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WO1996012389A1 - Appareil destine a deposer une couche de matiere sur un substrat - Google Patents

Appareil destine a deposer une couche de matiere sur un substrat Download PDF

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Publication number
WO1996012389A1
WO1996012389A1 PCT/US1995/013585 US9513585W WO9612389A1 WO 1996012389 A1 WO1996012389 A1 WO 1996012389A1 US 9513585 W US9513585 W US 9513585W WO 9612389 A1 WO9612389 A1 WO 9612389A1
Authority
WO
WIPO (PCT)
Prior art keywords
laser beam
target
target material
plume
travel
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.)
Ceased
Application number
PCT/US1995/013585
Other languages
English (en)
Other versions
WO1996012389A9 (fr
Inventor
Laxminarayana Ganapathi
Steven E. Giles
Rama Rao
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Educational Data Systems Inc
Original Assignee
Educational Data Systems Inc
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Educational Data Systems Inc filed Critical Educational Data Systems Inc
Priority to AU41948/96A priority Critical patent/AU4194896A/en
Publication of WO1996012389A1 publication Critical patent/WO1996012389A1/fr
Publication of WO1996012389A9 publication Critical patent/WO1996012389A9/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • 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
    • C23C14/0605—Carbon
    • 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
    • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating

Definitions

  • This invention relates to an apparatus for depositing a layer of material on a substrate, in particular, a layer such as hard diamond-like material comprising carbon and/or carbon bonded to any one or more species of boron, nitrogen or hydroge .
  • Diamond and "diamond-like" materials are of particular interest for use as protective coatings because these materials have a hardness of 10 or nearly 10 compared with sapphire's hardness of 9. Diamond, while harder than sapphire, is far more expensive, and thus its use has been limited.
  • PLD pulsed laser deposition
  • U.S. Patent No. 4,987,007 to Wagal et al. discloses one method of depositing DLC films using PLD.
  • An accelerating grid spaced from a graphite target is charged to a negative potential and is used to separate carbon ions from a plume.
  • the grid is charged to an opposite potential than the carbon ions so as to attract the ions.
  • the Wagal et al. patent suggests that a higher growth rate and a quality film may be achieved by using a higher energy laser than is disclosed in the Wagal et al. patent. These higher energy lasers are costly, however.
  • a method and apparatus for depositing high quality coatings of conventional and new materials on a substrate by a pulsed laser deposition process that includes the capacitive coupling of energy.
  • the apparatus in accordance with the present innovation includes a pulsed evaporation means such as a pulsed electron/ion beam or a pulsed laser beam directed to impinge on a solid carbon target. When properly focused, these pulsed sources provide very high power at the focal point, evaporating the carbon or carbon composite and forming a plume.
  • a capacitor stationed outside the vacuum chamber is discharged through a graphite ring placed between the target and the substrate. The energy stored in the capacitor is released in synchronization with the pulsed evaporation source and is applied to the plume. The energy coupled to the material plume is given by 1
  • C is the capacitance value of the external capacitor and V is the voltage to which it is charged.
  • V is the voltage to which it is charged.
  • C the capacitance value of the external capacitor
  • RC the time constant RC
  • Fig. 1 is a diagrammatic view of the augmented pulsed laser disposition apparatus of the present invention
  • Fig. 2 is detailed illustration of the scanning device used in the present invention.
  • Fig. 3 illustrates the placement of the ring electrode and its relation to the target and lens of the present invention
  • Fig. 4 is a graph comparing the absorption spectra of a sapphire sample with a diamond-like coating produced with the apparatus of the present invention, and a sapphire sample without the coating;
  • Fig. 5 is a graph comparing the absorption spectra of a thicker sapphire sample with a diamond-like coating produced with the apparatus of the present invention, and a sapphire sample without the coating;
  • Fig. 6A-6B are graphs of the transmission of sapphire with and without the diamond-like coating.
  • Fig. l illustrates the preferred embodiment of the augmented pulsed laser deposition apparatus of the present invention.
  • a vacuum chamber 1 is provided, preferably sustaining a pressure of 10"*Torr.
  • a pulsed laser 2 preferably a pulsed Q-switched Nd:YAG laser Surelite 11-10 model from Continuum, is positioned outside the vacuum chamber 1, and emits a pulsed beam 3.
  • a source producing a pulsed electron/ion beam may be used.
  • the pulsed beam 3 enters an optical device 4, such as a cross post adaptor from Newport, model CA-1, which prevents the formation of an elliptical focused spot at the carbon target 12.
  • the beam then enters the vacuum chamber through a quartz window 5 mounted to a feedthrough collar 6. Once the laser beam 3 has entered the vacuum chamber
  • a mirror 7a shown in Fig. 2
  • the scanning device 10 contains a lens 8, such as a CVI PLCX-25-4/773-UV- AR/AR1064, to focus the laser beam 3 and a ring electrode 9.
  • the focused laser beam 11 emerges from the scanning device and strikes a high purity carbon target 12 which may be obtained from Goodfellow.
  • the lens 8 is positioned in the laser beam to assure that a minimum focused spot of the laser beam strikes the face of the carbon target 12. Striking the carbon target with the laser beam 11 causes carbon vaporization and forms a plume of material 18.
  • the plume of vaporized material 18 created by the laser pulse emerges from the carbon target 12 at normal incidence to the f ce of the target 12. Material including carbon atoms and ions pass from the face of the carbon target 12, through the ring electrode 9 and collect on the substrate 19 with the ring electrode 9 applying energy to the plume 18.
  • a high voltage power supply 13 External to the vacuum chamber l is a high voltage power supply 13 connected in parallel to a high voltage capacitor 14 and charging the capacitor 14 to a voltage in the range of 0.5-3.0KV.
  • the capacitor 14, preferably 0.1-0.5 ⁇ f, is connected in series between the carbon target 12 and ring electrode 9 by high voltage feedthroughs 15 and flexible conductors 16. The polarity of the ring electrode 9 is maintained at positive high voltage while the carbon target 12 is negative in polarity.
  • the capacitor 14 discharges the instant the plume 18 is formed during a laser pulse since the plume 18, in effect, completes the circuit and provides a path for the capacitor 14 to discharge.
  • no special trigger circuitry is needed due to the manner in which the circuit elements are arranged.
  • the resulting discharge of energy into the plume 18 increases ionization and dramatically increases the diameter of the plume and area of the film that can be deposited.
  • the additional energy from the capacitor 14 excites carbon atoms to much higher energy states than if the capacitor 14 was not used. This results in uniform, large area films with improved adherence to the substrate 19.
  • the capacitive augmentation reduces the need for higher power lasers and hence the associated cost.
  • the power density present in the focused spot of the laser beam can severely erode the carbon target 12 in a short period of time. Not only is the carbon target 12 damaged but the quality of the DLC film can be compromised as well.
  • a method and apparatus that moves the carbon target 12 and simultaneously scans the laser beam 11 thus changing the location on the carbon target 12 where the laser beam 11 is focused has been devised as a solution to this problem.
  • the carbon target 12 is moved horizontally using a motorized linear actuator 17, such as a model VF-165-2 from Huntington Mechanical Lab, mounted to the feedthrough collar 6 and extending into the chamber 1_.
  • the carbon target 12, mounted at the end of the linear actuator 17, moves in the direction indicated by the arrow Al.
  • Damage to the carbon target 12 is further reduced by a scanning device 10 that moves the focused laser beam vertically. Details of the scanning device 10 are shown in Fig. 2 & 3.
  • the laser beam 3 enters the chamber via a quartz window 5 and is turned 90 degrees by a stationary mirror 7a, such as a CVI Yl-1025-45, fixed to the chamber baseplate 20.
  • a second mirror 7b such as a CVI Yl- 1025-45, redirects the laser beam so that it passes through the lens 8.
  • the mirror 7b, ring electrode 9 and lens 8 are mounted on a bracket 21 that is attached to the shaft of a second motorized linear actuator 22 fixed to the chamber baseplate 20. As the motorized linear actuator 22 is operated, the distance between mirrors 7a and 7b changes depending on the direction of motion of the actuator 22. This results in a corresponding change in the position of the focused laser beam 11 emerging from the scanning device 7.
  • Fig. 3 shows a top view of scanning device 10 in more detail.
  • the combined motion of both linear actuators results in the focused laser beam 11 scanning the carbon target 12 in a raster pattern.
  • the focused laser beam 11 is constantly moved via scanning device 10 while the carbon target 12 is periodically advanced as the laser beam 11 reaches its lowest or highest point of travel.
  • the continuously moving plume 18 created by the capacitively augmented PLD yields hard, uniform DLC films on substrates of large areas.
  • Figs. 4 and 5 graphically compare the absorption spectrum of a sapphire sample coated using the apparatus of the present invention with that of an uncoated sapphire sample.
  • curve 2 1/8 inch sapphire sample is illustrated.
  • the uncoated sapphire sample spectrum (curve 1) exhibits an absorption peak at approximately 200nm, however the remaining portions of the spectrum covering the UV-visible region show the uncoated sapphire is near transparent, exhibiting only approximately 5% absorption.
  • the spectrum of the coated sapphire sample (curve 2) exhibits substantially similar absorption characteristics. The approximately 5% difference between the two spectra (curve 1 and curve 2) at 250nm decreases as the wavelength is increased, with the difference at 900nm being negligible.
  • Fig. 5 illustrates the spectrum of an uncoated 1/4 inch sapphire sample (curve 1) as compared to the spectrum of an coated sapphire sample of the same thickness (curve 2) .
  • Curve 1 and curve 2 show heavy absorption near the 200nm end of the spectrum.
  • the coated sample (curve 2) absorbs approximately 5% more than does the uncoated sample (curve 1) .
  • the difference between the two absorption spectra decreases until it is negligible at 900nm.
  • Fig. 6A and 6B show the transmission, as measured in a spectrometer, of sapphire one-eight inch thick samples.
  • Fig. 6A graphically illustrates the transmission of an uncoated sample
  • Fig. 6B illustrates the transmission of a sample coated with a 50A thick diamond-like coating produced with the method and apparatus of the present invention.
  • the coating has no measurable effect of the transmission of the sapphire in the entire spectrum.
  • Both spectra show a drop in transmission with the longer wavelengths, but this is intrinsic to sapphire.
  • a diamond-like coating produced with the method and apparatus of the present invention is transparent to wavelengths in the ranges of 250-900nm and 2500-10,OOOnm.

Landscapes

  • 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)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

Appareil et procédé destiné au dépôt, sur de la céramique, du verre et du plastique, de couche lisses, amorphes ou microcristallines, présentant la dureté du diamant et assurant une protection contre les agressions chimiques et l'abrasion. Dans une chambre à vide (1), un laser pulsé (2) dirige un faisceau (3) à travers le dispositif optique (4), la fenêtre (5), et la lentille (8), avec ses miroirs (7a, b), du dispositif de balayage (10) positionnant le faisceau focalisé (11) sur la cible carbone (12) pour produire un panache (18) de substance vaporisée. Les couches sont produites par augmentation du panache au moyen d'un circuit à condensateurs (13, 14, 15, 16). Une électrode annulaire (9) et la cible permettent de coupler au panache l'énergie stockée dans un condensateur, lequel couplage est synchrone avec le processus de dépôt par laser pulsé. L'augmentation du panache accroît d'une part l'énergie et l'ionisation de l'espèce de dépôt, et favorise d'autre part l'élargissement de la zone de panache jusqu'à ce qu'elle coïncide avec la zone du substrat (19) où doit être déposé le film. Un moteur linéaire (17) permet de positionner exactement la cible, ce qui, associé au dispositif de balayage, évite d'endommager la cible.
PCT/US1995/013585 1994-10-18 1995-10-18 Appareil destine a deposer une couche de matiere sur un substrat Ceased WO1996012389A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU41948/96A AU4194896A (en) 1994-10-18 1995-10-18 Apparatus for depositing a layer of material on a substrate

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US32489494A 1994-10-18 1994-10-18
US324,894 1994-10-18

Publications (2)

Publication Number Publication Date
WO1996012389A1 true WO1996012389A1 (fr) 1996-04-25
WO1996012389A9 WO1996012389A9 (fr) 1996-10-10

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Country Link
AU (1) AU4194896A (fr)
WO (1) WO1996012389A1 (fr)

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7134381B2 (en) 2003-08-21 2006-11-14 Nissan Motor Co., Ltd. Refrigerant compressor and friction control process therefor
US7146956B2 (en) 2003-08-08 2006-12-12 Nissan Motor Co., Ltd. Valve train for internal combustion engine
US7228786B2 (en) 2003-06-06 2007-06-12 Nissan Motor Co., Ltd. Engine piston-pin sliding structure
US7255083B2 (en) 2002-10-16 2007-08-14 Nissan Motor Co., Ltd. Sliding structure for automotive engine
US7273655B2 (en) 1999-04-09 2007-09-25 Shojiro Miyake Slidably movable member and method of producing same
US7284525B2 (en) 2003-08-13 2007-10-23 Nissan Motor Co., Ltd. Structure for connecting piston to crankshaft
US7318514B2 (en) 2003-08-22 2008-01-15 Nissan Motor Co., Ltd. Low-friction sliding member in transmission, and transmission oil therefor
US7322749B2 (en) 2002-11-06 2008-01-29 Nissan Motor Co., Ltd. Low-friction sliding mechanism
US7406940B2 (en) 2003-05-23 2008-08-05 Nissan Motor Co., Ltd. Piston for internal combustion engine
US7458585B2 (en) 2003-08-08 2008-12-02 Nissan Motor Co., Ltd. Sliding member and production process thereof
US7500472B2 (en) 2003-04-15 2009-03-10 Nissan Motor Co., Ltd. Fuel injection valve
US7572200B2 (en) 2003-08-13 2009-08-11 Nissan Motor Co., Ltd. Chain drive system
US7771821B2 (en) 2003-08-21 2010-08-10 Nissan Motor Co., Ltd. Low-friction sliding member and low-friction sliding mechanism using same
US8096205B2 (en) 2003-07-31 2012-01-17 Nissan Motor Co., Ltd. Gear
WO2023072543A1 (fr) * 2021-10-28 2023-05-04 Joachim Richter Systeme und Maschinen GmbH & Co. KG Dispositif et procédé permettant de produire une couche de graphène

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4370176A (en) * 1980-02-01 1983-01-25 Commissariat A L'energie Atomique Process for fast droping of semiconductors
US4664940A (en) * 1983-03-07 1987-05-12 Marcel Bensoussan Process for the formation of a flux of atoms and its use in an atomic beam epitaxy process
US4701592A (en) * 1980-11-17 1987-10-20 Rockwell International Corporation Laser assisted deposition and annealing
US4762975A (en) * 1984-02-06 1988-08-09 Phrasor Scientific, Incorporated Method and apparatus for making submicrom powders
USH872H (en) * 1987-09-15 1991-01-01 The United States Of America As Represented By The Department Of Energy Method of applying coatings to substrates
US4987007A (en) * 1988-04-18 1991-01-22 Board Of Regents, The University Of Texas System Method and apparatus for producing a layer of material from a laser ion source
US5084300A (en) * 1989-05-02 1992-01-28 Forschungszentrum Julich Gmbh Apparatus for the ablation of material from a target and coating method and apparatus
US5098737A (en) * 1988-04-18 1992-03-24 Board Of Regents The University Of Texas System Amorphic diamond material produced by laser plasma deposition
US5203929A (en) * 1990-07-24 1993-04-20 Toyota Jidosha Kabushiki Kaisha Method of producing amorphous magnetic film
US5300485A (en) * 1990-03-02 1994-04-05 Samitomo Electric Industries, Ltd. Method of preparing oxide superconducting films by laser ablation
US5330968A (en) * 1991-06-12 1994-07-19 Sumitomo Electric Industries, Ltd. Laser ablation process for preparing oxide superconducting thin films

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4370176A (en) * 1980-02-01 1983-01-25 Commissariat A L'energie Atomique Process for fast droping of semiconductors
US4701592A (en) * 1980-11-17 1987-10-20 Rockwell International Corporation Laser assisted deposition and annealing
US4664940A (en) * 1983-03-07 1987-05-12 Marcel Bensoussan Process for the formation of a flux of atoms and its use in an atomic beam epitaxy process
US4762975A (en) * 1984-02-06 1988-08-09 Phrasor Scientific, Incorporated Method and apparatus for making submicrom powders
USH872H (en) * 1987-09-15 1991-01-01 The United States Of America As Represented By The Department Of Energy Method of applying coatings to substrates
US4987007A (en) * 1988-04-18 1991-01-22 Board Of Regents, The University Of Texas System Method and apparatus for producing a layer of material from a laser ion source
US5098737A (en) * 1988-04-18 1992-03-24 Board Of Regents The University Of Texas System Amorphic diamond material produced by laser plasma deposition
US5084300A (en) * 1989-05-02 1992-01-28 Forschungszentrum Julich Gmbh Apparatus for the ablation of material from a target and coating method and apparatus
US5300485A (en) * 1990-03-02 1994-04-05 Samitomo Electric Industries, Ltd. Method of preparing oxide superconducting films by laser ablation
US5203929A (en) * 1990-07-24 1993-04-20 Toyota Jidosha Kabushiki Kaisha Method of producing amorphous magnetic film
US5330968A (en) * 1991-06-12 1994-07-19 Sumitomo Electric Industries, Ltd. Laser ablation process for preparing oxide superconducting thin films

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7273655B2 (en) 1999-04-09 2007-09-25 Shojiro Miyake Slidably movable member and method of producing same
US7255083B2 (en) 2002-10-16 2007-08-14 Nissan Motor Co., Ltd. Sliding structure for automotive engine
US7322749B2 (en) 2002-11-06 2008-01-29 Nissan Motor Co., Ltd. Low-friction sliding mechanism
US8152377B2 (en) 2002-11-06 2012-04-10 Nissan Motor Co., Ltd. Low-friction sliding mechanism
US7500472B2 (en) 2003-04-15 2009-03-10 Nissan Motor Co., Ltd. Fuel injection valve
US7406940B2 (en) 2003-05-23 2008-08-05 Nissan Motor Co., Ltd. Piston for internal combustion engine
US7228786B2 (en) 2003-06-06 2007-06-12 Nissan Motor Co., Ltd. Engine piston-pin sliding structure
US8096205B2 (en) 2003-07-31 2012-01-17 Nissan Motor Co., Ltd. Gear
US7458585B2 (en) 2003-08-08 2008-12-02 Nissan Motor Co., Ltd. Sliding member and production process thereof
US7146956B2 (en) 2003-08-08 2006-12-12 Nissan Motor Co., Ltd. Valve train for internal combustion engine
US7284525B2 (en) 2003-08-13 2007-10-23 Nissan Motor Co., Ltd. Structure for connecting piston to crankshaft
US7572200B2 (en) 2003-08-13 2009-08-11 Nissan Motor Co., Ltd. Chain drive system
US7134381B2 (en) 2003-08-21 2006-11-14 Nissan Motor Co., Ltd. Refrigerant compressor and friction control process therefor
US7771821B2 (en) 2003-08-21 2010-08-10 Nissan Motor Co., Ltd. Low-friction sliding member and low-friction sliding mechanism using same
US7318514B2 (en) 2003-08-22 2008-01-15 Nissan Motor Co., Ltd. Low-friction sliding member in transmission, and transmission oil therefor
WO2023072543A1 (fr) * 2021-10-28 2023-05-04 Joachim Richter Systeme und Maschinen GmbH & Co. KG Dispositif et procédé permettant de produire une couche de graphène

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Publication number Publication date
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