US3598384A - Metal vapor generators - Google Patents

Metal vapor generators Download PDF

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Publication number
US3598384A
US3598384A US856529A US3598384DA US3598384A US 3598384 A US3598384 A US 3598384A US 856529 A US856529 A US 856529A US 3598384D A US3598384D A US 3598384DA US 3598384 A US3598384 A US 3598384A
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United States
Prior art keywords
metal vapor
chamber
opening
substance
walls
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Expired - Lifetime
Application number
US856529A
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English (en)
Inventor
Mario Zucchinelli
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SAES Getters SpA
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SAES Getters SpA
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Publication of US3598384A publication Critical patent/US3598384A/en
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B5/00General methods of reducing to metals
    • C22B5/02Dry methods smelting of sulfides or formation of mattes
    • C22B5/16Dry methods smelting of sulfides or formation of mattes with volatilisation or condensation of the metal being produced
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • C23C14/243Crucibles for source material
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/02Manufacture of electrodes or electrode systems
    • H01J9/12Manufacture of electrodes or electrode systems of photo-emissive cathodes; of secondary-emission electrodes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/20Manufacture of screens on or from which an image or pattern is formed, picked up, converted or stored; Applying coatings to the vessel
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/38Exhausting, degassing, filling, or cleaning vessels
    • H01J9/395Filling vessels

Definitions

  • FIG. 1 is a plan view of a generator of the present invention
  • FIG. 2 is an elevation view of the generator of FIG. 1;
  • FIG. 3 is an enlarge sectional view taken along line 3-3 of FIG. 2;
  • FIG. 4 is an enlarged sectional view taken along line 4-4 of FIG. 2;
  • FIG. 5 is an enlarged sectional view taken along line 5-5 of FIG. 1.
  • a particle free device for releasing a metal vapor comprising a container having continuous walls defining a chamber. The extremities of the walls are juxtaposed parallel to one another to form an opening. A particulate metal vapor releasing substance is within the chamber. Also within the chamber and adjacent to the opening is a member placed such that the opening is rendered permeable to metal vapor but impermeable to the particulate substance.
  • the container can have any convenient shape, but in one preferred embodiment of the present invention is made from a generally rectangular sheet of material, bent around its longer axis such that the longitudinal extremities of the sheet material are juxtaposed parallel to one another, and define an opening through which the metal vapor is released.
  • the container is made of a material of high electrical resistance permitting activation of the metal vapor releasing substance by imposing an electrical potential across the ends ofthe container to heat the container.
  • the particulate metal vapor releasing substance within the chamber can be virtually any suitable material but is generally a mixture of a compound of the desired metal and a reducing agent for the compound.
  • Mercuric oxide can also be employed if mercury is the desired metal.
  • Any suitable reducible agent such as those described in Eichenbaum or the Italian patent supra can be employed, examples of which include, among others, silicon and aluminum.
  • the desired metal is barium, any of the well known barium aluminum alloys can be employed.
  • the metal vapor releasing substance is particulate in order to provide a large surface area for vaporization of the metal and/or chemical reaction. However if the particles are too small they tend to escape from the device. Generally those which pass through a US. standard screen of I70 mesh/inch and are retained on a screen of 45 mesh/inch, i.e. those exhibiting a particle size of about l0 to 9011., are suitable.
  • the member within the chamber is located adjacent to the opening whereby the opening is rendered permeable to metal vapor, but impermeable to the particulate substance.
  • the member can have any suitable geometric shape but is preferably elongated having its axis parallel to the extremities of the walls or sheet.
  • the cross section can be any regular of irregular polygon and, thus, can be triangular, square, or hexagonal but is preferably round since such a cross section gives the best seal against loose particles.
  • the member within the chamber is a wire having a diameter greater than the distance between the extremities of the walls.
  • the device 10 comprises a container or tube I I having terminals 12 and I3 in each end thereof.
  • the terminals I2 and I3 seal the ends of the tube II and together with the walls thereof, define a chamber containing the metal vapor releasing substance I4 which preferably fills the chamber.
  • the tube II is formed from a continuous sheet of material such that the tube 11 has a lower wall 15 connected to sidewalls I6 and 17 which in turn are connected to top walls 18 and 19.
  • the edges of the sheet which is comprised of top walls 18 and [9 meet in juxtaposed relationship defining an opening 20 of width d which is generally to 300 microns.
  • a member 21 which is preferably a wire of circular cross section.
  • the wire 21 is held in place by the substance 14.
  • the diameter of the wire 21 is greater than the dimension d.
  • the axis of the wire 21 is parallel to the longitudinal edge of the top wall 18 and, therefore, also the top wall 19;
  • a common method of producing the device 10 is to compress the particulate substance 14 and form the walls I5, 16, I7, l8, and I9 into the general form of FIG. 3 but with the walls to and I7 angled outward at a greater angle than shown, thus making 1! much larger.
  • the walls 16 and I7 are then pressed towards one another to reduce d to the desired value.
  • the compressed material M adjacent to the opening 20 fractures and produces loose particles.
  • the device I0 is placed in a vessel such as an image intensifier tube in which it is desired to introduce cesium vapor.
  • the terminals 12 and I3 are connected to a source of potential not shown, and the tube evacuated by any known means.
  • Current is then caused to flow through the nichrome tube II by impressing a potential across the terminals I2 and I3 until the tube 11 is heated to about 1,000 K, whereupon the substance 14, which is a mixture of one part by weight of Cs CrO and two parts by weight of Si, releases cesium vapor. No loose particles are observed in the vessel either before or after cesium vapor release.
  • a particle free device for releasing a metal vapor comprising;
  • the metal vapor releasing substance is a mixture of an alkali metal chromate and a reducing agent for the chromate
  • a particle free device for releasing a metal vapor comprising:
  • said device comprising:
  • a particle free device for releasing a metal vapor comprising; a container having walls defining a chamber; an opening in at least one of said walls; a particulate, metal vapor releasing substance within the chamber; and a member within the chamber and adjacent to the opening whereby the opening is rendered permeable to metal vapor but impermeable to the particulate substance wherein the chamber is completely filled with the metal vapor releasing substance which holds the member in place.
  • delete delete delete delete delete delete delete delete delete delete 20 delete "absorption”, insert -sorption "absorb”, insert sorb- "enlarge”, insert -enlarged- "45”, insert -450 "of", insert -or "absorb” insert -sorb and sealed this 22nd day of February 1972.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Physical Vapour Deposition (AREA)
US856529A 1968-09-13 1969-09-10 Metal vapor generators Expired - Lifetime US3598384A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
IT2118568 1968-09-13

Publications (1)

Publication Number Publication Date
US3598384A true US3598384A (en) 1971-08-10

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Family Applications (1)

Application Number Title Priority Date Filing Date
US856529A Expired - Lifetime US3598384A (en) 1968-09-13 1969-09-10 Metal vapor generators

Country Status (4)

Country Link
US (1) US3598384A (ja)
DE (1) DE1945508B2 (ja)
FR (1) FR2018043A1 (ja)
NL (1) NL6913693A (ja)

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3746502A (en) * 1971-12-20 1973-07-17 Xerox Corp Evaporation crucible
US3748090A (en) * 1971-12-20 1973-07-24 Xerox Corp Evaporation crucible
US3984088A (en) * 1974-10-16 1976-10-05 Leybold-Heraeus Gmbh & Co. Kg Vaporizing crucible for vacuum vapor coating systems
US4112290A (en) * 1976-10-27 1978-09-05 Denki Kagaku Kogyo Kabushiki Kaisha Evaporation vessel for use in vacuum evaporation
US4227961A (en) * 1975-06-27 1980-10-14 Futaba Denshi Kogyo K.K. Process for forming a single-crystal film
US5417766A (en) * 1994-04-26 1995-05-23 Itt Corporation Channel evaporator
WO2002093664A2 (en) * 2001-05-15 2002-11-21 Saes Getters S.P.A Cesium dispensers and process for the use thereof
US20050145179A1 (en) * 2002-09-06 2005-07-07 Saes Getters S.P.A. Accessory member for dispensers of alkali metals
US20090266201A1 (en) * 2006-03-13 2009-10-29 Saes Getters S.P.A. Use of Magnesium-Copper Compositions for the Evaporation of Magnesium and Magnesium Dispensers
US7625505B2 (en) 2004-09-10 2009-12-01 Saes Getters S.P.A. Mixtures for evaporation of lithium and lithium dispensers
US20100189929A1 (en) * 2009-01-28 2010-07-29 Neal James W Coating device and deposition apparatus
US7842194B2 (en) 2004-11-24 2010-11-30 Saes Getters S.P.A. Dispensing system for alkali metals capable of releasing a high quantity of metals
CN105359248A (zh) * 2013-07-11 2016-02-24 工程吸气公司 改进的金属蒸气给料器

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2378476A (en) * 1943-02-11 1945-06-19 American Optical Corp Coating apparatus
US2793609A (en) * 1953-01-26 1957-05-28 British Dielectric Res Ltd Means for the deposition of materials by evaporation in a vacuum
US3014115A (en) * 1957-09-09 1961-12-19 Howard E Ingersoll Liquid mercury vaporizer
US3058842A (en) * 1958-12-29 1962-10-16 Ibm Evaporation method
US3446936A (en) * 1966-01-03 1969-05-27 Sperry Rand Corp Evaporant source
US3457097A (en) * 1964-02-10 1969-07-22 Yawata Seitetsu Kk Method of coating ferrous metal with molten aluminum
US3466424A (en) * 1967-08-31 1969-09-09 Nasa Evaporant source for vapor deposition

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2378476A (en) * 1943-02-11 1945-06-19 American Optical Corp Coating apparatus
US2793609A (en) * 1953-01-26 1957-05-28 British Dielectric Res Ltd Means for the deposition of materials by evaporation in a vacuum
US3014115A (en) * 1957-09-09 1961-12-19 Howard E Ingersoll Liquid mercury vaporizer
US3058842A (en) * 1958-12-29 1962-10-16 Ibm Evaporation method
US3457097A (en) * 1964-02-10 1969-07-22 Yawata Seitetsu Kk Method of coating ferrous metal with molten aluminum
US3446936A (en) * 1966-01-03 1969-05-27 Sperry Rand Corp Evaporant source
US3466424A (en) * 1967-08-31 1969-09-09 Nasa Evaporant source for vapor deposition

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Publication: The Review of Scientific Instruments; Vol. 35, No. 6; June, 1964 (Eichenbaum et al.) *

Cited By (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3746502A (en) * 1971-12-20 1973-07-17 Xerox Corp Evaporation crucible
US3748090A (en) * 1971-12-20 1973-07-24 Xerox Corp Evaporation crucible
US3984088A (en) * 1974-10-16 1976-10-05 Leybold-Heraeus Gmbh & Co. Kg Vaporizing crucible for vacuum vapor coating systems
US4227961A (en) * 1975-06-27 1980-10-14 Futaba Denshi Kogyo K.K. Process for forming a single-crystal film
US4112290A (en) * 1976-10-27 1978-09-05 Denki Kagaku Kogyo Kabushiki Kaisha Evaporation vessel for use in vacuum evaporation
US5417766A (en) * 1994-04-26 1995-05-23 Itt Corporation Channel evaporator
US20040206205A1 (en) * 2001-05-15 2004-10-21 Saes Getters S.P.A. Cesium mixtures and use thereof
US20040001916A1 (en) * 2001-05-15 2004-01-01 Saes Getters S.P.A. Cesium dispensers and process for the use thereof
US6753648B2 (en) 2001-05-15 2004-06-22 Saes Getters S.P.A. Cesium dispensers and process for the use thereof
WO2002093664A2 (en) * 2001-05-15 2002-11-21 Saes Getters S.P.A Cesium dispensers and process for the use thereof
KR100742424B1 (ko) 2001-05-15 2007-07-24 사에스 게터스 에스.페.아. 세슘 디스펜서 및 세슘 디스펜서의 사용 방법
WO2002093664A3 (en) * 2001-05-15 2003-02-06 Getters Spa Cesium dispensers and process for the use thereof
US20050145179A1 (en) * 2002-09-06 2005-07-07 Saes Getters S.P.A. Accessory member for dispensers of alkali metals
US7794630B2 (en) 2004-09-10 2010-09-14 Saes Getters S.P.A. Lithium dispenser for lithium evaporation
US7625505B2 (en) 2004-09-10 2009-12-01 Saes Getters S.P.A. Mixtures for evaporation of lithium and lithium dispensers
US20100021623A1 (en) * 2004-09-10 2010-01-28 Saes Getters S.P.A. Lithium dispenser for lithium evaporation
US7842194B2 (en) 2004-11-24 2010-11-30 Saes Getters S.P.A. Dispensing system for alkali metals capable of releasing a high quantity of metals
US20090266201A1 (en) * 2006-03-13 2009-10-29 Saes Getters S.P.A. Use of Magnesium-Copper Compositions for the Evaporation of Magnesium and Magnesium Dispensers
US8029597B2 (en) 2006-03-13 2011-10-04 Saes Getters S.P.A. Use of magnesium-copper compositions for the evaporation of magnesium and magnesium dispensers
US20100189929A1 (en) * 2009-01-28 2010-07-29 Neal James W Coating device and deposition apparatus
CN105359248A (zh) * 2013-07-11 2016-02-24 工程吸气公司 改进的金属蒸气给料器
CN105359248B (zh) * 2013-07-11 2017-07-07 工程吸气公司 改进的金属蒸气给料器

Also Published As

Publication number Publication date
FR2018043A1 (ja) 1970-05-29
NL6913693A (ja) 1970-03-17
DE1945508B2 (de) 1971-06-09
DE1945508A1 (de) 1970-03-19

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