WO2003095698A2 - Dispositif et procede de metallisation sous vide par faisceau electronique de couches formees de maniere reactive sur des substrats - Google Patents

Dispositif et procede de metallisation sous vide par faisceau electronique de couches formees de maniere reactive sur des substrats Download PDF

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Publication number
WO2003095698A2
WO2003095698A2 PCT/DE2003/001524 DE0301524W WO03095698A2 WO 2003095698 A2 WO2003095698 A2 WO 2003095698A2 DE 0301524 W DE0301524 W DE 0301524W WO 03095698 A2 WO03095698 A2 WO 03095698A2
Authority
WO
WIPO (PCT)
Prior art keywords
substrate
reactive gas
electron beam
shield
supplied
Prior art date
Application number
PCT/DE2003/001524
Other languages
German (de)
English (en)
Other versions
WO2003095698A3 (fr
Inventor
Otmar Zimmer
Peter Siemroth
Bernd Schultrich
Steffen Schenk
Ulf Seyfert
Christian Hecht
Ekkehart Reinhold
Bernd Schuhmacher
Original Assignee
Fraunhofer-Gesellschaft Zur Förderung Der Angewan Dten Forschung E.V.
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
Priority claimed from DE10228925A external-priority patent/DE10228925B4/de
Application filed by Fraunhofer-Gesellschaft Zur Förderung Der Angewan Dten Forschung E.V. filed Critical Fraunhofer-Gesellschaft Zur Förderung Der Angewan Dten Forschung E.V.
Priority to AU2003239759A priority Critical patent/AU2003239759A1/en
Publication of WO2003095698A2 publication Critical patent/WO2003095698A2/fr
Publication of WO2003095698A3 publication Critical patent/WO2003095698A3/fr

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Classifications

    • 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
    • C23C14/0021Reactive sputtering or evaporation
    • 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
    • C23C14/28Vacuum evaporation by wave energy or particle radiation
    • C23C14/30Vacuum evaporation by wave energy or particle radiation by electron bombardment

Definitions

  • the invention relates to a device and a method for electron beam vapor deposition of reactively formed layers on substrates in a vacuum, coatings on the surfaces of substrates as e.g. Oxides, nitrides, carbides but also carbonitrides etc. can be trained.
  • evaporation is e.g. of a metal within a vacuum chamber using electron beams, with which the respective metal can be heated, melted and subsequently evaporated, is known per se.
  • Such an evaporation process can usually be carried out at internal pressures in vacuum chambers of approximately 0.01 to 0.1 Pa.
  • layer application rates of several ⁇ m / s can be achieved, the particle energy of the metal vapor generated with the electron beam being below 1 eV.
  • the interaction between metal vapor and electron beam is negligible.
  • the layers thus formed from the pure metal on substrates have a porous and stem-like structure.
  • the increased partial pressure also has the effect that the particle energies of the atoms contained in the steam are additionally reduced by impacts, and the porosity (increase) and adhesive strength (reduction) of the coating formed on the substrate surface are also adversely affected.
  • a crucible containing metal is arranged within a separate inner chamber in a vacuum chamber and an electron beam is directed through an opening to form a metal vapor on the metal surface.
  • an increased beam power in particular a high acceleration voltage, is accordingly required.
  • Such an electron beam source must be operated with acceleration voltages that are above 30 kV.
  • this object is achieved with a device having the features of claim 1 and a method with the features of claim 13.
  • Advantageous embodiments and developments of the invention can be achieved with the features mentioned in the subordinate claims.
  • the device according to the invention for electron beam vapor deposition of reactively formed layers on substrates uses a crucible containing the respective chemical element within a vacuum chamber. With an electron beam source present on the vacuum chamber, an electron beam can vaporize the chemical element onto the surface be directed within the crucible.
  • a shield is provided between the crucible containing the chemical element and the substrate in which an aperture for the steam directed onto the substrate is formed.
  • this shield and the substrate on which the reactively formed coating is to be formed there is at least one additional element which is suitable for the excitation, dissociation and / or ionization of a reactive gas used in each case.
  • Both the at least one gas inlet for the reactive gas and the at least one element for activating, dissociating and / or ionizing the reactive gas are arranged within areas protected from vapor deposition, by appropriate design of the shield and the design and arrangement of the aperture. With such an arrangement, the at least one additional element is not directly influenced by the interactions of the reactive gas with the vapor formed.
  • a gas mixture can also be supplied through the at least one gas inlet for reactive gas, which also contains inert gas in addition to reactive gas.
  • reactive gas which also contains inert gas in addition to reactive gas.
  • inert gas can also be supplied separately, an inert gas supply also being able to be arranged in front of the shielding, that is to say inside the vacuum chamber, and the inert gas can be supplied, for example, into the area of influence of the electron beam and / or into the vapor formed.
  • the excitation, dissociation and / or ionization of the respective reactive gas is achieved with the at least one element by appropriate energy supply. This can be achieved by means of electrical discharges, microwave discharges or also by means of electromagnetic fields formed.
  • the one or more elements can be designed as corresponding electrodes, coils but also as antennas.
  • the reactive gas can be activated, for example, by arc, glow and / or hollow cathode discharges, and the one or more element (s) can accordingly be designed accordingly.
  • one or more electrodes can be used, to which a direct voltage positive relative to the electrical potential of the vacuum chamber is connected.
  • it can be one or more ring electrodes that are formed around the respective aperture opening.
  • the diaphragm opening can be designed as a slit diaphragm, preferably with a rectangular or square cross section.
  • the reactive gas supplied should be passed through the hollow cathode.
  • a suitable inert gas is, for example, argon.
  • the diaphragm opening should be designed and the diaphragm opening and the at least one element should be arranged in such a way that steam cannot impinge directly on the one or more correspondingly used element (s), i.e. a linear movement of Steam particles, starting from the crucible to one or more element (s), are not possible.
  • the supply of the required reactive gas can be significantly reduced with the invention and the reactive layer formation can be carried out at partial pressures which are 0,1 0.15 Pa, preferably also 0,1 0.1 Pa.
  • the electron beam source can be operated with significantly lower power and with acceleration voltages below 20 kv.
  • different coatings can be formed from different reactively formed, for example metal, compounds on surfaces of substrates. In addition to metals, other chemical elements such as silicon or boron can also be used.
  • the reactive gas supplied can thus be pure oxygen for the formation of oxide layers, but also pure nitrogen for the formation of nitride layers.
  • hydrocarbon compounds can be used, which preferably have a relatively low binding energy, so that a reactive carbide layer or carbonitride layer can be produced after the at least partial splitting.
  • ammonia as a correspondingly suitable reactive gas, which can be split up accordingly, to form nitride layers.
  • hydrogen-containing compounds as reactive gas, the released hydrogen can be easily removed from the vacuum chamber by means of the already existing vacuum pump.
  • the volume flow of the reactive gas supplied can be controlled or regulated.
  • the power of a microwave generator can also be regulated or controlled.
  • the respective power of the electron beam source can also be influenced accordingly.
  • a suitable sensor e.g. optically by means of an emission spectroscope.
  • a further advantageous possibility of exerting influence is that a favorable electrical potential can also be applied to the substrate, on the surface of which the corresponding coating is to be formed.
  • a corresponding positive or negative electrical voltage which may also take into account the plasma-relevant parameters, can be connected, so that the layer formation rate and the quality of the coating formed can be additionally improved.
  • the invention can also be used to maintain defined and reproducible conditions when carrying out the coating process.
  • the influence desired according to the invention is limited to a certain range which is favorable for the process.
  • the evaporation process, especially the electron beam, remains largely unaffected by this.
  • the solution according to the invention can be used in the case of substrates moved translationally through a vacuum chamber to form surface layers.
  • a corresponding rotation of a substrate within a vacuum chamber is also possible.
  • Figure 1 shows an example of a device according to the invention in schematic form.
  • FIG. 1 shows an example of a device according to the invention in schematic form.
  • a crucible 7 is arranged within a vacuum chamber; in which a metal is contained as chemical element 8.
  • an electron beam source 10 which is present on the vacuum chamber, an electron beam 11 directed to the surface of the chemical element 8, for example a metal, and steam 9 formed by corresponding energy input, which, as indicated by the arrow, is led to the substrate 4 to be coated.
  • a shield 3 is arranged between the crucible 7 containing the chemical element 8 and the substrate 4, which in this example can be passed through a vacuum chamber as indicated by the horizontally oriented arrow.
  • this shield 3 an aperture 6 is formed, on which in this example a funnel-shaped inlet for the steam 9 is additionally present.
  • the shield 3 forms part of a reaction chamber, the remaining part of the reaction chamber being essentially formed by the substrate 4.
  • the shield 3 as a whole as a reaction chamber, in which the respective substrate to be coated can then be accommodated.
  • the electrode 1 which in this example is designed as a ring electrode around the aperture.
  • this ring electrode 1 as an element, a ne excitation, dissociation and / or ionization of a reactive gas supplied through the gas inlet 5 can be achieved, so that the reactivity between the respective steam 9 and the respective reactive gas or an elementary component of such a reactive gas within zone 2 is increased.
  • two or more electrodes can also be arranged separately in accordance with one another.
  • titanium is used as the chemical element 8 within the crucible 7.
  • the vacuum chamber is evacuated to a pressure of 10 -3 Pa.
  • nitrogen is fed in via the gas inlet 5 until a partial pressure of 0.08 Pa has been reached in the region between the shield 3 and the substrate 4, and is stabilized to this partial pressure by means of an appropriate control system.
  • the electron beam source 10 is operated with an acceleration voltage of 16 kV.
  • a direct voltage of 60 V is applied to the electrode 1, which is positive with respect to the electrical potential within the vacuum chamber and in particular the electrical potential that is present at the crucible 7.
  • a discharge current of a few 100 A is established at the electrode 1 and the electrical voltage during this discharge is approximately 40 to 50 V.
  • the respective layer thickness can be influenced by the corresponding speed at which the substrate is moved through the vacuum 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)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Physical Vapour Deposition (AREA)
  • Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)

Abstract

L'invention concerne un dispositif et un procédé de métallisation sous vide par faisceau électronique de couches formées de manière réactive sur des substrats. Il est prévu, selon l'invention, comparativement à des solutions classiques, d'augmenter le rendement et d'améliorer la qualité des couches formées de manière réactive. A cet effet, il est prévu dans une chambre à vide, un creuset contenant un élément chimique, un substrat à traiter, ainsi qu'une source de faisceau électronique, au niveau de la chambre à vide. Il est prévu, entre le creuset contenant l'élément chimique et le substrat, un blindage avec une ouverture d'obturateur à travers laquelle la vapeur formée peut parvenir jusqu'au substrat. Le blindage protège à cet effet au moins un élément pour activer, dissocier et/ou ioniser un gaz réactif, introduit par l'intermédiaire d'au moins un orifice d'admission de gaz disposée de manière protégée entre le substrat et le blindage.
PCT/DE2003/001524 2002-05-10 2003-05-07 Dispositif et procede de metallisation sous vide par faisceau electronique de couches formees de maniere reactive sur des substrats WO2003095698A2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU2003239759A AU2003239759A1 (en) 2002-05-10 2003-05-07 Device and method for the electron beam attenuation of reactively formed layers on substrates

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE10221816 2002-05-10
DE10221816.1 2002-05-10
DE10228925A DE10228925B4 (de) 2002-05-10 2002-06-25 Vorrichtung und Verfahren zum Elektronenstrahlaufdampfen von reaktiv gebildeten Schichten auf Substraten
DE10228925.5 2002-06-25

Publications (2)

Publication Number Publication Date
WO2003095698A2 true WO2003095698A2 (fr) 2003-11-20
WO2003095698A3 WO2003095698A3 (fr) 2004-04-29

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PCT/DE2003/001524 WO2003095698A2 (fr) 2002-05-10 2003-05-07 Dispositif et procede de metallisation sous vide par faisceau electronique de couches formees de maniere reactive sur des substrats

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AU (1) AU2003239759A1 (fr)
WO (1) WO2003095698A2 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7595098B2 (en) * 2003-04-03 2009-09-29 Microemissive Displays Limited Method and apparatus for depositing material on a substrate
WO2019096391A1 (fr) * 2017-11-16 2019-05-23 Applied Materials, Inc. Procédé et appareil pour le dépôt en phase vapeur d'une couche isolante d'oxyde métallique sur un substrat

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5227203A (en) * 1992-02-24 1993-07-13 Nkk Corporation Ion-plating method and apparatus therefor
EP0650159A1 (fr) * 1993-10-20 1995-04-26 Matsushita Electric Industrial Co., Ltd. Procédé de fabrication d'un support d'enregistrement magnétique

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH089776B2 (ja) * 1990-11-27 1996-01-31 日本鋼管株式会社 イオンプレーティング方法および装置
JPH0737666B2 (ja) * 1991-01-28 1995-04-26 株式会社日本製鋼所 化合物薄膜の形成方法及び装置

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5227203A (en) * 1992-02-24 1993-07-13 Nkk Corporation Ion-plating method and apparatus therefor
EP0650159A1 (fr) * 1993-10-20 1995-04-26 Matsushita Electric Industrial Co., Ltd. Procédé de fabrication d'un support d'enregistrement magnétique

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
PATENT ABSTRACTS OF JAPAN Bd. 016, Nr. 512 (C-0998), 22. Oktober 1992 (1992-10-22) & JP 04 191364 A (NKK CORP), 9. Juli 1992 (1992-07-09) *
PATENT ABSTRACTS OF JAPAN Bd. 017, Nr. 025 (C-1017), 18. Januar 1993 (1993-01-18) & JP 04 246168 A (JAPAN STEEL WORKS LTD:THE), 2. September 1992 (1992-09-02) *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7595098B2 (en) * 2003-04-03 2009-09-29 Microemissive Displays Limited Method and apparatus for depositing material on a substrate
WO2019096391A1 (fr) * 2017-11-16 2019-05-23 Applied Materials, Inc. Procédé et appareil pour le dépôt en phase vapeur d'une couche isolante d'oxyde métallique sur un substrat

Also Published As

Publication number Publication date
AU2003239759A1 (en) 2003-11-11
WO2003095698A3 (fr) 2004-04-29
AU2003239759A8 (en) 2003-11-11

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