US2100045A - Deposition of metallic films from metal vaporized in vacuo - Google Patents

Deposition of metallic films from metal vaporized in vacuo Download PDF

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Publication number
US2100045A
US2100045A US105091A US10509136A US2100045A US 2100045 A US2100045 A US 2100045A US 105091 A US105091 A US 105091A US 10509136 A US10509136 A US 10509136A US 2100045 A US2100045 A US 2100045A
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United States
Prior art keywords
metal
vapor
support
heating
chamber
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US105091A
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English (en)
Inventor
Alexander Paul
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Owens Corning Intellectual Capital LLC
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Individual
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Assigned to OCV INTELLECTUAL CAPITAL, LLC reassignment OCV INTELLECTUAL CAPITAL, LLC CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). Assignors: SAINT-GOBAIN VETROTEX FRANCE
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING 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
    • C23C—COATING 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation

Definitions

  • films are deposited at substantially higher pressures than 1/ 10,000 mm. which have the characteristics of films hitherto deposited at this pressure, by heating the metallic vapor in its passage from its source to the support of the lm.
  • FIGS 1, 2 and 3. are vertical sections through alternative forms of apparatus for carrying out the invention, shown partly diagrammatically;
  • Figure 4 is a part section of an alternate form of vapor heating device
  • Figure 5 is a section through an alternative form oi' heating vessel
  • Figure 6 is a section through an alternative form o1' heating device for the metal.
  • the vacuum chamber I contains the support 2 on which the metal iilm is to be deposited, and the heating vessel 3 contains the metal to be vaporized.
  • the supports for the various parts ln the chamber are not shown in the drawing.
  • the heating vessel 3 is a refractory tube having holes 4 for the issueof the metal vapor.
  • the vessel 3 is heated by current passed through the spiral 5 from the conductors 6.
  • Between the heating vessel 3 and the support 2 is a device for heating the metal vapor, consisting oi two wire mesh screens 1 connected with conductors 8 whereby current is passed through the screens to heat them to at least the vaporization temperature of the metal to be deposited.
  • the metal vapor issuing from the holes l, passes through the meshes of the screens 'l in its passage to the support 2, and is heated by the screens, and is deposited on the support 2 in the form of a lm of good quality.
  • films have been deposited, at a chamber pressure of 1/ 100 mm. and even higher, which are of as good quality as lms heretofore deposited at pressures of 1/10,00Q mm. and lower.
  • FIG. 2 shows an alternative form of heating vessel 3 and an alternative form of vapor heating device.
  • the vessel here consists of a tube of metal of high melting point, such as tungsten or molybdenum, which itself forms the heating element through which current is passed by the conductors i.
  • the vapor heating device consists of a tube 9 bent in zig-zag, supplied with a gas inert to the metal vapor at its right hand end and closed at its left hand end.
  • the tube 9 may itself form the heating element, as shown in the drawing, current being supplied to it by the conductors 8.
  • the tube may be made of palladium, and the gas supplied may be hydrogen, to which the walls of the tube are porous.
  • the tube may be made of a porous refractory material, and heated by a spiral wire heating element.
  • the heated gas issuing through thewalls ofthe tube 9 heats the metal vapor in its passage between the zig-zags of the tube.
  • 'I'he quantity of gas introduced must not be so large as unduly to increase the vaporization temperature of the metal. Even without continuous evacuation, sufficient gas can be introduced to heat the metal vapor effectively current by conductors l (of which one is visible),
  • a metal plate i3 which-is heated to a temperature at least equal to the vaporization temperature of the metal to be deposited, by current passed through it from conductors d (of which one is visible). The metal vapor issuing from the outlet I2 impinges against the heated plate it in its passage to the support t and is heated thereby.
  • the heating of the'vapor heating device such as the wire mesh screen l may be eilected as shown in Figure 4, in which the screen is in two parte 'la and 1b insulated one from the other and connected to high tension conductors l, whereby a glow discharge is maintained between the as shown in Figure 6, where the metal l0 is contained in a refractory vessel 3, while above it are located plates l5; the plates i5 and the metall it are connected to high tension conductors it, whereby a glow discharge is maintained between the plates and the metal.
  • a heating vessel such as that shown in cross-section in Figure 5 is of advantage, in which the cross-sectional area (that is to say, the space for the vapor) increases from the surface lil of the metal to the outlet Ill.
  • the ionization may be produced by electrodes it ( Figure 1) within the chamber l, to which electric potential is applied.
  • applicant has produced lms of good quality with a gas pressurein the vacuum. chamber exceeding 1/100 mm., but the maximum pressure which can be used depends on the rate of vaporization, the degree of heating of the vapor in its passage to the support, the vapor pressure of the metal used and whether the gas is ionized, and, for any given set of conditions, can best be ascertained by trial.
  • Apparatus for depositing a metal film on a support in an evacuated chamber comprising means for vaporizing the metal and means located between the source of the vapor and the support adapted to heat the metal vapor.
  • Apparatus for depositing a-metal lm on a support in an evacuated chamber comprising means for vapog the metal. a metallic member adapted to allow the metal vapor to pass through it, interposed between the source of the vapor and the support, and means for heating the metallic member to a temperature above the vaporization temperature of the metal.
  • Apparatus for depositing a' metal nlm on a support in an evacuated chamber comprising means for vaporiaing the metal. a wire mesh screen vlocated between the source oi' the vapor and the support, and means for heating the wire mesh screen to a temperature above the vaporisation temperature of the metal.
  • Apparatus ior depositing a metal film on a support in an evacuated chamber, comprising means for vaporizing the metal, a metallic member so located that the vapor issuing from the source impinges upon it in the passage of the vapor to the support, and means for heating the metallic member to a temperature above the vaporization temperature of the metal.
  • Apparatus for depositing a metal nlm on al support in an evacuated chamber comprising means for vaporizing the metal, a metallic member adapted to allow the metal vapor to pass through it, interposed between the source of the vapor and the support, an electrode, and means for producing a glow discharge between the metallic member and the electrode.
  • Apparatus for depositing a metal nlm on a support in an evacuated chamber comprising means for vaporizing the metal, two wire mesh screens located between the source of the vapor and the support and means for producing a, glow discharge between the two wire mesh screens.
  • Apparatus as in claim 1 comprising two electrodes and means for producing an electric discharge between them adapted to ionize the gas in the chamber.
  • Apparatus as in claim 2 comprising two electrodes and means for producing an electric discharge between them adapted to ionize tlie gas in the chamber.
  • Apparatus for depositing a metal ilm on a support in .an ,evacuated chamber comprising a vessel adapted to contain the metal to be vaporized and means for supplying heat to the metal to vaporize it, the vessel being so shaped that its cross-sectional area increases from the surface of the metal to the outlet, and means located between the outlet and the support adapted to heat the vapor.
  • Apparatus for depositing a metal nlm on a support in an evacuated chamber comprising a metallic vessel adapted to contain the metal to be vaporized, means for passing an electric current through the vessel to heat it to a temperature above the vaporization temperature of the metal, and means located between the outlet of the vessel and the support adapted to heat the vapor.
  • Apparatus for depositing a metal film on a support in an evacuated chamber comprising a vessel adapted to contain the metal to be vaporized, an electrode, means for producing a glow discharge between the metal and the electrode, adapted to heat the metal to vaporize it, and means located between the outlet of the vessel and the support adapted to heat the vapor.
  • Apparatus as in claim 9, comprising two electrodes and means for producing an electric discharge between them adapted to ionize the gas in the chamber.
  • Apparatus as in claim 10 comprising two electrodes and means for producing an electric discharge between them adapted to ionize the gasv in the chamber.
  • Apparatus as in claim 11, comprising two electrodes and means for producing an electric discharge between them adapted to ionize the gas in the chamber.
  • Process of depositing a metal illm on a support-in an evacuated chamber comprising the steps of vaporizing the metal and heating the vapor in its passage from its source to the support.
  • Apparatus for depositing a metal lm on a support in an evacuated chamber comprising means for vaporizing the metal, a tubular member interposed between the source of the vapor and the support, means for heating the tubular member to a temperature above the vaporization temperature oi' the metal and means for supplying into the tubular member a gas inert to the metal, the walls of the tubular member being porous to the gas. the rate ot introduction of the gas being so low that the vaporization temperature of the'metal is not substantially increased by reason of rise of pressure in the chamber;
  • Process of depositing ametal illm on a support in an evacuated chamber comprising the steps of embodying the metal to be deposited in a comparatively large portion of another metal, having, at the pressure inthe chamber, a. vapor pressure low in comparison with that of the metal to be deposited, heating the combined mass of metal to vaporize the metal to be deposited, and without appreciably vaporizing the other metal, heating the vapor in its passage from its source to the support.
  • Apparatus i'or depositing a metal lm on a support in an evacuated chamber, comprising f means for heating the gas.
  • Apparatus as in claim 18, comprising two electrodes and means for producing an electric discharge between them adapted to ionize the gas in the chamber.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)
US105091A 1935-10-12 1936-10-10 Deposition of metallic films from metal vaporized in vacuo Expired - Lifetime US2100045A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE483029X 1935-10-12

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US2100045A true US2100045A (en) 1937-11-23

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US (1) US2100045A (de)
BE (1) BE417869A (de)
FR (1) FR811756A (de)
GB (1) GB483029A (de)
NL (1) NL46111C (de)

Cited By (31)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2416211A (en) * 1943-09-15 1947-02-18 American Optical Corp Apparatus for coating articles
US2420722A (en) * 1942-12-11 1947-05-20 Bausch & Lomb Apparatus for coating surfaces
US2426377A (en) * 1943-12-07 1947-08-26 Ruben Samuel Selenium rectifier and method of making
US2440135A (en) * 1944-08-04 1948-04-20 Alexander Paul Method of and apparatus for depositing substances by thermal evaporation in vacuum chambers
US2447789A (en) * 1945-03-23 1948-08-24 Polaroid Corp Evaporating crucible for coating apparatus
US2463765A (en) * 1943-04-27 1949-03-08 Hunt A H Ltd Manufacture of electrical condensers
US2469929A (en) * 1943-09-24 1949-05-10 American Optical Corp Apparatus for coating articles
US2479541A (en) * 1942-12-29 1949-08-16 American Optical Corp Apparatus for treating surfaces
US2557530A (en) * 1946-09-07 1951-06-19 Eastman Kodak Co Electric heating element
US2772318A (en) * 1952-12-31 1956-11-27 Holland Leslie Arthur Apparatus for vaporization of metals and metalloids
US2793609A (en) * 1953-01-26 1957-05-28 British Dielectric Res Ltd Means for the deposition of materials by evaporation in a vacuum
US2850225A (en) * 1955-11-10 1958-09-02 Wisconsin Alumni Res Found Pump
US2864332A (en) * 1957-09-06 1958-12-16 Raymond F Woolley Crystal plating apparatus
US2894679A (en) * 1953-11-23 1959-07-14 Wisconsin Alumni Res Found Pump
US2910766A (en) * 1953-02-24 1959-11-03 Pritikin Nathan Method of producing an electrical component
US2917814A (en) * 1952-06-07 1959-12-22 John G Ruckelshaus Resistance time measuring devices
US2962393A (en) * 1953-04-21 1960-11-29 John G Ruckelshaus Method of preparing electrical resistors
US2998376A (en) * 1956-10-29 1961-08-29 Temescal Metallurgical Corp High-vacuum evaporator
US3117210A (en) * 1959-07-13 1964-01-07 Wisconsin Alumni Res Found Apparatus for evaporating materials
US3405251A (en) * 1966-05-31 1968-10-08 Trw Inc Vacuum evaporation source
US3540993A (en) * 1965-12-17 1970-11-17 Euratom Sputtering apparatus
US3795783A (en) * 1968-06-26 1974-03-05 Glaverbel Apparatus for surface coating articles
US3824039A (en) * 1971-03-24 1974-07-16 British Oxygen Co Ltd Sublimable targets
US3894926A (en) * 1973-02-09 1975-07-15 Lee Jau Yien In-out transporter for an enclosed chamber
US3999039A (en) * 1973-12-22 1976-12-21 Flachglas Aktiengesellschaft Delog-Detag Resistance heated vaporizer
EP0132322A2 (de) * 1983-06-29 1985-01-30 Stauffer Chemical Company Thermische Crack-Anlage zur Herstellung von Pnictidfilmen in Hochvakuumverfahren
EP0152668A2 (de) * 1984-02-17 1985-08-28 Stauffer Chemical Company Verfahren zur Hochvakuumbeschichtung mittels einer Vorrichtung zur kontinuierlichen Zuführung von Pnictid
US4725510A (en) * 1980-12-24 1988-02-16 U.S. Philips Corporation Source for vapor-depositing manganese
EP2431493A1 (de) * 2010-09-17 2012-03-21 Princo Corp. Verdampfungsboot zur Vakuumdampfablagerung und Vakuumdampf-Ablagerungssystem
CN102409296A (zh) * 2010-09-20 2012-04-11 巨擘科技股份有限公司 真空蒸镀用镀材舟及真空蒸镀系统
WO2023011733A1 (en) * 2021-08-06 2023-02-09 MAX-PLANCK-Gesellschaft zur Förderung der Wissenschaften e.V. Method of operating an evaporation system, deflection device, and evaporation system

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
IT380674A (de) * 1939-02-22
DE748945C (de) * 1940-12-24 1944-12-02 Verfahren zum Aufdampfen von duennen Schichten
US2433922A (en) * 1942-10-15 1948-01-06 American Optical Corp Apparatus for treating surfaces
US2479540A (en) * 1942-12-29 1949-08-16 American Optical Corp Method of coating by vacuum distillation
DE970970C (de) * 1943-02-09 1958-11-20 Heraeus Gmbh W C Einrichtung zum Herstellen von Oberflaechenschichten durch Verdampfen oder Sublimieren des UEberzugsstoffes im Hochvakuum
DE1046437B (de) * 1953-10-15 1958-12-11 Physikalisch Tech Werkstaetten Verfahren zum Verdampfen chemischer Verbindungen
DE1149113B (de) * 1958-06-16 1963-05-22 Western Electric Co Verfahren zur Herstellung eines nichtelektrolytischen Kondensators mit Metalloxyddielektrikum
US3104178A (en) * 1960-12-23 1963-09-17 Ibm Evaporative coating method

Cited By (33)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2420722A (en) * 1942-12-11 1947-05-20 Bausch & Lomb Apparatus for coating surfaces
US2479541A (en) * 1942-12-29 1949-08-16 American Optical Corp Apparatus for treating surfaces
US2463765A (en) * 1943-04-27 1949-03-08 Hunt A H Ltd Manufacture of electrical condensers
US2416211A (en) * 1943-09-15 1947-02-18 American Optical Corp Apparatus for coating articles
US2469929A (en) * 1943-09-24 1949-05-10 American Optical Corp Apparatus for coating articles
US2426377A (en) * 1943-12-07 1947-08-26 Ruben Samuel Selenium rectifier and method of making
US2440135A (en) * 1944-08-04 1948-04-20 Alexander Paul Method of and apparatus for depositing substances by thermal evaporation in vacuum chambers
US2447789A (en) * 1945-03-23 1948-08-24 Polaroid Corp Evaporating crucible for coating apparatus
US2557530A (en) * 1946-09-07 1951-06-19 Eastman Kodak Co Electric heating element
US2917814A (en) * 1952-06-07 1959-12-22 John G Ruckelshaus Resistance time measuring devices
US2772318A (en) * 1952-12-31 1956-11-27 Holland Leslie Arthur Apparatus for vaporization of metals and metalloids
US2793609A (en) * 1953-01-26 1957-05-28 British Dielectric Res Ltd Means for the deposition of materials by evaporation in a vacuum
US2910766A (en) * 1953-02-24 1959-11-03 Pritikin Nathan Method of producing an electrical component
US2962393A (en) * 1953-04-21 1960-11-29 John G Ruckelshaus Method of preparing electrical resistors
US2894679A (en) * 1953-11-23 1959-07-14 Wisconsin Alumni Res Found Pump
US2850225A (en) * 1955-11-10 1958-09-02 Wisconsin Alumni Res Found Pump
US2998376A (en) * 1956-10-29 1961-08-29 Temescal Metallurgical Corp High-vacuum evaporator
US2864332A (en) * 1957-09-06 1958-12-16 Raymond F Woolley Crystal plating apparatus
US3117210A (en) * 1959-07-13 1964-01-07 Wisconsin Alumni Res Found Apparatus for evaporating materials
US3540993A (en) * 1965-12-17 1970-11-17 Euratom Sputtering apparatus
US3405251A (en) * 1966-05-31 1968-10-08 Trw Inc Vacuum evaporation source
US3795783A (en) * 1968-06-26 1974-03-05 Glaverbel Apparatus for surface coating articles
US3824039A (en) * 1971-03-24 1974-07-16 British Oxygen Co Ltd Sublimable targets
US3894926A (en) * 1973-02-09 1975-07-15 Lee Jau Yien In-out transporter for an enclosed chamber
US3999039A (en) * 1973-12-22 1976-12-21 Flachglas Aktiengesellschaft Delog-Detag Resistance heated vaporizer
US4725510A (en) * 1980-12-24 1988-02-16 U.S. Philips Corporation Source for vapor-depositing manganese
EP0132322A2 (de) * 1983-06-29 1985-01-30 Stauffer Chemical Company Thermische Crack-Anlage zur Herstellung von Pnictidfilmen in Hochvakuumverfahren
EP0132322A3 (de) * 1983-06-29 1986-06-11 Stauffer Chemical Company Thermische Crack-Anlage zur Herstellung von Pnictidfilmen in Hochvakuumverfahren
EP0152668A2 (de) * 1984-02-17 1985-08-28 Stauffer Chemical Company Verfahren zur Hochvakuumbeschichtung mittels einer Vorrichtung zur kontinuierlichen Zuführung von Pnictid
EP0152668A3 (de) * 1984-02-17 1986-06-25 Stauffer Chemical Company Verfahren zur Hochvakuumbeschichtung mittels einer Vorrichtung zur kontinuierlichen Zuführung von Pnictid
EP2431493A1 (de) * 2010-09-17 2012-03-21 Princo Corp. Verdampfungsboot zur Vakuumdampfablagerung und Vakuumdampf-Ablagerungssystem
CN102409296A (zh) * 2010-09-20 2012-04-11 巨擘科技股份有限公司 真空蒸镀用镀材舟及真空蒸镀系统
WO2023011733A1 (en) * 2021-08-06 2023-02-09 MAX-PLANCK-Gesellschaft zur Förderung der Wissenschaften e.V. Method of operating an evaporation system, deflection device, and evaporation system

Also Published As

Publication number Publication date
GB483029A (en) 1938-04-11
BE417869A (de)
NL46111C (de)
FR811756A (fr) 1937-04-22

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