EP1899499B1 - Procede pour produire sur un substrat une couche presentant des nanoparticules - Google Patents

Procede pour produire sur un substrat une couche presentant des nanoparticules Download PDF

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Publication number
EP1899499B1
EP1899499B1 EP06777538A EP06777538A EP1899499B1 EP 1899499 B1 EP1899499 B1 EP 1899499B1 EP 06777538 A EP06777538 A EP 06777538A EP 06777538 A EP06777538 A EP 06777538A EP 1899499 B1 EP1899499 B1 EP 1899499B1
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EP
European Patent Office
Prior art keywords
process chamber
nanoparticles
substrate
nanoparticle
stream
Prior art date
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EP06777538A
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German (de)
English (en)
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EP1899499A1 (fr
Inventor
Rene Jabado
Ursus KRÜGER
Daniel Körtvelyessy
Volkmar LÜTHEN
Ralph Reiche
Michael Rindler
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Siemens AG
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Siemens AG
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Publication of EP1899499A1 publication Critical patent/EP1899499A1/fr
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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
    • C23C24/00—Coating starting from inorganic powder
    • 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
    • C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00

Definitions

  • the invention relates to a method having the features according to the preamble of claim 1.
  • nanoparticles are understood as meaning particles having a particle size of less than one micrometer. Nanoparticles have - in contrast to the same material without nanoparticle structure - sometimes very extraordinary properties. This is due to the fact that the surface-to-volume ratio of nanoparticles is particularly high; For example, even with spherical nanoparticles consisting of one hundred atoms, over fifty atoms are O-surface atoms. The resulting high reactivity of the nanoparticles offers the possibility of aligning materials more specifically than otherwise possible to the respective intended use. For example, nanoparticles are used as coating materials. A general technical overview of nanotechnology is available, for example, from the website of the German Physikalisch-Technische Bundesweg.
  • the Japanese abstract 06128728A discloses a method of depositing a film of superfine particles.
  • the method uses a storage chamber in which the superfine particles move to the bottom of the chamber due to gravity, creating a concentration gradient. From the storage chamber, the particles pass to a coating chamber in which the particles are directed onto a substrate to be coated.
  • EP-A-441300 discloses a method and an apparatus for producing a nanoparticle-comprising layer, wherein nanoparticles are passed from a first process chamber into a second process chamber laterally over the surface of a substrate.
  • US-2004/0121084 A1 discloses a method and apparatus wherein nanoparticles are directed from a first process chamber into a second process chamber and thus deposited on a substrate.
  • GB-A-932923 discloses a method and apparatus for forming a coating on a substrate wherein very finely divided powder is passed and deposited in parallel across the surface of a substrate.
  • DE-19935053 A1 discloses a method and apparatus wherein ultrafine particles are deposited on a substrate and irradiated, activated and reacted with a high energy beam.
  • the invention has for its object to provide a method for producing a nanoparticle-containing layer, which can be particularly simple to perform and yet offers a very large margin in the design and composition of the layer to be produced.
  • the invention provides that in a first process chamber nanoparticles are released and a nanoparticle flow is generated.
  • the nanoparticle stream is passed into a second process chamber, and the nanoparticles are deposited on a substrate in the second process chamber.
  • the nanoparticle current is conducted laterally, in particular parallel, over the surface of the substrate and the nanoparticles are deposited on the surface of the substrate with the thus-directed nanoparticle current.
  • a significant advantage of the method according to the invention is the fact that the production or release of the nanoparticles takes place spatially separated from the deposition of the nanoparticles on the substrate. Even before the deposition process, the nanoparticles are thus completely finished-preferably in the solid state of matter-and are merely incorporated into the layer to be produced on the substrate.
  • the formation of the nanoparticles is spatially separate from the deposition of the nanoparticles, it is possible to freely determine or influence the nature of the nanoparticles to a much greater extent than would be possible if the production of the nanoparticles in the course of the deposition process , So would be done simultaneously with the deposition of the layer to be produced; because of the separation of the two processes, the process control for the deposition process and the process control for the nanoparticle formation can be optimized separately from each other.
  • a significantly larger state area of the phase diagram of the nanoparticles can be used technically than in a "one-step production method” in which the materials constituting the nanoparticles evaporate and in the context of one and the same process atomically or ionically condense into the layer structure while undergoing a chemical reaction.
  • the method according to the invention thus makes it possible to produce completely novel layer systems.
  • Nanoparticles or nanocrystallites in the solid state of matter are preferably deposited on the substrate as nanoparticles.
  • nanoparticle-comprising layer it is also possible to additionally deposit further material on the substrate in the second process chamber-simultaneously with the finished nanoparticles-which then together with the nanoparticles forms the nanoparticle-comprising layer.
  • a carrier gas is enriched with the nanoparticles and the carrier gas enriched with the nanoparticles is conducted into the second process chamber.
  • the process parameters in the first process chamber are optimized with regard to the formation or release of the nanoparticles; the process parameters in the second process chamber are optimized for optimal deposition of the finished nanoparticles.
  • a higher pressure is preferably in the first process chamber than in the second process chamber set; the temperature in the first process chamber is preferably below the temperature of the second process chamber.
  • the carrier gas stream is preferably conducted via a throttle device.
  • the flow rate of the carrier gas is then adjusted or regulated in the second process chamber.
  • the deposition rate of the nanoparticles within the second process chamber can be specifically influenced, at least influenced, by the throttle device.
  • the nanoparticles are released and moved by means of an external electromagnetic field to form the nanoparticle stream in the direction of the second process chamber.
  • an effusor cell is preferably used as the first process chamber.
  • an anticorrosion layer an adhesion layer, a wear protection layer, a sensor layer or a catalytic layer can be produced with the described method.
  • the invention also relates to an arrangement for producing a nanoparticle-containing layer on a substrate.
  • the invention has for its object to allow a particularly large margin in the design and composition of the layer to be produced.
  • a first process chamber is provided which is suitable for releasing nanoparticles and for generating a nanoparticle stream
  • a second process chamber is connected to the first process chamber, into which the nanoparticle stream is conducted and in which Nanoparticles are deposited on the substrate.
  • FIG. 1 one recognizes a first process chamber which is formed by an effusor cell 10.
  • the Effusorzelle 10 has an inlet opening E10, in which a carrier gas 20 - symbolized by an arrow - is fed into the Effusorzelle 10.
  • the further gas flow of the carrier gas 20 is in the FIG. 1 visualized by further arrows 25.
  • a nanoparticle base material 30 Within the Effusorzelle 10 is a nanoparticle base material 30, with in one in the FIG. 1 not shown, nanoparticles 40 are formed and released. The released nanoparticles 40 are detected by the carrier gas 20, so that a in the FIG. 1 forms left-directed nanoparticle stream 50, which is directed to an outlet opening A10 of Effusorzelle 10.
  • a throttle device 70 Connected to the outlet opening A10 of the effusor cell 10 is a throttle device 70, which on the output side is connected to a first inlet opening A80 of a second process chamber 80.
  • the second process chamber 80 is a reactor chamber that is in a high vacuum.
  • the pressure P2 in the reactor chamber 80 is preferably in a range between 10 -5 mbar and 1 mbar.
  • a substrate 100 is arranged, on which a nanoparticle 40 having layer 110 is to be deposited.
  • the substrate 100 is arranged in the region of the first inlet opening A80 of the reactor chamber 80 such that the effusor cell 10 leaving and Throttling device 70 passing nanoparticle current 50 flows laterally over the surface 120 of the substrate 100, resulting in a deposition of the nanoparticles 40 on the surface 120 of the substrate 100 and the layer formation of the layer 110 result.
  • the layer 110 should not consist exclusively of nanoparticles 40; Rather, a layer 110 is to be formed, which contains further materials in addition to the nanoparticles 40.
  • the reactor chamber 80 has a second inlet opening B80, through which a material flow 150 with further material is conducted into the reactor chamber 80.
  • the flow of material 150 is oriented to direct the further material directly onto the surface 120 of the substrate 100.
  • the material stream 150 preferably impinges on the surface 120 of the substrate 100 at a right angle; the flow of material 150 is therefore also at a right angle to the nanoparticle stream 50, which is preferably aligned parallel to the surface 120 of the substrate 100.
  • the further material contained in the material flow 150 and the nanoparticles 40 of the nanoparticle stream 50 together form the layer 110 which deposits on the surface 120 of the substrate 100.
  • the nanoparticles 40 are transported via the carrier gas stream 20 into the reactor chamber 80.
  • the pressure P1 in the effusion cell 10 is higher than the pressure P2 in the reactor chamber 80.
  • the pressure within the effusion cell 10 is in a pressure range between 10 -2 mbar and 10 -5 mbar.
  • nanoclusters or nanocrystallites can be formed as nanoparticles 40.
  • a cBN (cubic) material may be used as the nanoparticle base material 30.
  • the effusor cell 10 comprises an electromagnetic device 200 disposed in the effusor cell 10 or at the effusor cell 10; in the example according to the FIG. 2
  • the electromagnetic device 200 is attached to the bottom of the effusor cell 10.
  • the electromagnetic device 200 generates an electromagnetic field in such a way that the nanoparticles 40 formed from the nanoparticle base material 30 form a nanoparticle stream 50, which leaves the effusor cell 10 in the direction of the reactor chamber 80 and is then fed into it.
  • FIG. 3 3 shows a third exemplary embodiment of an arrangement for producing a layer 110 containing nanoparticles 40.
  • the nanoparticle stream 50 is formed by the interaction of a carrier gas 20 and an electromagnetic device 200.
  • the nanoparticle current 50 is therefore formed by a superimposition of two forces acting on the nanoparticles 40. This is, on the one hand, the electromagnetic force of the electromagnetic device 200 and, on the other hand, the mechanical motive force due to the flow of the carrier gas 20.

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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 Or Chemical Processes And Apparatus (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)

Claims (11)

  1. Procédé de production sur un substrat ( 100 ) d'une couche ( 110 ) ayant des nanoparticules ( 40 ), dans lequel
    - on libère des nanoparticules ( 40 ) et on produit un courant ( 50 ) de nanoparticules,
    - on envoie le courant ( 50 ) de nanoparticules dans une deuxième chambre ( 80 ) de traitement, le courant de nanoparticules étant conduit latéralement, parallèlement, sur la surface ( 120 ) du substrat ( 100 ) se trouvant dans la deuxième chambre ( 80 ) de traitement, et
    - on dépose sur le substrat ( 100 ), les nanoparticules ( 40 ) par le courant de nanoparticules ainsi dirigé dans la deuxième chambre ( 80 ) de traitement,
    caractérisé
    - en ce que dans la deuxième chambre de traitement, on dépose sur le substrat, supplémentairement, au moins un autre matériau qui forme conjointement avec les nanoparticules, la couche ayant les nanoparticules,
    - dans lequel on envoie l'autre matériau sous la forme d'un courant ( 150 ) de matériau, sur la surface ( 120 ) du substrat ( 100 ) et
    - dans lequel on dirige ce courant ( 150 ) de matériau, de manière à ce qu'il arrive suivant un angle droit sur la surface du substrat ( 100 ).
  2. Procédé suivant l'une des revendications 1 précédentes,
    caractérisé en ce que
    - on accélère les nanoparticules ( 40 ) dans la première chambre ( 10 ) de traitement, à l'aide d'un champ ( 200 ) électromagnétique extérieur, parallèlement à la surface ( 120 ) du substrat ( 100 ) se trouvant dans la deuxième chambre de traitement et on les met en mouvement dans la direction de la deuxième chambre de traitement en formant le courant ( 50 ) de nanoparticules.
  3. Procédé suivant l'une des revendications précédentes,
    caractérisé en ce que
    - pour la formation du courant de nanoparticules dans la première chambre de traitement, on enrichit un gaz ( 20 ) porteur en les nanoparticules ( 40 ) et
    - en ce que l'on conduit le gaz porteur enrichi en les nanoparticules, dans la deuxième chambre ( 80 ) de traitement.
  4. Procédé suivant la revendication 3, caractérisé
    - en ce que l'on conduit le gaz porteur enrichi en les nanoparticules, de la première chambre de traitement à la deuxième chambre de traitement, par un dispositif ( 70 ) d'étranglement et
    - en ce que l'on règle, par le dispositif d'étranglement, le flux du gaz porteur dans la deuxième chambre de traitement.
  5. Procédé suivant la revendication 4,
    caractérisé en ce que l'on règle, par le dispositif d'étranglement, la vitesse de dépôt des nanoparticules dans la deuxième chambre de traitement.
  6. Procédé suivant l'une des revendications précédentes,
    caractérisé en ce que l'on établit dans la deuxième chambre de traitement, une pression ( P2 ) plus basse que dans la première chambre de traitement.
  7. Procédé suivant l'une des revendications précédentes,
    caractérisé en ce que l'on utilise comme première chambre de traitement, une cellule ( 10 ) d'effuseur et on produit le courant de nanoparticules dans la cellule d'effuseur.
  8. Procédé suivant l'une des revendications précédentes,
    caractérisé en ce que l'on dépose sur le substrat des nanoagglomérats ou des nanocristallites.
  9. Dispositif de production sur un substrat d'une couche ayant des nanoparticules,
    - dans lequel il y a une première chambre ( 10 ) de traitement, qui est appropriée à la libération de nanoparticules ( 40 ) et à la production d'un courant ( 50 ) de nanoparticules, et
    - dans lequel, avec la première chambre ( 10 ) de traitement communique une deuxième chambre ( 81 ) de traitement, dans laquelle le courant ( 50 ) de nanoparticules est guidé, et dans laquelle les nanoparticules se déposent sur le substrat ( 100 ),
    caractérisé
    - en ce qu'une première ouverture ( A80 ) d'entrée de la deuxième chambre de traitement est disposée de manière à ce que le courant de nanoparticules s'écoule latéralement, parallèlement, sur la surface ( 120 ) du substrat ( 100 ) et de manière à ce que les nanoparticules ( 40 ) se déposent, par le courant de nanoparticules ainsi dirigé, sur la surface du substrat.
    - en ce que la deuxième chambre de traitement a une deuxième ouverture ( B80 ) d'entrée, pour l'introduction d'au moins un autre matériau, qui se dépose sur le substrat et qui forme conjointement avec les nanoparticules, la couche ayant des nanoparticules, et
    - en ce que la deuxième ouverture ( A80 ) d'entrée est disposée de manière à ce que l'autre matériau arrive sous la forme d'un courant ( 150 ) de matériau, suivant un angle droit, sur la surface du substrat ( 100 ).
  10. Dispositif suivant la revendication 9, caractérisé en ce qu'un dispositif ( 200 ) électromagnétique est disposé dans ou sur la première chambre de traitement, de manière à ce que les nanoparticules libérées dans la première chambre de traitement soient, à l'aide d'un champ ( 200 ) électromagnétique extérieur, accélérées parallèlement à la surface ( 120 ) du substrat ( 100 ) se trouvant dans la deuxième chambre de traitement et soient mises en mouvement dans la direction de la deuxième chambre de traitement avec formation du courant ( 50 ) de nanoparticules.
  11. Procédé suivant l'une des revendications précédentes 9 ou 10, caractérisé en ce que la première chambre de traitement est formée par une cellule ( 10 ) d'effuseur.
EP06777538A 2005-07-07 2006-07-03 Procede pour produire sur un substrat une couche presentant des nanoparticules Active EP1899499B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102005032711A DE102005032711A1 (de) 2005-07-07 2005-07-07 Verfahren zum Herstellen einer Nanopartikel aufweisenden Schicht auf einem Substrat
PCT/EP2006/063778 WO2007006674A1 (fr) 2005-07-07 2006-07-03 Procede pour produire sur un substrat une couche presentant des nanoparticules

Publications (2)

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EP1899499A1 EP1899499A1 (fr) 2008-03-19
EP1899499B1 true EP1899499B1 (fr) 2010-11-10

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EP06777538A Active EP1899499B1 (fr) 2005-07-07 2006-07-03 Procede pour produire sur un substrat une couche presentant des nanoparticules

Country Status (9)

Country Link
US (1) US7906171B2 (fr)
EP (1) EP1899499B1 (fr)
JP (1) JP2009500522A (fr)
CN (1) CN101218373A (fr)
AT (1) ATE487809T1 (fr)
DE (2) DE102005032711A1 (fr)
DK (1) DK1899499T3 (fr)
ES (1) ES2355429T3 (fr)
WO (1) WO2007006674A1 (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101331137B1 (ko) * 2011-10-13 2013-11-20 충남대학교산학협력단 코어-쉘 와이어에 의한 나노입자의 발생 및 그를 이용한 나노입자의 처리 장치 및 방법
DE102012106078A1 (de) * 2012-07-06 2014-05-08 Reinhausen Plasma Gmbh Beschichtungsvorrichtung und Verfahren zur Beschichtung eines Substrats
KR101724375B1 (ko) 2015-07-03 2017-04-18 (주)광림정공 나노구조 형성장치

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GB932923A (en) 1961-06-26 1963-07-31 Armco Steel Corp Coating metallic sheet or strip material with powdered annealing separator substances
GB2226257B (en) 1988-11-30 1992-07-22 City Electrical Factors Ltd Powdering cables
DE4000885A1 (de) 1990-01-13 1991-07-18 Philips Patentverwaltung Mehrkomponentige submikroskopische partikel und verfahren zu ihrer herstellung
JP2890599B2 (ja) 1990-02-06 1999-05-17 ソニー株式会社 加工方法
US5139537A (en) * 1991-06-13 1992-08-18 Julien D Lynn Titanium-nitride coated grinding wheel and method therefor
JP3429014B2 (ja) 1992-10-16 2003-07-22 真空冶金株式会社 超微粒子のガスデポジション方法及び装置
EP0659911A1 (fr) * 1993-12-23 1995-06-28 International Business Machines Corporation Procédé pour la formation d'un film polycristallin sur un substrat
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JP2963993B1 (ja) * 1998-07-24 1999-10-18 工業技術院長 超微粒子成膜法
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DE10027948A1 (de) * 2000-06-08 2001-12-20 Henkel Kgaa Verfahren zur Herstellung von Nanopartikel-Suspensionen
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JP2004200476A (ja) * 2002-12-19 2004-07-15 Canon Inc 圧電素子の製造方法

Also Published As

Publication number Publication date
WO2007006674A1 (fr) 2007-01-18
DE102005032711A1 (de) 2007-01-11
DK1899499T3 (da) 2011-02-14
US20090047444A1 (en) 2009-02-19
ES2355429T3 (es) 2011-03-25
ATE487809T1 (de) 2010-11-15
EP1899499A1 (fr) 2008-03-19
CN101218373A (zh) 2008-07-09
JP2009500522A (ja) 2009-01-08
US7906171B2 (en) 2011-03-15
DE502006008288D1 (de) 2010-12-23

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