US3925187A - Apparatus for the formation of coatings on a substratum - Google Patents

Apparatus for the formation of coatings on a substratum Download PDF

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Publication number
US3925187A
US3925187A US236609A US23660972A US3925187A US 3925187 A US3925187 A US 3925187A US 236609 A US236609 A US 236609A US 23660972 A US23660972 A US 23660972A US 3925187 A US3925187 A US 3925187A
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Prior art keywords
substratum
target
targets
chamber
ions
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US236609A
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English (en)
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Jacques Leon Bernard
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Centre National dEtudes Spatiales CNES
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Centre National dEtudes Spatiales CNES
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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
    • C23C14/34—Sputtering
    • C23C14/46—Sputtering by ion beam produced by an external ion source

Definitions

  • An intermediate chamber, located at the exit of the duoplasmatron, may be fed with a reacting gas [58] Field of Search 204/l92, 298, 118/491 (Oxygen, nitrogen, etc.) in Order to obtain compound [56] References Cited coatings (oxides, nitrides, etc.).
  • the present invention is concerned with a process and an apparatus for the formation of coatings, and especially of thin layers, on a substratum.
  • Thin layers are generally obtained by known processes such as the so-called cathodic sputtering process in which a target, made of the coating material, is striked by high speed particles, the atoms of ejected material being collected on the suitably located substratum, which is generally placed in front of the target and even parallel to it.
  • a thermionic cathode emits electrons which ionize by collision the atoms of an inert gas, such as argon, and the positive argon ions fall upon the target, brought to a high negative potential, so as to eject its constitutive material and coat the substratum as indicated.
  • an inert gas such as argon
  • the drawback of this known process is the presence of an appreciable residual pressure to 10' torr) while the thin layer is being built up, and the persistence of a certain amount of plasma around the target and the substratum, which lowers the working efficiency in the layer formation.
  • this layer may be contaminated by the plasma ions which, while the discharge is established, impinge against the walls of the enclosure.
  • the ions striking the target are focussed into a beam directed and accelerated towards the target, under a vacuum of more than 10" torr (and preferably comprised between 10 and 10" torr), which eliminates the above-mentioned drawback.
  • An object of the invention is to develop an apparatus and a process for building up multiple layers on a substratum, e.g., for the manufacture of semi-conductors, in one single operation during which the vacuum is practically maintained at the same value, indicated above, whereas, in the prior art, the vacuum had to be released, and a manipulation undertaken, after the building up of every individual layer.
  • Another object of the invention is to develop an apparatus and a process for obtaining easily some coatings made up of several layers of chemical compounds, such as oxides, nitrides, sulfides, etc., by introducing gases, reacting with the target, at a suitable and specially adapted point of the apparatus.
  • chemical compounds such as oxides, nitrides, sulfides, etc.
  • FIG. 1 shows the envelope 1 of an evacuated enclosure inside which a vacuum of 10 10 torr is maintained by a pumping system (not shown) connected at 2.
  • This source of ions comprises an oxide-coated cathode 3c, activated by Joule effect by means of heating filaments 4 and 5, and an anode 3A, maintained at a positive potential of 500 V with respect to the cathode, and at a negative potential, adjustable between 5 kV and 30 k ⁇ /, with respect to ground.
  • a highly ionized plasma is built up at the anode level; the ions making up this plasma are picked up by the grounded suck-in electrode 6 located in front and close to the outlet of the ion source.
  • the atoms ejected from target 7 are collected on a substratum 8 where they build up a thin layer.
  • target 7 is perpendicular to the path of the beam and carried by a support 9 cooled by water circulating through pipes 10.
  • substratum 8 will advantageously be fixed on a heater capable of maintaining temperatures of about 550C during the building up of the thin layer.
  • the ions produced by source 3 are generally those of an inert gas, such as argon, introduced into the enclosure 3 by means of a suitable device 11 in the form of a capillary tube called a microleak connection.
  • a reactive gas such as oxygen, nitrogen, hydrogen sulfide or carbon dioxide (or even carbon monoxide), may also be resorted to, so as to build up a thin layer of oxide, nitride, sulfide or carbide on the substratum.
  • the outlet of the plasmatron is equipped with an inserted part, called pre-chamber 12, in which said reactive gas is introduced through a conduit 13.
  • pre-chamber 12 an inserted part, called pre-chamber 12, in which said reactive gas is introduced through a conduit 13.
  • concentration of ions in the impinging beam and therefore, stoichiometry of the layers may be varied.
  • the target may be a circular one, of about 10 cm diameter, when the diameter of the ion beam will be 5 cm at the level of the target.
  • a rotating diaphragm l4 protects the substratum during the ejection of the first atom layers of the target.
  • Enclosure 1 is connected in 2 to an oil diffusion pumping unit, for instance, (not shown), through an optically tight trap, cooled by liquid nitrogen.
  • the target is made of high purity tantalum (99.999 Ta).
  • the gases introduced during the discharge have the following purity level argon (99.9995 Ar); nitrogen (99.995% N oxygen (99.998% 0
  • the connections joining the gas containers with the source of ions 3 are very short and made of copper.
  • the atomizing or sputtering efficiency will be defined by the ratio of the number of impinging ions to the number of atoms ejected from the target.
  • the number of impinging ions is determined by an accurate computation of the ionic current read from a cylinder of Faraday substituted to the target.
  • the number of tantalum atoms ejected is computed from the loss of weight of the target. In order to give this computation a sufficient accuracy, the bombardment is sustained for three hours and the loss of weight of the target, in this case, averages 50 mg, the accuracy of the measurement being within O.l mg.
  • the efficiency of tantalum sputtering with argon ions is given by the formula S 0.147 (Am/It) it being supposed that the argon ions were only charged with:
  • the speed of growing of the layer is 1,800 A/ hour, which permits to accurately control its thickness.
  • Tantalum is deposited on a pyrex substratum, optically polished and previously degassed by heating at 550C for 1 hour. Before the deposition, the target is submitted to a preparatory sputtering by the beam of argon ions to eliminate all superficially absorbed gases.
  • the residual pressure inside the enclosure is less than 10" torr.
  • the layers obtained are strongly adherent to the substratum and show no cavities.
  • the layer is amorphous if the temperature of the substratum is less than 200C;
  • the layer is well crystallised in the isometric phase (face-centered cubes) if the temperature of the substratum is more than 250C.
  • the electric resistance of the tantalum layer is measured, during the deposition, by means of two copper contacts previously applied on the substratum.
  • the thickness of the layers is measured by means of a so called talistep" device.
  • the layers that were obtained showed a thickness of about 6,000 A. ln the case of the isometric phase, i.e., for temperatures of substratum between 250C and 550C, the influence of temperature on resistivity, measured at room temperature, is small.
  • the values of resistivity were found to be comprised between 28 and 32 microhm/cm at C.
  • the coefficient of resistance was measured between room temperature and 250C.
  • the influence of the temperature of the substratum on the temperature factor is small if the layer is well crystallized in the isometric phase.
  • the coefficient of resistance is 2,200 ppm. by degree C.
  • FIG. 2 shows another embodiment of the invention giving still better results.
  • Target 7 is inclined, preferably by to 45", on the axis of the ion beam, and this arrangement improves considerably the efficiency of sputtering.
  • the substratum 8 is carried by a turntable, rotated by means (not shown) outside enclosure 1. This arrangement enables to deposit several thin layers in one and the same apparatus without interrupting the vacuum.
  • a multilayer i.e., a laminate made of several different layers superimposed, may be obtained in one operation, without penetration of air in the enclosure after completion of each individual layer, as it is the case when the targets are changed from the outside.
  • FIG. 3 This is achieved by means of an apparatus according to FIG. 3, in which several (here two) targets 15 made of different materials, are mounted within the apparatus on a common support 17.
  • the ion beam is directed on the selected target in order to build up a layer of coating on substratum 8, then another target is brought into position, in the place of the first, by rotating support 7 by outside means, so as to build up another layer of different composition without interrupting the vacuum.
  • the apparatus according to the invention is very versatile and particularly suitable for the manufacture of thin and pure layers, of accurately controllable composition and easy to duplicate, which are especially useful in the microelectronics field. Any target of either semiconducting or insulating material may be disintegrated and deposited with this apparatus.
  • Apparatus for forming a thin coating of material on a substratum including an enclosure which will withstand a high vacuum, said enclosure being partitioned into a first chamber containing a duoplasmatron, an intermediate chamber and a third chamber, said duoplasmatron including activation means for delivery of ions and inlet means for feeding said duoplasmatron with gas, the intermediate chamber being positioned so as to allow the transit therethrough of ions from said duoplasmatron into said third chamber, said third chamber containing a target device, a substratum device, and a set of ion focusing electrodes for directing the ions entering said third chamber to said target whose ejected particles are deposited onto said substratum, and means for supplying from a gas source a gas capable of reacting with the material of said target and a small passage for connecting said gas source with said intermediate chamber so as to introduce a small amount of reacting gas into said intermediate chamber.
  • the target means comprises several distinct targets of different materials, each associated with support means for carrying said targets, said apparatus also comprising mechanical means for altering the relative position of the ion beam and of said support means to thereby selectively bring said beam into impingement with any one of said targets.
  • Apparatus according to claim 3 in which the rotating support comprises a cooling system passing through the axis of the rotating support for cooling conjointly all the targets.
  • said substratum device comprises several distinct means for supporting substrata, a turntable for carrying said substrata and driving means for revolving said turntable, which is capable of being operated from the outside of the apparatus.

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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)
  • Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)
US236609A 1971-03-25 1972-03-21 Apparatus for the formation of coatings on a substratum Expired - Lifetime US3925187A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR7110598A FR2129996B1 (enrdf_load_stackoverflow) 1971-03-25 1971-03-25

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USB236609I5 USB236609I5 (enrdf_load_stackoverflow) 1975-01-28
US3925187A true US3925187A (en) 1975-12-09

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4199448A (en) * 1976-06-09 1980-04-22 The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration Reverse osmosis membrane of high urea rejection properties
US4305801A (en) * 1980-04-16 1981-12-15 The United States Of America As Represented By The United States Department Of Energy Line-of-sight deposition method
US4346123A (en) * 1979-08-02 1982-08-24 Balzers Aktiengesellschaft Method of depositing hard wear-resistant coatings on substrates
US4508049A (en) * 1978-11-02 1985-04-02 Siemens Aktiengesellschaft Method and a device for the production of electrical components, in particular laminated capacitors
USRE32849E (en) * 1978-04-13 1989-01-31 Litton Systems, Inc. Method for fabricating multi-layer optical films
WO1989004382A1 (en) * 1987-11-02 1989-05-18 Jens Christiansen Process and device for producing thin layers of a material which melts or sublimes at high temperatures on a substrate
US4994164A (en) * 1987-08-05 1991-02-19 U.S. Philips Corporation Metal ion implantation apparatus
US5087478A (en) * 1989-08-01 1992-02-11 Hughes Aircraft Company Deposition method and apparatus using plasma discharge
US5250327A (en) * 1986-04-28 1993-10-05 Nissin Electric Co. Ltd. Composite substrate and process for producing the same
GB2321063A (en) * 1997-01-08 1998-07-15 Oxford Plasma Technology Ltd Reactive particle beam sputtering
US5855950A (en) * 1996-12-30 1999-01-05 Implant Sciences Corporation Method for growing an alumina surface on orthopaedic implant components
US6348113B1 (en) * 1998-11-25 2002-02-19 Cabot Corporation High purity tantalum, products containing the same, and methods of making the same
US6413380B1 (en) 2000-08-14 2002-07-02 International Business Machines Corporation Method and apparatus for providing deposited layer structures and articles so produced
US20070209741A1 (en) * 2006-03-07 2007-09-13 Carpenter Craig M Methods of producing deformed metal articles

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3939052A (en) 1975-01-15 1976-02-17 Riley Leon H Depositing optical fibers
CH611938A5 (enrdf_load_stackoverflow) * 1976-05-19 1979-06-29 Battelle Memorial Institute
US4142958A (en) * 1978-04-13 1979-03-06 Litton Systems, Inc. Method for fabricating multi-layer optical films
US5601652A (en) * 1989-08-03 1997-02-11 United Technologies Corporation Apparatus for applying ceramic coatings

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3408283A (en) * 1966-09-15 1968-10-29 Kennecott Copper Corp High current duoplasmatron having an apertured anode positioned in the low pressure region
US3409529A (en) * 1967-07-07 1968-11-05 Kennecott Copper Corp High current duoplasmatron having an apertured anode comprising a metal of high magnetic permeability
US3472751A (en) * 1965-06-16 1969-10-14 Ion Physics Corp Method and apparatus for forming deposits on a substrate by cathode sputtering using a focussed ion beam
US3484358A (en) * 1966-09-01 1969-12-16 Bell Telephone Labor Inc Method and apparatus for reactive sputtering wherein the sputtering target is contacted by an inert gas
US3576729A (en) * 1967-06-05 1971-04-27 Smiths Industries Ltd Sputtering methods and apparatus

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3472751A (en) * 1965-06-16 1969-10-14 Ion Physics Corp Method and apparatus for forming deposits on a substrate by cathode sputtering using a focussed ion beam
US3484358A (en) * 1966-09-01 1969-12-16 Bell Telephone Labor Inc Method and apparatus for reactive sputtering wherein the sputtering target is contacted by an inert gas
US3408283A (en) * 1966-09-15 1968-10-29 Kennecott Copper Corp High current duoplasmatron having an apertured anode positioned in the low pressure region
US3576729A (en) * 1967-06-05 1971-04-27 Smiths Industries Ltd Sputtering methods and apparatus
US3409529A (en) * 1967-07-07 1968-11-05 Kennecott Copper Corp High current duoplasmatron having an apertured anode comprising a metal of high magnetic permeability

Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4199448A (en) * 1976-06-09 1980-04-22 The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration Reverse osmosis membrane of high urea rejection properties
USRE32849E (en) * 1978-04-13 1989-01-31 Litton Systems, Inc. Method for fabricating multi-layer optical films
US4508049A (en) * 1978-11-02 1985-04-02 Siemens Aktiengesellschaft Method and a device for the production of electrical components, in particular laminated capacitors
US4346123A (en) * 1979-08-02 1982-08-24 Balzers Aktiengesellschaft Method of depositing hard wear-resistant coatings on substrates
US4305801A (en) * 1980-04-16 1981-12-15 The United States Of America As Represented By The United States Department Of Energy Line-of-sight deposition method
US5250327A (en) * 1986-04-28 1993-10-05 Nissin Electric Co. Ltd. Composite substrate and process for producing the same
US4994164A (en) * 1987-08-05 1991-02-19 U.S. Philips Corporation Metal ion implantation apparatus
WO1989004382A1 (en) * 1987-11-02 1989-05-18 Jens Christiansen Process and device for producing thin layers of a material which melts or sublimes at high temperatures on a substrate
US5087478A (en) * 1989-08-01 1992-02-11 Hughes Aircraft Company Deposition method and apparatus using plasma discharge
US5855950A (en) * 1996-12-30 1999-01-05 Implant Sciences Corporation Method for growing an alumina surface on orthopaedic implant components
GB2321063A (en) * 1997-01-08 1998-07-15 Oxford Plasma Technology Ltd Reactive particle beam sputtering
US6348113B1 (en) * 1998-11-25 2002-02-19 Cabot Corporation High purity tantalum, products containing the same, and methods of making the same
US20030168131A1 (en) * 1998-11-25 2003-09-11 Michaluk Christopher A. High purity tantalum, products containing the same, and methods of making the same
US6893513B2 (en) * 1998-11-25 2005-05-17 Cabot Corporation High purity tantalum, products containing the same, and methods of making the same
US7431782B2 (en) 1998-11-25 2008-10-07 Cabot Corporation High purity tantalum, products containing the same, and methods of making the same
US7585380B2 (en) 1998-11-25 2009-09-08 Cabot Corporation High purity tantalum, products containing the same, and methods of making the same
US6413380B1 (en) 2000-08-14 2002-07-02 International Business Machines Corporation Method and apparatus for providing deposited layer structures and articles so produced
US20070209741A1 (en) * 2006-03-07 2007-09-13 Carpenter Craig M Methods of producing deformed metal articles
US8382920B2 (en) 2006-03-07 2013-02-26 Global Advanced Metals, Usa, Inc. Methods of producing deformed metal articles
US8974611B2 (en) 2006-03-07 2015-03-10 Global Advanced Metals, Usa, Inc. Methods of producing deformed metal articles

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FR2129996B1 (enrdf_load_stackoverflow) 1975-01-17
USB236609I5 (enrdf_load_stackoverflow) 1975-01-28
FR2129996A1 (enrdf_load_stackoverflow) 1972-11-03

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