WO2001004379A1 - Anlage und verfahren zur vakuumbehandlung bzw. zur pulverherstellung - Google Patents

Anlage und verfahren zur vakuumbehandlung bzw. zur pulverherstellung Download PDF

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Publication number
WO2001004379A1
WO2001004379A1 PCT/CH2000/000364 CH0000364W WO0104379A1 WO 2001004379 A1 WO2001004379 A1 WO 2001004379A1 CH 0000364 W CH0000364 W CH 0000364W WO 0104379 A1 WO0104379 A1 WO 0104379A1
Authority
WO
WIPO (PCT)
Prior art keywords
plasma
deposition
arrangement
discharge
axes
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/CH2000/000364
Other languages
German (de)
English (en)
French (fr)
Inventor
Johann Karner
Mauro Pedrazzini
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.)
OC Oerlikon Balzers AG
Original Assignee
Unaxis Balzers AG
Balzers AG
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 Unaxis Balzers AG, Balzers AG filed Critical Unaxis Balzers AG
Priority to EP00938445A priority Critical patent/EP1194611B1/de
Priority to JP2001509574A priority patent/JP4806146B2/ja
Priority to DE50008516T priority patent/DE50008516D1/de
Publication of WO2001004379A1 publication Critical patent/WO2001004379A1/de
Priority to US10/045,855 priority patent/US6703081B2/en
Anticipated expiration legal-status Critical
Priority to US10/759,611 priority patent/US20050028737A1/en
Ceased legal-status Critical Current

Links

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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/50Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
    • C23C16/513Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using plasma jets

Definitions

  • the present invention is based on a method for vacuum treatment according to the preamble of claim 9 or on a method for producing powder according to that of claim 10.
  • the present invention has the basic objective of being reactive plasma-assisted, ie using a PECVD process, to deposit materials onto a deposition surface, be they materials that are very difficult to manufacture in general, namely metastable materials such as cBN, ⁇ -Al 2 0 3 , C 3 N 4 or, and in particular, diamond material, or in principle materials, but this with the highest possible deposition rate and at the lowest possible temperature, in particular when Si-containing compounds, particularly microcrystalline ⁇ C-Si: H, are to be deposited.
  • metastable materials such as cBN, ⁇ -Al 2 0 3 , C 3 N 4 or, and in particular, diamond material, or in principle materials
  • a disadvantage of these known procedures is that on the one hand only workpiece surfaces of relatively small, in particular flat, extent can be treated homogeneously, in particular coated, and on the other hand it would be entirely desirable to increase the amount of powder or cluster produced per unit of time. It would therefore be desirable, particularly for the diamond coating, to implement a uniform layer thickness distribution over the entire surface, and also with the highest possible coating rate.
  • the method according to the invention for treating workpieces - also as a basis for the system according to the invention - is characterized in that at least two plasma jets with essentially parallel beam axes are generated in the vacuum atmosphere and that the at least one workpiece surface to be treated is along a surface is arranged in the vacuum atmosphere, from which a predetermined plasma density distribution is generated by the plasma jets.
  • the method for powder production according to the invention is characterized in that in the vacuum atmosphere at least two plasma beams with essentially parallel ones
  • Beam axes are generated and a collecting surface for the powder in the vacuum atmosphere is arranged so that from it the plasma beams a predetermined plasma density distribution is generated.
  • the concentration function is shown along a plane E, which is arranged at a distance x n ⁇ n parallel to the plasma beam axis A and viewed along a straight line g in the plane E perpendicular to the beam axis A.
  • the distance dimension is x IBin normalized, the concentration measure with regard to the maximum concentration on the plane E at the location S of the distance x ⁇ .
  • a metastable material preferably cBN, ⁇ -Al 2 O 3 , C 3 N 4 or, and particularly preferably, diamond is deposited on the deposition surface.
  • a silicon compound is deposited on the deposition surface, preferably microcrystalline silicon ⁇ C-Si: H and preferably silane as the reactive gas.
  • the plasma jets are realized as low-voltage arc discharges, by far preferably as high-current arc discharges, preferably by means of cold cathode discharges, but particularly preferably using hot cathode discharges.
  • the deposition surface is arranged in the vacuum atmosphere and with respect to the plasma jets in such a way that predetermined minimum plasma density fluctuations occur along this surface.
  • This is achieved in particular by the fact that plasma densities of at most 20%, preferably at most 10%, preferably even at most 5% of the plasma density maxima of the respective closest plasma rays occur along the deposition surface, the plasma rays being able to be operated in the same way, ie then essentially equal maximum plasma densities in their Have axes.
  • the plasma radiation charges can be operated independently of one another, which opens up the possibility of carrying out the aforementioned optimization on a case-by-case basis.
  • the methods according to the invention are preferably carried out in such a way that when the deposition surface is arranged in such a way that the prevailing plasma density maxima are 20% of the closest beam plasma density maxima, a deposition rate on the deposition surface of at least 400 nm / min is obtained, preferably at the temperature mentioned of at most 500 ° C.
  • the plasma density distribution is coordinated by means of at least one magnetic field parallel to the beam axis.
  • a gas flow essentially parallel to the beam axes is created.
  • the workpieces be rotated about axes of rotation and / or linearly at least approximately parallel to the beam axes moved, preferably oscillating back and forth. Furthermore, it has been shown that with the procedure according to the invention still further effectiveness can be achieved with regard to workpieces which can be treated at the same time or the amount of powder deposited, by arranging at least one first deposition surface between the plasma beams and at least one second deposition surface between the plasma beams and the wall of a treatment chamber with the vacuum atmosphere.
  • FIG. 8 in a representation analogous to FIG. 1, the modeled plasma density distribution according to the invention along a flat deposition surface, parallel to and spaced from two provided plasma beam axes.
  • FIG. 2 schematically shows, in longitudinal section, a system according to the invention for carrying out the method according to the invention.
  • a vacuum chamber 1 at least two, as in FIGS. 3 to 6 preferably at least six, plasma jets 3 are generated. They are preferably, as is also shown in FIG. 2, formed by high-current, low-voltage discharge on corresponding discharge paths, preferably each with a hot cathode 5, directly or indirectly heated, as shown, preferably heated directly with the heating current I H via a heating circuit.
  • the hot cathodes 5 are operated in a cathode chamber arrangement 8, for example, as shown in FIG. 2, with individual cathode chambers 8a, into which (not shown) a working gas, such as argon, is admitted and which are connected to the interior via screens 7 the
  • a working gas such as argon
  • Communicate chamber 1 In principle, however, other types of cathode can also be used to generate the plasma jets, for example hollow cathodes, if high-purity coatings are to be produced and contamination is to be prevented by sublimated hot cathode atoms.
  • FIG. 2 further 9 denote the discharge gap anodes and 11 the discharge generators.
  • the deposition surfaces 13 are provided, which pass at predetermined distances from the beam axes A, between the plasma beams 3, in accordance with the desired plasma density distributions on these surfaces 13 and thus on the deposition arrangement.
  • the deposition surfaces 13 are defined in the workpiece treatment according to the invention by workpiece carrier surfaces, for receiving one or more workpieces (s), or they are formed by collecting surfaces, according to the invention the aim is to produce powder or clusters on these surfaces.
  • the reactive gas is through a gas inlet arrangement 15 in the
  • Chamber 1 let in, used reactive gas sucked out at the pump opening 17.
  • a magnetic field H essentially parallel to the beam axes A is generated in the chamber 1, by means of which, in addition, the local plasma density distribution can be adjusted.
  • FIGS. 3 to 6 show, in a top view and schematically, the arrangements of plasma jets 3 with inventive deposition surfaces 13 guided in between and defined by workpiece carriers 13a or collecting surfaces.
  • Plasma density distribution is achieved, here with minimal inhomogeneity.
  • FIG. 5 also shows in broken lines how, in addition to the deposition surface 13 carried out between the plasma jets 3, which is acted on on both sides, between the plasma jets 3 and the recipient or chamber wall further deposition surfaces 14 can be arranged, which Treatment is only exposed on one side.
  • workpieces to be treated on the one deposition surface 13, in particular to be coated are provided on the deposition surface 13, and only to be treated, in particular to be coated, on the deposition surfaces 13a.
  • FIG. 7 shows the plasma density distribution resulting from two spaced-apart plasma beams as a function of the heating current I. If a flat deposition surface is now placed in a region parallel to the plane of the figure in FIG. 7 such that plasma density maxima of 20% of the maximum plasma densities prevailing in beam axis A occur on this surface, the qualitative at d entered plasma density distribution along this surface results , In a representation analogous to FIG. 1, such a plasma density distribution is shown modeled in FIG. 8, again with (a) with an assumed linear dependence of the plasma density on the arc axis distance x, with (b) with a square assumption.
  • a further homogenization of the realized deposition distribution can be achieved, in particular in the coating, in that the workpieces about an axis A .., preferably essentially perpendicular to the beam axes A, are rotated and / or, as shown in FIG. 6, are moved linearly along the beam axes, shown in FIG. 6 with the double arrow F.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)
  • Physical Vapour Deposition (AREA)
PCT/CH2000/000364 1999-07-13 2000-07-04 Anlage und verfahren zur vakuumbehandlung bzw. zur pulverherstellung Ceased WO2001004379A1 (de)

Priority Applications (5)

Application Number Priority Date Filing Date Title
EP00938445A EP1194611B1 (de) 1999-07-13 2000-07-04 Anlage und verfahren zur vakuumbehandlung bzw. zur pulverherstellung
JP2001509574A JP4806146B2 (ja) 1999-07-13 2000-07-04 真空処理ないしは粉末製造のための装置および方法
DE50008516T DE50008516D1 (de) 1999-07-13 2000-07-04 Anlage und verfahren zur vakuumbehandlung bzw. zur pulverherstellung
US10/045,855 US6703081B2 (en) 1999-07-13 2002-01-11 Installation and method for vacuum treatment or powder production
US10/759,611 US20050028737A1 (en) 1999-07-13 2004-01-16 Installation and method for vacuum treatment or powder production

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CH1292/99 1999-07-13
CH129299 1999-07-13

Related Child Applications (1)

Application Number Title Priority Date Filing Date
US10/045,855 Continuation US6703081B2 (en) 1999-07-13 2002-01-11 Installation and method for vacuum treatment or powder production

Publications (1)

Publication Number Publication Date
WO2001004379A1 true WO2001004379A1 (de) 2001-01-18

Family

ID=4207024

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CH2000/000364 Ceased WO2001004379A1 (de) 1999-07-13 2000-07-04 Anlage und verfahren zur vakuumbehandlung bzw. zur pulverherstellung

Country Status (5)

Country Link
US (2) US6703081B2 (https=)
EP (1) EP1194611B1 (https=)
JP (1) JP4806146B2 (https=)
DE (1) DE50008516D1 (https=)
WO (1) WO2001004379A1 (https=)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8430961B2 (en) 2007-09-07 2013-04-30 Applied Materials, Inc. Source gas flow path control in PECVD system to control a by-product film deposition on inside chamber

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JP4806146B2 (ja) * 1999-07-13 2011-11-02 エリコン・トレーディング・アクチェンゲゼルシャフト,トリュープバッハ 真空処理ないしは粉末製造のための装置および方法
USH2212H1 (en) * 2003-09-26 2008-04-01 The United States Of America As Represented By The Secretary Of The Navy Method and apparatus for producing an ion-ion plasma continuous in time
JP2008508166A (ja) 2004-06-18 2008-03-21 リージェンツ・オブ・ザ・ユニヴァーシティー・オブ・ミネソタ 高周波プラズマを用いてナノ粒子を生成するための方法および装置
US20050281958A1 (en) * 2004-06-22 2005-12-22 Walton Scott G Electron beam enhanced nitriding system (EBENS)
US20080003377A1 (en) * 2006-06-30 2008-01-03 The Board Of Regents Of The Nevada System Of Higher Ed. On Behalf Of The Unlv Transparent vacuum system
US20090014423A1 (en) * 2007-07-10 2009-01-15 Xuegeng Li Concentric flow-through plasma reactor and methods therefor
US20080191193A1 (en) * 2007-01-22 2008-08-14 Xuegeng Li In situ modification of group iv nanoparticles using gas phase nanoparticle reactors
US20080220175A1 (en) * 2007-01-22 2008-09-11 Lorenzo Mangolini Nanoparticles wtih grafted organic molecules
US8968438B2 (en) * 2007-07-10 2015-03-03 Innovalight, Inc. Methods and apparatus for the in situ collection of nucleated particles
US8471170B2 (en) 2007-07-10 2013-06-25 Innovalight, Inc. Methods and apparatus for the production of group IV nanoparticles in a flow-through plasma reactor
US9761424B1 (en) 2011-09-07 2017-09-12 Nano-Product Engineering, LLC Filtered cathodic arc method, apparatus and applications thereof
US10304665B2 (en) 2011-09-07 2019-05-28 Nano-Product Engineering, LLC Reactors for plasma-assisted processes and associated methods
DE102012024340A1 (de) * 2012-12-13 2014-06-18 Oerlikon Trading Ag, Trübbach Plasmaquelle
US10151025B2 (en) * 2014-07-31 2018-12-11 Seagate Technology Llc Helmholtz coil assisted PECVD carbon source
US11834204B1 (en) 2018-04-05 2023-12-05 Nano-Product Engineering, LLC Sources for plasma assisted electric propulsion

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Also Published As

Publication number Publication date
US6703081B2 (en) 2004-03-09
US20050028737A1 (en) 2005-02-10
JP2003504515A (ja) 2003-02-04
DE50008516D1 (de) 2004-12-09
EP1194611A1 (de) 2002-04-10
EP1194611B1 (de) 2004-11-03
JP4806146B2 (ja) 2011-11-02
US20020114898A1 (en) 2002-08-22

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