US3927638A - Vacuum evaporation plating apparatus - Google Patents

Vacuum evaporation plating apparatus Download PDF

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Publication number
US3927638A
US3927638A US459955A US45995574A US3927638A US 3927638 A US3927638 A US 3927638A US 459955 A US459955 A US 459955A US 45995574 A US45995574 A US 45995574A US 3927638 A US3927638 A US 3927638A
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United States
Prior art keywords
heating
deposit
photosensitive
heating means
tellurium
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Expired - Lifetime
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US459955A
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English (en)
Inventor
Fukumatsu Sakaue
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Fujifilm Business Innovation Corp
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Fuji Xerox Co Ltd
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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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0623—Sulfides, selenides or tellurides
    • 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
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
    • G03G5/00—Recording members for original recording by exposure, e.g. to light, to heat, to electrons; Manufacture thereof; Selection of materials therefor
    • G03G5/02—Charge-receiving layers
    • G03G5/04—Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor
    • G03G5/08—Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor characterised by the photoconductive material being inorganic
    • G03G5/082—Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor characterised by the photoconductive material being inorganic and not being incorporated in a bonding material, e.g. vacuum deposited

Definitions

  • FIG. 1 A first figure.
  • the vacuum evaporation process of this invention is I represented by those processes where a certain substance is evaporated in a vacuum and the vapor thus generated is condensed on a base plate, this basic process being extensively used in many fields.
  • This apparatus typically includes an evaporator capable of being electrically heated and loaded with substance to be evaporated. The evaporator is heated, and the heat thus generated is transmitted to the substance, to thus effectuate the desired evaporation.
  • the conventional evaporation apparatus may be unsatisfactory for depositing semiconductor films or other layers which are adversely affected by the composition of the deposited film, since, when evaporating a substance which is subject to fractional distillation when evaporated, like an alloy, the distribution of the composition of the deposited film thus obtained may lack desired uniformity.
  • the apparatus of FIG. 1 includes a tank 1, the interior of which is made vacuous to approximately 10 Torr by vacuum apparatus 2.
  • An evaporator 3 is loaded with a sensitizer 4, which may be 10% Te 90% Se (Te is tellurium, Se is selenium, and is percent by weight as used here and hereafter).
  • the evaporator 3 is electrically heated by a power source 5, the temperature of which is controlled to thus evaporate sensitizer 4.
  • the vapor thus generated is deposited on a base 8 comprising an aluminum plate positioned onv a base heating device 7, which is electrically heated from a power source 6.
  • the sensitizer'4 is thus evaporated to obtain a sensitive plate for electrophotography, the deposited film having a distribution of Te in the direction of thickness as shown in FIG. 2.
  • a satisfactory photosensitive plate for electrophotography should have a density of Te on the surface of or less; therefore, a photosensitive plate having Te distributed as shown in FIG. 2 has quite limited usefulness.
  • the surface of the plate is subject to abrasion with attendant roughening thereof. This in turn, varies the characteristics of the photosensitive plate at the surface thereof and thus lessens the usefulness of the plate.
  • a primary purpose of this invention is to provide an evaporation plating method and apparatus for optionally controlling, to a certain extent, the fractional distillation of a substance subject to fractional distillation when evaporated.
  • FIG. 1 is a schematic view of the general construction of a conventional vacuum evaporation plating apparatus.
  • FIG. 3 is a schematic view of the general construction of an illustrative vacuum evaporation plating apparatus in accordance with the present invention. 1
  • FIG. 4 is a side elevation of an illustrative evaporator which may be used in the apparatus of FIG. 3;
  • FIG. 7 is a side elevation of another illustrative evap-' orator which may be used in the apparatus of FIG. 3.
  • FIGS. 2, 5 and 6 are graphs illustrating the distribution of Te in the direction of thickness of deposited film;
  • FIG. 2 illustrating the film deposited by the conventional vacuum evaporation plating apparatus of FIG. 1, and
  • FIGS. 5 and 6 respectively illustrating the films deposited by the embodiment of FIG. 4.
  • tank 11 has the interior thereof rendered vacuous to approximately 10* Torr, for example, by a vacuum apparatus 12.
  • the tank 11 has a baseboard heating device 14 which is heated from an electric power source 13 and kept at a certain level of temperature.
  • device 14 is positioned in the upper section of tank 1, and is provided with a base plate 15.
  • Tank 1 1 has an evaporator 17 typically made of stainless steel plate 0.8mm thick.
  • the evaporator has a tubular shape as shown in the side elevation of FIG. 4 and is approximately positioned at the center of tank 11.
  • the evaporator contains an evaporant or substance 18 to be deposited.
  • An upper heater 19 heats the substance 18 by radiation and is positioned in the upper section of evaporator 17.
  • a lower heater 20 heats the bottom section of the evaporator and is positioned in the lower section thereof.
  • a shielding plate 21 typically made of a tantalum ribbon keeps substance 18 from spattering out of evaporator 17 and keeps heat radiation from upper heater 19 from adversely affecting the base plate 15. Plate 21 is positioned between the opening 16 of evaporator 17 and upper heater 19.
  • a reflecting plate 22 with an open upper section is positioned around lower heater 20 to reflect heat generated by lower heater 20 over the bottom section of the evaporator.
  • the ratings of upper heater 19 and lower heater 20 are typically 200V AC and lKW, these heaters being respectively controlled by power source 23 and power source 24.
  • Power sources 23 and 24 are placed in operation by switches 25 and 26 respectively.
  • EXPERIMENT l 30 g of 10% Te Q Se was employed as substance 18 and the interior of tank 11 was made vacuous to 10 Torr.
  • the temperature of base plate 15 was set at the I 60C and the space between base plate and opening 16 of evaporator 17 was set to approximately 15cm.
  • the lower heater then had 150V applied thereto for two minutes.
  • Switch 26 of the lower heater was turned ofi and switch of upper heater 19 was turned on.
  • the upper heater 19 had 150V applied thereto for two minutes whereby all of substance 18 was evaporated and a deposited film of approximately 100p. was formed on base plate 15.
  • the distribution of Te in the direction of thickness of the deposited film is illustrated in FIG. 5. The distribution was determined by quantitative analysis with an XMA (X-ray micro analyser).
  • the lower heater 20 was first energized for three minutes and then turned off.
  • Upper heater 19 was then energized for one and a half minutes and then turned off.
  • the lower heater 20 was first energized for four minutes and then turned off.
  • Upper heater 19 was then energized for one and a half minutes and then turned off.
  • the evaporator 17 was heated from the bottom section by lower heater 20; however, an evaporator 31 (see FIG. 7) may comprise a resistant substance so that evaporator 31 itself has an electric current passed therethrough, whereby substance 18 is heated from within.
  • lower heater 20 is not necessary.
  • the vacuum evaporation apparatus of the present invention includes an evaporator having a heat source for heating by radiation the evaporation surface of an evaporant together with a heat source for heating the evaporant either from within or from the bottom portion thereof so that fractional distillation of the evaporant can be controlled to thereby control the distribution of the film constituents in the direction of thickness of the deposited film.
  • the composition of the deposited film in the direction of the thickness thereof can be kept virtually constant in a certain range of thickness by the proper selection and use of both of the aforesaid heat sources. It should also be appreciated that both the heat sources may be operated at the same time or heat source 19 prior to heat source 20 in order to effect the advantageous results of this invention.
  • the surface composition thereof may be kept virtually free of undesired variations so that the deposited film hasa long life with the initial characteristics thereof maintained intact over its useful life.
  • the vacuum evaporation plating apparatus of the present invention can be manufactured at low cost, due to the simple construction thereof, and evaporation can be controlled in accordance with an established program. Further, due to the low level of calorific capacity of the apparatus as a whole, the operational performance is also considerably improved.
  • a vacuum evaporation plating apparatus for controlling fractional distillation of respective components of a photosensitive material, said apparatus comprising a single container for said photosensitive material;
  • a first heating means for heating with radiation the evaporating surface of the photosensitive material, said first heating means being disposed above said material such that said electromagnetic radiations impinge directly on said evaporating surface;
  • a second heating means for heating the photosensitive material from either the interior or bottom thereof;
  • said first and second heating means controlling the deposition of said components to control the relative percentages of said components in the photosensitive film deposit through the thickness thereof.
  • Apparatus as in claim 1 including means for activating said second heating means and then said first heating means.
  • photosensitive material is 10% by weight tellurium and by weight selenium, the thickness of said deposit on the receiving means being at least p. and the percentage of tellurium near the surface of said deposit being less than 25%.
  • Apparatus for vacuum-evaporating a multi-element photosensitive material having at least first and second elements where said first element evaporates less readily than said second element said apparatus comprising a single container for said multi-element material;
  • first heating means including a heating element for radiating continuous wave electromagnetic radiations onto the evaporating surface of said material to evaporate the material, said first heating means being disposed above said material such that said electromagnetic radiations impinge directly on said evaporating surface;
  • Apparatus as in claim 4 including reflecting means for preventing the radiation of said heating element from directly reaching the receiving means upon which the film deposit forms, said first and second heating means controlling the deposition of said first and second elements to control the relative percentages of said elements in the photosensitive film deposit through the thickness thereof.
  • said heating element extending longitudinally in said containing means over said multi-element material and said reflecting means extending longitudinally in said containing means between said opening and said heating element.

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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)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Physical Vapour Deposition (AREA)
  • Photoreceptors In Electrophotography (AREA)
US459955A 1973-06-04 1974-04-11 Vacuum evaporation plating apparatus Expired - Lifetime US3927638A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP48061799A JPS5234039B2 (enrdf_load_stackoverflow) 1973-06-04 1973-06-04

Publications (1)

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US3927638A true US3927638A (en) 1975-12-23

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US459955A Expired - Lifetime US3927638A (en) 1973-06-04 1974-04-11 Vacuum evaporation plating apparatus

Country Status (5)

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US (1) US3927638A (enrdf_load_stackoverflow)
JP (1) JPS5234039B2 (enrdf_load_stackoverflow)
DE (1) DE2426687A1 (enrdf_load_stackoverflow)
FR (1) FR2232077B1 (enrdf_load_stackoverflow)
NL (1) NL7407523A (enrdf_load_stackoverflow)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3331653A1 (de) * 1982-09-04 1984-03-08 Konishiroku Photo Industry Co., Ltd., Tokyo Behaelter mit dampfquelle
DE4133615A1 (de) * 1990-10-12 1992-04-16 Custom Metalliz Serv Inc Verdampfungsquelle fuer die vakuum-metallisierung
US6337105B1 (en) * 1997-07-14 2002-01-08 Matsushita Electric Industrial Co., Ltd. Method and apparatus for forming thin functional film
US20060153986A1 (en) * 2005-01-07 2006-07-13 Hitoshi Yamamoto Evaporation method and apparatus using infrared guiding heater
US20060162663A1 (en) * 2003-07-04 2006-07-27 Verreyken Guido Vapor deposition apparatus
EP1978563A3 (en) * 2007-03-23 2012-10-24 FUJIFILM Corporation Radiation detector and method for producing photoconductive layer for recording thereof
US20130160712A1 (en) * 2010-09-01 2013-06-27 Sharp Kabushiki Kaisha Evaporation cell and vacuum deposition system the same
US20230062455A1 (en) * 2021-09-01 2023-03-02 Entegris, Inc. Vaporizer assembly

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6286155A (ja) * 1985-10-11 1987-04-20 Mitsubishi Electric Corp 溶融物質の蒸気噴出装置
DE4104415C1 (enrdf_load_stackoverflow) * 1991-02-14 1992-06-04 4P Verpackungen Ronsberg Gmbh, 8951 Ronsberg, De
JP4593008B2 (ja) * 2001-05-23 2010-12-08 キヤノンアネルバ株式会社 蒸着源並びにそれを用いた薄膜形成方法及び形成装置

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3057282A (en) * 1959-04-06 1962-10-09 Eastman Kodak Co Fluid treating device for sheet or strip materials
US3515852A (en) * 1967-08-10 1970-06-02 Sylvania Electric Prod Metal-evaporating source
US3519479A (en) * 1965-12-16 1970-07-07 Matsushita Electronics Corp Method of manufacturing semiconductor device
US3634647A (en) * 1967-07-14 1972-01-11 Ernest Brock Dale Jr Evaporation of multicomponent alloys
US3655429A (en) * 1969-04-16 1972-04-11 Westinghouse Electric Corp Method of forming thin insulating films particularly for piezoelectric transducers

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3057282A (en) * 1959-04-06 1962-10-09 Eastman Kodak Co Fluid treating device for sheet or strip materials
US3519479A (en) * 1965-12-16 1970-07-07 Matsushita Electronics Corp Method of manufacturing semiconductor device
US3634647A (en) * 1967-07-14 1972-01-11 Ernest Brock Dale Jr Evaporation of multicomponent alloys
US3515852A (en) * 1967-08-10 1970-06-02 Sylvania Electric Prod Metal-evaporating source
US3655429A (en) * 1969-04-16 1972-04-11 Westinghouse Electric Corp Method of forming thin insulating films particularly for piezoelectric transducers

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3331653A1 (de) * 1982-09-04 1984-03-08 Konishiroku Photo Industry Co., Ltd., Tokyo Behaelter mit dampfquelle
DE4133615A1 (de) * 1990-10-12 1992-04-16 Custom Metalliz Serv Inc Verdampfungsquelle fuer die vakuum-metallisierung
US6337105B1 (en) * 1997-07-14 2002-01-08 Matsushita Electric Industrial Co., Ltd. Method and apparatus for forming thin functional film
US20060162663A1 (en) * 2003-07-04 2006-07-27 Verreyken Guido Vapor deposition apparatus
US20060153986A1 (en) * 2005-01-07 2006-07-13 Hitoshi Yamamoto Evaporation method and apparatus using infrared guiding heater
WO2006073965A3 (en) * 2005-01-07 2006-11-23 Universal Display Corp Evaporation method and apparatus using infrared guiding heater
US7431807B2 (en) 2005-01-07 2008-10-07 Universal Display Corporation Evaporation method using infrared guiding heater
EP1978563A3 (en) * 2007-03-23 2012-10-24 FUJIFILM Corporation Radiation detector and method for producing photoconductive layer for recording thereof
US20130160712A1 (en) * 2010-09-01 2013-06-27 Sharp Kabushiki Kaisha Evaporation cell and vacuum deposition system the same
US20230062455A1 (en) * 2021-09-01 2023-03-02 Entegris, Inc. Vaporizer assembly

Also Published As

Publication number Publication date
JPS5010288A (enrdf_load_stackoverflow) 1975-02-01
FR2232077B1 (enrdf_load_stackoverflow) 1977-03-11
FR2232077A1 (enrdf_load_stackoverflow) 1974-12-27
DE2426687A1 (de) 1974-12-19
JPS5234039B2 (enrdf_load_stackoverflow) 1977-09-01
NL7407523A (enrdf_load_stackoverflow) 1974-12-06

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