EP0275844A2 - Dispositif getter non évaporable comportant un support céramique et son procédé de fabrication - Google Patents

Dispositif getter non évaporable comportant un support céramique et son procédé de fabrication Download PDF

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Publication number
EP0275844A2
EP0275844A2 EP87830452A EP87830452A EP0275844A2 EP 0275844 A2 EP0275844 A2 EP 0275844A2 EP 87830452 A EP87830452 A EP 87830452A EP 87830452 A EP87830452 A EP 87830452A EP 0275844 A2 EP0275844 A2 EP 0275844A2
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EP
European Patent Office
Prior art keywords
support
getter device
porous
weight percent
chosen
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
EP87830452A
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German (de)
English (en)
Other versions
EP0275844B1 (fr
EP0275844A3 (en
Inventor
Claudio Boffito
Ettore Giorgi
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SAES Getters SpA
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SAES Getters SpA
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Publication date
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Publication of EP0275844A2 publication Critical patent/EP0275844A2/fr
Publication of EP0275844A3 publication Critical patent/EP0275844A3/en
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Publication of EP0275844B1 publication Critical patent/EP0275844B1/fr
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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

Definitions

  • the present invention relates to a non-evapo­rable getter device comprising a ceramic support, as well as a method for the manufacture of such a device.
  • Non-evaporable getter devices are well-known in the art. They usually consist of a powdered metal or alloy which when heated to an elevated temperature, diffuse into the bulk a protective layer such that the surface of the particles become reactive towards a large number of gases.
  • the non-evaporable getter material is held in a support such as, for instance, by pressing the powder into a U-shaped metal ring channel.
  • a wire which has previously been coated with a ceramic insulating material such as alumina.
  • the wire coated with alumina is used as one electrode in an electrophoretic coating bath in which there are suspend­ed particles of the getter material.
  • the getter material is electrophoretically deposited onto the ceramic coated wire.
  • the use of such a support has several disadvantages. Firstly the alumina layer on the wire must be very thin otherwise it is very difficult to cause sufficient electric current to flow to effect the deposition. Due to the high electri­cal resistance of the alumina coating it is also very difficult to control the parameters of deposition, resulting in an uneven deposition. An additional diffi­culty is that during a subsequent sintering process the electrophoretically deposited getter material detaches from the ceramic support producing flakes and undesirable loose particles.
  • a ceramic support is coated with a thin electrically conductive film.
  • the ceramic support may be of any ceramic material which is compatible with use in high vacuum, preferably alumina. It may be of any shape size or thickness.
  • the thin conductive film may be of any conductive material such as tin oxide or other conductive oxides. It is preferable however to use a thin metal layer such as aluminium or copper.
  • the ceramic may be coated with this thin metallic film by any known method such as electroplating or by deposition in vacuum.
  • the thin metal film can be Ni, Cu, Ag, Mo or Fe but is preferably aluminium. Its thickness is preferably between 0.1 ⁇ m and 5 ⁇ m.
  • the thin conductive film is then made to be one electrode of an electroplating bath.
  • a thicker metallic film having a thickness of several micrometers and preferably between 5 ⁇ m and 50 ⁇ m.
  • the electroplated metal film may be of any metal which is compatible with use in high vacuum such as Ti, Zr, Mo, Fe, Cu, Ag, Pt, Au but it is preferably nickel.
  • the thin conductive film and the thicker metal layer constitute an intermediate electrically conductive layer which could however be a single metal­lic layer.
  • the electroplated support is electrophoretical­ly coated with a mixture of a particulate non-evaporable getter material and an antisintering material.
  • the electrophoretic coating takes place according to a process as described in UK Patent application publica­tion GB 2,157,486 A.
  • the particular non-evaporable getter material is any getter material suitable for the sorption of active gases in vacuum. It is preferably chosen from the group consisting of titanium, zirconium and their hydrides. Its particle size should be between 20-60 ⁇ m and preferably with an average size of 40 ⁇ m.
  • the antisintering material is in particulate form and is any material which is capable of hindering the sintering of the non-evaporable getter material. It is preferably chosen from the group consisting of graphite, refractory metals and zirconium based alloys. If a zirconium based alloy is used as an antisintering material, then it is preferably chosen from the group consisting of:
  • the antisintering material preferably has a particle size of between 20-60 ⁇ m with an average particle size of 40 ⁇ .
  • the weight ratio of the particu­late non-evaporable getter material to the particulate antisintering material is from 1 : 4 to 4 : 1.
  • the getter material If a hydrided material is used as the getter material then this temperature should be maintained for a sufficient time as to release all hydrogen.
  • the getter device is then heated at a higher temperature such as between 900°C and 1000°C to produce a porous non-evaporable getter device in which the thicker metal layer diffuses into the ceramic support and the electrophoretically coated getter mixture.
  • the getter device is then allowed to cool to room teperature whereupon it is removed from the vacuum oven and is ready for use.
  • the term "sintering" as used herein refers to the process of heating powdered material at a tempe­rature and for a time sufficient to give some mass transfer between adjacent particles without appreciably reducing the surface area of the powdered material. The mass transfer serves to bind the particles together thereby increasing strength and reducing the number of loose particles. Lower temperatures require longer times.
  • the sintering temperature of a material is that temperature at which the above-described sintering takes place in about one hour. In a preferred embodiment of the present invention a temperature is chosen which is at or slightly above the sintering temperature of the non-evaporable getter material and below the sinter­ing temperature of the antisintering material.
  • ceramic means any material that is not electrically conductive at the temperature of use including glass-ceramics, quartz-glass, SiO2, refractory metal oxides in general and Al2O3 in particular.
  • Figure 1 shows a porous non-evaporable getter device 102 comprising a ceramic substrate 104.
  • Ceramic support 104 has one of its surfaces 106 coated with a thin film 108 of conductive material.
  • On the thin film 108 of conductive material is an electrodeposited thicker layer 110 of metal.
  • Onto thicker film 110 has been electrophoretically deposited particles 112, 112 ⁇ of particulate non-evaporable getter material and particles 114, 114 ⁇ of antisintering material.
  • FIG. 2 shows a porous non-evaporable getter device 202 similar to that shown in Fig. 1 except that it has now been subject to a sintering process.
  • Getter device 202 comprises a ceramic support 204 that supports particles of non-evaporable getter material 206, 206 ⁇ and particles 208, 208 ⁇ of antisintering material.
  • the thin and thick conductive layers have diffused into the ceramic to produce a diffusion layer 210 and they have diffused into the getter and/or antisintering material particles to produce diffusion zones 212, 212 ⁇ .
  • these diffusion zones may result from a single metallic layer.
  • This comparative example was designed to show the behaviour of a prior art porous non-evaporable getter device comprising a ceramic support and a porous sintered getter material layer.
  • a metallic wire was coated with a thin layer of alumina thereby forming a tube which was coated electrophoretically following the process as described in the above mentioned UK Patent Application Publication GB 2,157,486 A using getter material particles of titanium hydride and antisintering particles of a Zr-V-Fe alloy both having a particle size of approximately 40 ⁇ m. After the sintering process and cooling down to room temperature a metallurgical cross-section was made and is shown in Fig. 3.
  • Figure 3 shows the cross-section 302 where can be seen the ceramic support 304 of alumina.
  • the sintered non-evaporable getter material 306 comprising titanium and Zr-V-Fe is found to be separated from the ceramic support 304 by a space 308 showing a detach­ment of the getter material 306 from the ceramic support 304.
  • This example is designed to show the behaviour of a porous non-evaporable getter device of the present invention.
  • An alumina tube was taken and its external surface was coated with aluminium in a vacuum deposition apparatus. Using the aluminium film as an electrode a thicker layer of Ni was electroplated upon it. The Ni layer was then used as an electrode in an electrophore­tic deposition bath exactly as for Example 1.
  • the porous non-evaporable getter material again comprised Ti hydride and a Zr-V-Fe alloy as an antisintering agent. The particle size of both components was approxi­mately 40 ⁇ m. After the sintering operation and cooling to room temperature a cross-section 402 of the getter device was made and reported in Fig. 4.
  • the alumina support 404 and the getter material 406 are shown to be clearly adhering to each other along line 408. The aluminium and nickel layers can no longer be seen as they have diffused into the alumina and the getter material.
  • the deposition took place in a few seconds at an applied voltage of 15 V with the passage of 1 ampere. No H2 formation was observed and the deposition was able to take place for 20 seconds thus providing a sufficient quantity of getter material with a smooth uniform surface appearance.
  • This example illustrates that embodiment of the present invention wherein the intermediate electrically conductive layer is a single metal.
  • Example 2 The procedure of Example 2 is repeated except that the aluminium is replaced with nickel such that the intermediate electrically conductive layer is substantially all nickel.

Landscapes

  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Separation Of Gases By Adsorption (AREA)
  • Manufacture Of Electron Tubes, Discharge Lamp Vessels, Lead-In Wires, And The Like (AREA)
  • Vessels, Lead-In Wires, Accessory Apparatuses For Cathode-Ray Tubes (AREA)
  • Common Detailed Techniques For Electron Tubes Or Discharge Tubes (AREA)
EP87830452A 1986-12-22 1987-12-21 Dispositif getter non évaporable comportant un support céramique et son procédé de fabrication Expired - Lifetime EP0275844B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IT2280786 1986-12-22
IT22807/86A IT1201540B (it) 1986-12-22 1986-12-22 Dispositivo getter non evaporabile comprendente un supporto ceramico e metodo per la sua fabbricazione

Publications (3)

Publication Number Publication Date
EP0275844A2 true EP0275844A2 (fr) 1988-07-27
EP0275844A3 EP0275844A3 (en) 1990-02-28
EP0275844B1 EP0275844B1 (fr) 1993-07-28

Family

ID=11200649

Family Applications (1)

Application Number Title Priority Date Filing Date
EP87830452A Expired - Lifetime EP0275844B1 (fr) 1986-12-22 1987-12-21 Dispositif getter non évaporable comportant un support céramique et son procédé de fabrication

Country Status (5)

Country Link
EP (1) EP0275844B1 (fr)
JP (1) JPH0687402B2 (fr)
DE (1) DE3786779T2 (fr)
IN (1) IN169971B (fr)
IT (1) IT1201540B (fr)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3923745A1 (de) * 1989-07-18 1991-01-31 Eltro Gmbh Laservorrichtung mit ramanzelle
WO1995023425A1 (fr) * 1994-02-28 1995-08-31 Saes Getters S.P.A. Ecran plat a emission de champ renfermant un degazeur, et son procede de fabrication
EP1100107A2 (fr) * 1999-11-12 2001-05-16 Sony Corporation Getter, affichage à panneau plat et méthode pour sa fabrication
US6735845B2 (en) * 1997-02-20 2004-05-18 Mks Instruments Inc. Method of producing an integrated reference pressure sensor element
DE102014203083A1 (de) * 2014-02-20 2015-08-20 Mahle International Gmbh Adsorbervorrichtung
US20150334845A1 (en) * 2013-02-25 2015-11-19 Kyocera Corporation Package for housing electronic component and electronic device
CN114318233A (zh) * 2021-12-10 2022-04-12 兰州空间技术物理研究所 一种具有薄膜镀层的吸气剂及其制备方法和应用
CN115185169A (zh) * 2022-09-07 2022-10-14 上海晶维材料科技有限公司 一种用于空间氢原子钟上具有抗粉化能力的吸附泵
WO2023186704A1 (fr) * 2022-04-01 2023-10-05 Saes Getters S.P.A. Substrat comprenant une base et un film getter intégré pour fabriquer des dispositifs microélectroniques

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6911065B2 (en) * 2002-12-26 2005-06-28 Matheson Tri-Gas, Inc. Method and system for supplying high purity fluid
CN109680249A (zh) * 2019-01-25 2019-04-26 苏州大学 非蒸散型薄膜吸气剂及其制备方法
CN110820031A (zh) * 2019-11-19 2020-02-21 有研工程技术研究院有限公司 一种微型吸气剂的制备方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3620645A (en) * 1970-05-01 1971-11-16 Getters Spa Getter device
GB2000370A (en) * 1977-06-27 1979-01-04 Philips Nv Electric lamps
FR2447745A1 (fr) * 1979-02-05 1980-08-29 Getters Spa Procede d'adsorption d'eau, de vapeur d'eau et d'autres gaz, utilisant un alliage ternaire adsorbant non vaporisable
GB2157073A (en) * 1984-03-16 1985-10-16 Getters Spa Cathode ray tube with an electrophoretic getter
US4620645A (en) * 1984-03-26 1986-11-04 Aeroil Products Company, Inc. Portable asphalt melting and dispensing apparatus

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3620645A (en) * 1970-05-01 1971-11-16 Getters Spa Getter device
GB2000370A (en) * 1977-06-27 1979-01-04 Philips Nv Electric lamps
FR2447745A1 (fr) * 1979-02-05 1980-08-29 Getters Spa Procede d'adsorption d'eau, de vapeur d'eau et d'autres gaz, utilisant un alliage ternaire adsorbant non vaporisable
GB2157073A (en) * 1984-03-16 1985-10-16 Getters Spa Cathode ray tube with an electrophoretic getter
US4620645A (en) * 1984-03-26 1986-11-04 Aeroil Products Company, Inc. Portable asphalt melting and dispensing apparatus

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3923745A1 (de) * 1989-07-18 1991-01-31 Eltro Gmbh Laservorrichtung mit ramanzelle
WO1995023425A1 (fr) * 1994-02-28 1995-08-31 Saes Getters S.P.A. Ecran plat a emission de champ renfermant un degazeur, et son procede de fabrication
US6735845B2 (en) * 1997-02-20 2004-05-18 Mks Instruments Inc. Method of producing an integrated reference pressure sensor element
US7155803B2 (en) 1997-02-20 2007-01-02 Mks Instruments Inc. Method of manufacturing a sensor element having integrated reference pressure
EP1100107A2 (fr) * 1999-11-12 2001-05-16 Sony Corporation Getter, affichage à panneau plat et méthode pour sa fabrication
EP1100107A3 (fr) * 1999-11-12 2004-06-02 Sony Corporation Getter, affichage à panneau plat et méthode pour sa fabrication
US20150334845A1 (en) * 2013-02-25 2015-11-19 Kyocera Corporation Package for housing electronic component and electronic device
US9756731B2 (en) * 2013-02-25 2017-09-05 Kyocera Corporation Package for housing electronic component and electronic device
DE102014203083A1 (de) * 2014-02-20 2015-08-20 Mahle International Gmbh Adsorbervorrichtung
CN114318233A (zh) * 2021-12-10 2022-04-12 兰州空间技术物理研究所 一种具有薄膜镀层的吸气剂及其制备方法和应用
WO2023186704A1 (fr) * 2022-04-01 2023-10-05 Saes Getters S.P.A. Substrat comprenant une base et un film getter intégré pour fabriquer des dispositifs microélectroniques
CN115185169A (zh) * 2022-09-07 2022-10-14 上海晶维材料科技有限公司 一种用于空间氢原子钟上具有抗粉化能力的吸附泵

Also Published As

Publication number Publication date
EP0275844B1 (fr) 1993-07-28
EP0275844A3 (en) 1990-02-28
DE3786779D1 (de) 1993-09-02
IT1201540B (it) 1989-02-02
JPS63182283A (ja) 1988-07-27
IN169971B (fr) 1992-01-18
IT8622807A0 (it) 1986-12-22
DE3786779T2 (de) 1993-11-18
JPH0687402B2 (ja) 1994-11-02

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