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
  • C23C14/02—Pretreatment of the material to be coated
  • C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
• • 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
  • C23C14/02—Pretreatment of the material to be coated
  • C23C14/027—Graded interfaces
• • 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
  • C23C14/0641—Nitrides
• • 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
  • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
  • C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T428/00—Stock material or miscellaneous articles
  • Y10T428/31504—Composite [nonstructural laminate]
  • Y10T428/31678—Of metal

Definitions

• the present invention relates to a hard, wear-resistant aluminum nitride based coating, an article coated there with and a method for producing such a coating.
• Layers based on Al ⁇ _ Ti x N respectively based on Al ⁇ _ x Ti x Si y N are commonly used in a Ti/Al stoichiometry range near the maximum hardness. In the case of TiAIN, this stoichiometry corresponds approximately to Alo.e 5 Tio. 35 N. If an Al proportion exceeding these conditions, e.g. 75 to 85 at . % of metals, is selected, both hardness and wear resistance are known to break down rapidly. Essentially the same behaviour has been expected and found for Al ⁇ _ x Cr x N and similar hard materials.
• the object of the invention to provide a hard coating which can be easily produced using cathodic arc evaporation technology and magnetron sputtering technology or a combination thereof.
• the invention achieves the object by a coating according to Claim 1.
• the measures of the invention firstly have the result that an article can be coated by the hard coating according to the present invention using cathodic arc evaporation technology without further handling of the chamber in which the process is performed. Additionally, the coating is surprisingly hard with respect to the parameters .
• the solution according to the present invention is based on the fact that at a further increase of the Al content of any Al ⁇ _ x Me x N system substantially beyond the composition prior known as the maximum hardness, to approximately more than 90 at . % of the total of elements except nitrogen, the hardness has been surprisingly found rising again. Furthermore, this tendency has been found as being enhanced in the presence of silicon. However, very close to pure A1N or Al ⁇ _ySi y N, respectively, the layer hardness decreases again. This can be explained by the buildup of a non-conductive layer, resulting in the suppression of ion bombardment during deposition.
• Figure 1 is a view of the schematic arrangement of the targets in the chamber according to a first example according to the present invention
• Figure 2 is a view of the schematic arrangement of the targets in the chamber according to a second example according to the present invention.
• Figure 3 is a cross-sectional view of an Alo. 91 Sio. 09 N layer showing the undesired formation of a weak columnar coating material due to the lack of ion bombardment;
• Figure 4 is a cross-sectional view of an Alo. 86 Sio. 09 Cro. 05 N layer showing the homogeneous and consistently fine structure achieved by maintaining coating conductivity by doping with a small amount of metal (in this case Cr) ;
• Figure 5 is the diagram of the hardness dependence on coating stoichiometry for the Al ⁇ _ x Cr x Si ( ( ⁇ - x ) / ⁇ o)N system. Besides the main hardness maximum known already, an unexpected secondary hardness maximum is observed at very high (Al+Si) contents.
• the second curve (not this invention) of the comparison system Al ⁇ _ x Cr x N without silicon addition, shows a similar behaviour but generally lower hardness;
• Figure 6 is the diagram of the hardness dependence on coating stoichiometry for the system Al ! _ x Zr x Si ( ( ⁇ _ x ) /s)N. This curve shows that the region below 8 at . % dopant addition even yields the global hardness for this system.
• Figure 8 is the grazing incidence X-ray diffraction diagram of a typical coating according to the present invention of composition l 0 . 834 Sio.i 23 Cr 0 .0 44 0 . 994 / in as- deposited state and after thermal treatment at 800°C in nitrogen atmosphere for one hour. It illustrates the coexistance of both hexagonal and cubic phase in this system.
• the thermal stability of the nanocomposite crystallographic structure is proven by the similarity of the observed diffraction peaks before and after annealing at high temperatures.
• AlN-based layers were deposited predominantly by arc evaporation technology. AlN-based layers can be prepared from a single target or from several separated ones.
• the Al 0 . 8 8sSio. ⁇ o Cr o .015 target 10 is used for the main layer preparation, the pure Cr target 20 is used for cleaning process and for adhesion and optional base layer system, alone or in combination with target 10.
• Electrode 30 consists of an AlSi alloy respectively pure Al
• the metal electrode 40 is used for ion cleaning, to form the optional base layer, and is used, during the process, together with the AlSi (Al) to create the main Al ⁇ - x Me x Si y N layer.
• the process becomes unstable.
• the arc voltage grows up - at a nitrogen pressure of 2 Pa, 100 A arc current - from 30 V to more than 40 V during the process which influences both process stability and coating quality.
• the addition of either or both, conductive nitrides and metallic conductive materials stabilize the evaporation process of AlSi respectively Al material in nitrogen or a nitrogen-based gas mixture atmosphere.
• the pure Al ⁇ _ y SiyN layer cross-section in comparison to an Al ⁇ _ x Cr x SiyN layer is shown on the figures 3 and 4.
• the difference is considered being caused by insufficient conductivity of the layer during the process.
• the ion bombardment is not maintained which causes grain coarsening during film growth, resulting in bad mechanical properties.
• the increase of the arc voltage during the process has been measured to be no more than 1 V.
• the material shows no significant voltage increase at all during deposition resulting in a homogeneous structure, which yields good mechanical properties, i.e. wear resistance, important for the use of the coating.
• Figure 5 shows the hardness dependence on coating stoichiometry for the system Al ⁇ _ x Cr x Si y N respectively Al ⁇ -- x Cr x N
• Figure 6 Ali_ x Zr x Si y N shows another dopant possibility and a higher silicon content.
• This stability can be explained by the two-phase structure of this material, which contains both hexagonal A1N phase and another, cubic phase (Fig. 8) .
• This nanocomposite system remains practically unchanged after annealing for one hour at 800°C in an inert atmosphere. This means an improvement for the use of such compounds as coatings for tooling applications, where high temperatures occur at the cutting edge.
• Example 1 Two-cathode solution (arc process)
• Target 1 Cr (partially shielded)
• Target 1 Ti Target 2 Al o . 9 oSi 0 . o 8 Cr o . O 2 alloy or blend
• Coating thickness 4 . 0 ⁇ m
• Target 1 Zr (partially shielded)
• Process sequence Pumping to high vacuum P ⁇ lxl0-5 hPa Heating in vacuum to process temperature, e.g. 450°C Ar plasma etching, Ar flow 200 seem, bias -750 V, Imin Arc metal ion etching, bias -1200 V, 5 min, Zr arc 70A, Ar flow 15 seem Adhesion layer (optional) , ZrN, Zr current 120 A, cathode 2 off, P (N 2 ) 1.8xl0 -2 hPa, bias -120 V, 2 min Graded interlayer, Al 1 _ x Zr x Si ( ( ⁇ - x) /s.
• Ar flow 200 seem, bias -750 V, Imin Arc metal ion etching, bias -1200 V, 5 min, Zr arc 70A, Ar flow 15 seem Adhesion layer (optional) , ZrN, Zr current 120 A, cathode 2 off, P (N 2 ) 1.8xl0 -2 hPa,
• Target 1 Cr (arc target)
• Target 2 Al 0 . 82 Sio.i 5 Cr 0 . 03 alloy or blend (sputter magnetron) Coating: Alo . siSio . ⁇ 4 Cr 0 .05 N
• Coating thickness 2.0 ⁇ m

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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)
• Cutting Tools, Boring Holders, And Turrets (AREA)
• Other Surface Treatments For Metallic Materials (AREA)
• Drilling Tools (AREA)

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• 2005
  • 2005-04-18 KR KR1020067021755A patent/KR101089528B1/ko not_active Expired - Fee Related
  • 2005-04-18 WO PCT/EP2005/003974 patent/WO2005100635A1/en not_active Ceased
  • 2005-04-18 US US11/568,088 patent/US7704611B2/en not_active Expired - Fee Related
  • 2005-04-18 JP JP2007508791A patent/JP5209960B2/ja not_active Expired - Fee Related
  • 2005-04-18 CA CA 2562402 patent/CA2562402C/en not_active Expired - Fee Related
  • 2005-04-18 EP EP20050739548 patent/EP1749118B1/en not_active Expired - Lifetime
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