document, le dépôt d'une couche de bore et de carbone, obtenu par plasma radiofréquence à partir d'un mélange de borane et d'hydrocarbures, est proposé principalement pour réduire la pression partielle de vapeur d'eau dans l'enceinte.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. In this document, 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.

Dans ce même document DE-A-38 14 389, l'utilisation de couches minces de titane, de hafnium et de zirconium est également mentionnée, mais pour être rejetée à cause des difficultés majeures rencontrées dans la production et la régénération de ces couches. In this same document DE-A-38 14 389, the use of thin layers of titanium, hafnium and zirconium is also mentioned, but to be rejected because of the major difficulties encountered in the production and regeneration of these layers.

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 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.

A ces fins, il est proposé conformément à l'invention de mettre en oeuvre la succession des étapes qui suivent :

  • a) on effectue par pulvérisation cathodique 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 température 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.
    • For these purposes, it is proposed in accordance with the invention to implement the succession of the following steps:
  • a) depositing a thin layer of non-evaporable getter on cathode sputtering on at least most of the surface of the wall of the enclosure,
  • b) the enclosure is assembled with a vacuum system, the vacuum is made using the vacuum system, the vacuum system is steamed at a given temperature while maintaining the enclosure at a temperature below the non-evaporable getter activation temperature,
  • c) the steaming of the vacuum system is stopped, and simultaneously the temperature of the enclosure is raised to the activation temperature, this temperature is maintained for a predetermined period appropriate to make the getter layer non-evaporable clean, then the temperature is lowered to room temperature.

    • La couche de getter non évaporable 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 susceptible 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.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. In addition, in the bedrooms of particle accelerators, 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.

    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.In addition, 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.

    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 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. Likewise, in electron machines, the design of the vacuum chamber could be greatly simplified by eliminating the lateral pumping channel become useless.

    Pour que l'efficacité du getter en couche mince puisse conduire à l'effet de pompage optimum recherché, le matériau utilisé posséde certaines caractéristiques isolées ou combinées en tout ou partie.So that the efficiency of the thin layer getter can lead to the desired optimum pumping effect, the material used has certain isolated characteristics 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 large adsorption capacity for 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.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.

    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, 200-250°C 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'activation doit être au plus égale à 400°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.

    Le matériau doit enfin posséder une grande solubilité, 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 2 nm (20Å), 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.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. For example, with a non-evaporable getter layer 1 µm thick and 2 nm (20 Å) thick, oxide formed surface at each exposure, an oxygen concentration of 2% in the getter would be reached after about 10 cycles, without counting the other gases pumped during the operation under empty; thicker layers could be considered, but they would take longer to deposit and their membership could become worse.

    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 ambiante, supérieure à 2 % peuvent constituer des getter non évaporables 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.Ultimately, 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. Note that titanium, zirconium and hafnium have a solubility for oxygen close to 20%, while vanadium and scandium have great diffusivity for gases. We can well heard also retained, alone or in association with at least one of the aforementioned bodies, any alloy comprising at least minus one of the bodies, so as to combine the effects obtained, or even to obtain new effects not resulting not directly 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 CO2 de l'ordre de 1 ls-1 par cm2 de surface.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 CO 2 of the order of 1 ls -1 per cm 2 of surface.

    Il 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 température dans la couche mince. Cette disposition est très avantageuse car elle permet d'utiliser, en tant que getter, des matériaux à pyrophoricité 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.It should be added as an additional advantage that the implementation of 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.

    On peut enfin noter que l'utilisation d'un getter non évaporable sous forme de couche mince offre la possibilité 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 pulvérisation cathodique simultanée de plusieurs corps, à l'aide d'une cathode composite dont il est question plus loin.We can finally note that the use of a getter non-evaporable in the form of a thin layer offers the possibility to create thermodynamically unstable materials, which widens the field of the choice of the optimum material in as a getter. This possibility can be exploited by simple way using a spraying technique simultaneous cathodic of several bodies, using a composite cathode which is discussed below.

    De façon plus détaillée, ou procède comme il suit:

  • 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, par pulvérisation cathodique, le dépôt du getter en une couche mince sur au moins la plus grande partie de la surface de la paroi définissant l'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 l'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.
    • In more detail, or proceed as follows:
  • a) the enclosure is cleaned; the thin layer deposition device is introduced inside the enclosure; a relative vacuum is created in the enclosure; the enclosure is steamed in order to remove as much of the water vapor as possible; then is carried out, by sputtering, the deposition of the getter in a thin layer on at least the largest part 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 internally coated 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) the steaming of the installation is stopped and simultaneously the temperature of the enclosure is raised 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.

    • 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 apparait un phénomène de pompage moléculaire dû à la réaction chimique, sur la surface de la couche de getter, des gaz présents dans l'enceinte.At the end of this procedure, the surface of the layer thin getter 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, gases present in the enclosure.

    Pour effectuer le dépôt du getter en couche mince sur la surface de la paroi de l'enceinte, un processus d'évaporation sous vide 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 est en pratique plus avantageux d'avoir recours à un processus de pulvérisation cathodique qui autorise un contrôle plus efficace des conditions de formation de la couche mince. To deposit the getter in a thin layer on the surface of the enclosure wall, a vacuum evaporation process seems difficult to control from efficient way to form a uniform layer and homogeneous, in particular when depositing several body, and it is in practice more beneficial to have use of a sputtering process which allows more effective control of the conditions of formation of the thin layer.

    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 centralement 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.In addition, 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. To do this, 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.

    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 l'invention dans des systèmes à vide souvent exposés à l'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.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. 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 circulation de faisceau de particules serait alors effacée et dans lesquels les problèmes d'instabilité du vide seraient éliminés.More specifically, 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.

    Claims (3)

    1. A process for using a getter to create, due to a getter function, a very high vacuum in a chamber defined by a metal wall capable to release gas at a surface thereof, said getter being deposited on at least a majority of said chamber wall surface,
      characterized by the succession of the following steps:
      a) a thin coating of a non-evaporable getter is deposited, carried out by cathode sputtering, on said at least majority of said chamber wall surface,
      b) said chamber is assembled with a vacuum system, a vacuum is made with the use of said vacuum system, said vacuum system is dehydrated at a given temperature while maintaining said chamber at a temperature lower than the temperature of activation of said non-evaporable getter,
      c) said dehydrating of said vacuum system is stopped, and simultaneously the temperature in said chamber is raised up to said activation temperature, said activation temperature is maintained for a predetermined period suitable to cleanse said non-evaporable getter coating, then the temperature is lowered to room temperature.
    2. A process according to claim 1, characterized in that said non-evaporable getter is selected from titanium and/or zirconium and/or hafnium and/or vanadium and/or scandium and/or an alloy including at least one of these.
    3. A process according to claim 1 or 2, characterized by the use, for depositing a non-evaporable getter coating made of an alloy of several metals, a cathode located centrally in said chamber, and which can be constituted with several wires of said respective alloy metals twisted around each other.
    EP97929213A 1996-06-19 1997-06-18 Method for using a non-vaporisable getter Expired - Lifetime EP0906635B1 (en)

    Applications Claiming Priority (3)

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

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    EP (1) EP0906635B1 (en)
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    ATE233946T1 (en) 2003-03-15
    NO317454B1 (en) 2004-11-01
    ES2193382T3 (en) 2003-11-01
    CA2258118A1 (en) 1997-12-24
    CA2258118C (en) 2010-08-17
    DE69719507T2 (en) 2004-02-19
    WO1997049109A1 (en) 1997-12-24
    PT906635E (en) 2003-07-31
    DK0906635T3 (en) 2003-06-23
    EP0906635A1 (en) 1999-04-07
    US6468043B1 (en) 2002-10-22
    NO985927L (en) 1998-12-17
    FR2750248B1 (en) 1998-08-28
    RU2193254C2 (en) 2002-11-20
    DE69719507D1 (en) 2003-04-10
    AU3340497A (en) 1998-01-07
    JP2001503830A (en) 2001-03-21
    FR2750248A1 (en) 1997-12-26
    NO985927D0 (en) 1998-12-17
    JP4620187B2 (en) 2011-01-26

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