WO2017136968A1 - Revêtement composite d'oxyde d'aluminium, outil de coupe en alliage dur ultrafin à structure étagée pourvu du revêtement composite et procédé de fabrication associé - Google Patents

Revêtement composite d'oxyde d'aluminium, outil de coupe en alliage dur ultrafin à structure étagée pourvu du revêtement composite et procédé de fabrication associé Download PDF

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WO2017136968A1
WO2017136968A1 PCT/CN2016/075333 CN2016075333W WO2017136968A1 WO 2017136968 A1 WO2017136968 A1 WO 2017136968A1 CN 2016075333 W CN2016075333 W CN 2016075333W WO 2017136968 A1 WO2017136968 A1 WO 2017136968A1
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layer
target
composite coating
tialn
alumina
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Chinese (zh)
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伍尚华
陈健
邓欣
刘伟
陈少华
刘汝德
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广东工业大学
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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
    • 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
    • C23C14/3435—Applying energy to the substrate during sputtering
    • C23C14/345—Applying energy to the substrate during sputtering using substrate bias
    • 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
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • 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
    • C23C14/08—Oxides
    • C23C14/081—Oxides of aluminium, magnesium or beryllium
    • 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
    • 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
    • C23C14/3464—Sputtering using more than one target
    • 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
    • C23C14/3485—Sputtering using pulsed power to the target
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • C23C28/044—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material coatings specially adapted for cutting tools or wear applications

Definitions

  • the invention relates to the technical field of cemented carbide cutters, in particular to an alumina composite coating, a gradient ultrafine cemented carbide cutter having the composite coating and a preparation method thereof.
  • coated carbide tools is an important milestone in the history of tool development. It is formed by coating a thin layer of refractory metal or non-metal compound with good wear resistance by a vapor deposition method on a cemented carbide substrate having good strength and toughness.
  • the coating reduces the diffusion and chemical reaction between the tool and the workpiece, thus reducing crater wear.
  • the coating has high hardness and heat resistance and reduces the coefficient of friction between the tool and the workpiece. Therefore, the coated tool can significantly improve the service life than the uncoated tool. Generally, the life of the coated tool can be compared with that of the uncoated tool. 2-5 times higher.
  • TiN coating has high hardness and good wear resistance, which can protect the tool.
  • TiN coating is oxidized at temperatures above 600 ° C, which limits its application.
  • the TiAlN coating can form a dense Al 2 O 3 film at a high temperature and has a good bonding force with the tool substrate.
  • the oxidation resistance temperature can reach 800 ° C, but it still cannot meet the high-speed cutting conditions exceeding 1000 ° C.
  • Al 2 O 3 has high abrasion resistance and red hardness, and maintains good chemical stability at 1000 °C. Coating the surface of the cutting tool with Al 2 O 3 coating can protect the tool under high-speed dry cutting conditions, thus effectively improving the machining efficiency and tool life of the cutting tool.
  • an alumina-based composite coating suitable for surface performance enhancement of a cemented carbide tool, a gradient ultra-fine cemented carbide tool having the composite coating, and a preparation method thereof are provided to overcome the prior art Insufficient is necessary.
  • One of the objects of the present invention is to provide a gradient ultra-fine cemented carbide tool having an alumina-based composite coating and a preparation method thereof, and the alumina-based composite coating has good bonding property with a tool base, and the tool has good wear resistance. Temperature performance.
  • Another object of the present invention is to provide an alumina-based composite coating and a preparation method thereof, which avoids the deficiencies of the prior art, and the alumina-based composite coating has good bonding property with the tool base, and has high temperature resistance and corrosion resistance. Good sex and wear resistance.
  • the tool substrate comprises a normal tissue layer, a cobalt-rich transition layer and a cobalt-depleted cubic phase layer, and the normal tissue layer, the cobalt-rich transition layer and the cobalt-depleted cubic phase layer are arranged in order from the inside to the outside;
  • the alumina-based composite coating layer comprises a TiAlN layer deposited on the surface of the cobalt-depleted cubic phase layer as a transition layer, a TiAlN/Al 2 O 3 layer deposited as a support layer on the transition layer, and deposited on the support layer as An ⁇ -Al 2 O 3 layer of the wear resistant layer, the TiAlN/Al 2 O 3 layer being alternately composed of a TiAlN layer and an Al 2 O 3 layer.
  • the content of cobalt in the above tool base is 5-15 wt.%;
  • the normal tissue layer is an ultrafine cemented carbide, and the WC grain size is 1-1000 nm;
  • the thickness of the normal tissue layer is greater than 2 mm, the thickness of the cobalt-rich transition layer is 20-100 microns; and the thickness of the cobalt-depleted cubic phase layer is 20-50 microns;
  • the alumina-based composite coating layer has a thickness of 1 to 20 ⁇ m, the transition layer has a thickness of 0.1 to 2 ⁇ m; the support layer has a thickness of 5 to 10 ⁇ m; and the wear-resistant layer has a thickness of 5 to 10 ⁇ m; Micron
  • each layer of TiAlN layer has a thickness of 5-20 nm, and each layer of Al 2 O 3 layer has a thickness of 5-10 nm.
  • the content of cobalt in the cutter base is 8-12 wt.%; the WC grain size of the normal tissue layer is 1 nm-400 nm; and the thickness of the alumina composite coating layer is 2-10 micrometers.
  • the above gradient ultrafine cemented carbide tool having an alumina-based composite coating, the TiAlN layer as the transition layer and the TiAlN layer in the support layer are all reacted and sputtered in a mixed atmosphere of N 2 or Ar and N 2 .
  • the Ti alloy target is prepared.
  • the gas pressure during the deposition process is 0.1-2Pa, the substrate temperature is 300-700°C, and the asymmetric bidirectional pulse power supply with alternating positive and negative poles is used to increase the bias voltage. 2-20%;
  • the Al 2 O 3 layer in the support layer is prepared by reactive sputtering of the Al target by bidirectional pulse DMS technology. Specifically, a symmetric bidirectional pulse power source is applied to both ends of the cathode target, and the cathode target material is a pure Al target, and the Al target is passed through the Al target. Reacting with O 2 in the atmosphere to form an Al 2 O 3 coating having a substrate temperature of 300-700 ° C or 1000-1015 ° C and a gas pressure of 0.1-2 Pa; a bidirectional pulse power supply with positive and negative bias applied to the cathode target The positive and negative bias ranges are 20-50V and 20-300V, respectively;
  • the ⁇ -Al 2 O 3 layer as a wear-resistant layer is prepared by reactive sputtering of an Al target by a bidirectional pulsed DMS technique, in particular, a symmetric bidirectional pulse power source is applied to both ends of the cathode target, and the material of the cathode target is a pure Al target.
  • the Al 2 O 3 coating is formed by reacting the Al target with O 2 in the atmosphere, the substrate temperature is 1000-1015 ° C, the gas pressure is 0.1-2 Pa, and the bidirectional pulse power source with positive and negative bias is applied to the cathode target.
  • the positive and negative bias ranges are 20-50V and 20-300V, respectively.
  • Providing a method for preparing a gradient ultra-fine cemented carbide tool having an alumina-based composite coating comprising preparing a tool base and preparing an alumina-based composite coating on a surface of the tool base;
  • the preparation of the alumina-based composite coating comprises sequentially preparing a TiAlN layer as a transition layer on the surface of the tool substrate, depositing a TiAlN/Al 2 O 3 layer as a support layer on the transition layer, and depositing ⁇ - as a wear layer on the support layer.
  • the TiAlN layer as the transition layer and the TiAlN layer in the support layer are prepared by reactive sputtering of an Al-Ti alloy target in a mixed atmosphere of N 2 or Ar and N 2 , and the gas pressure during deposition is 0.1-2 Pa, the matrix
  • the temperature is 300-700 ° C, and the asymmetric bidirectional pulse power supply with alternating positive and negative poles is used to increase the bias voltage, wherein the negative electrode change ratio is 2-20%;
  • the Al 2 O 3 layer in the support layer is prepared by reactive sputtering of the Al target by bidirectional pulse DMS technology. Specifically, a symmetric bidirectional pulse power source is applied to both ends of the cathode target, and the cathode target material is a pure Al target, and the Al target is passed through the Al target. Reacting with O 2 in the atmosphere to form an Al 2 O 3 coating having a substrate temperature of 300-700 ° C or 1000-1015 ° C and a gas pressure of 0.1-2 Pa; a bidirectional pulse power supply with positive and negative bias applied to the cathode target The positive and negative bias ranges are 20-50V and 20-300V, respectively;
  • the ⁇ -Al 2 O 3 layer as a wear-resistant layer is prepared by reactive sputtering of an Al target by a bidirectional pulsed DMS technique, in particular, a symmetric bidirectional pulse power source is applied to both ends of the cathode target, and the material of the cathode target is a pure Al target.
  • the Al 2 O 3 coating is formed by reacting the Al target with O 2 in the atmosphere, the substrate temperature is 1000-1015 ° C, the gas pressure is 0.1-2 Pa, and the bidirectional pulse power source with positive and negative bias is applied to the cathode target.
  • the positive and negative bias ranges are 20-50V and 20-300V, respectively.
  • An alumina composite coating for a gradient ultrafine cemented carbide tool comprising a TiAlN layer for deposition on a surface of a tool substrate as a transition layer, and TiAlN/Al 2 O 3 deposited as a support layer on the transition layer And a layer of ⁇ -Al 2 O 3 deposited as a wear layer on the support layer, the TiAlN/Al 2 O 3 layer being alternately composed of a TiAlN layer and an Al 2 O 3 layer.
  • the above alumina-based composite coating layer has a thickness of 1 to 20 ⁇ m, the transition layer has a thickness of 0.1 to 2 ⁇ m; the support layer has a thickness of 5 to 10 ⁇ m; and the wear-resistant layer has a thickness of 5 to 10 ⁇ m. ;
  • each layer of TiAlN layer has a thickness of 5-20 nm, and each layer of Al 2 O 3 layer has a thickness of 5-10 nm.
  • the above alumina-based composite coating layer has a thickness of 2 to 10 ⁇ m.
  • a method for preparing an alumina-based composite coating comprising sequentially preparing a TiAlN layer as a transition layer on a surface of a tool substrate, depositing a TiAlN/Al 2 O 3 layer as a support layer on the transition layer, and depositing on the support layer An ⁇ -Al 2 O 3 layer of the wear resistant layer;
  • the TiAlN layer as the transition layer and the TiAlN layer in the support layer are prepared by reactive sputtering of an Al-Ti alloy target in a mixed atmosphere of N 2 or Ar and N 2 , and the gas pressure during deposition is 0.1-2 Pa, the matrix
  • the temperature is 300-700 ° C, and the asymmetric bidirectional pulse power supply with alternating positive and negative poles is used to increase the bias voltage, wherein the negative electrode change ratio is 2-20%;
  • the Al 2 O 3 layer in the support layer is prepared by reactive sputtering of the Al target by bidirectional pulse DMS technology. Specifically, a symmetric bidirectional pulse power source is applied to both ends of the cathode target, and the cathode target material is a pure Al target, and the Al target is passed through the Al target. Reacting with O 2 in the atmosphere to form an Al 2 O 3 coating having a substrate temperature of 300-700 ° C or 1000-1015 ° C and a gas pressure of 0.1-2 Pa; a bidirectional pulse power supply with positive and negative bias applied to the cathode target The positive and negative bias ranges are 20-50V and 20-300V, respectively;
  • the ⁇ -Al 2 O 3 layer as the wear-resistant layer is prepared by reactive sputtering of the Al target by a bidirectional pulsed DMS technique, in particular, a symmetric bidirectional pulse power source is applied to both ends of the cathode target, and the material of the cathode target is a pure Al target.
  • the Al 2 O 3 coating is formed by reacting the Al target with O 2 in the atmosphere, the substrate temperature is 1000-1015 ° C, the gas pressure is 0.1-2 Pa, and the bidirectional pulse power source with positive and negative bias is applied to the cathode target.
  • the positive and negative bias ranges are 20-50V and 20-300V, respectively.
  • the gradient ultra-fine cemented carbide tool with the alumina-based composite coating has good bonding property between the tool base and the alumina composite coating, and the overall cutter has good wear resistance and temperature resistance.
  • the alumina composite coating has good adhesion to the tool base, and the adhesion between the coatings of the composite coating is good, and the high temperature resistance, corrosion resistance and wear resistance are good.
  • Fig. 1 is a schematic view of a gradient ultrafine cemented carbide tool having an alumina-based composite coating of the present invention.
  • FIG. 2 is a schematic view showing the interlayer structure of a gradient ultrafine cemented carbide tool having an alumina-based composite coating layer of the present invention.
  • a gradient ultra-fine cemented carbide tool having an alumina-based composite coating is composed of a tool base and an alumina-based composite coating provided on the tool base.
  • the tool substrate comprises a normal tissue layer, a cobalt-rich transition layer and a cobalt-depleted cubic phase layer, and the normal tissue layer, the cobalt-rich transition layer and the cobalt-depleted cubic phase layer are arranged in order from the inside to the outside.
  • the content of cobalt in the tool base is 5-15 wt.%, preferably the content of cobalt is 8-12 wt.%.
  • the normal tissue layer is an ultrafine cemented carbide having a WC grain size of 1-1000 nm, preferably a WC grain size of 1-500 nm.
  • the cobalt-depleted cubic phase layer is rich in cubic phase nitrides or carbonitrides, and the cubic phase nitrides and carbonitrides in the cemented carbide have a higher hardness than the densely packed hexagonal phase WC. Therefore, the cobalt-poor rich cube
  • the surface layer of the phase has a higher hardness.
  • the cobalt-rich transition layer is rich in a binder phase.
  • the core is a rigid tissue region, that is, a normal tissue layer.
  • the WC crystal grain is uniform and fine, and the average WC grain size is less than or equal to 500 nm, which has excellent mechanical properties of the ultrafine cemented carbide.
  • the alumina composite coating layer comprises a TiAlN layer deposited on the surface of the cobalt-depleted cubic phase layer as a transition layer, a TiAlN/Al 2 O 3 layer deposited as a support layer on the transition layer, and deposited on the support layer as wear resistant A layer of ⁇ -Al 2 O 3 , the TiAlN/Al 2 O 3 layer being alternately composed of a TiAlN layer and an Al 2 O 3 layer.
  • the support layer is used to increase toughness and strength.
  • the wear layer improves hardness and strength and has antioxidant properties.
  • the thickness of the normal tissue layer is greater than 2 mm, the thickness of the cobalt-rich transition layer is 20-100 microns, and the thickness of the cobalt-depleted cubic phase layer is 20-50 microns.
  • the thickness of the alumina-based composite coating as a whole is from 1 to 20 ⁇ m, preferably from 2 to 10 ⁇ m.
  • the thickness of the coating is controlled by adjusting the deposition time.
  • the thickness of the transition layer is 0.1-2 microns, and the transition layer enhances the bonding force with the cobalt-depleted cubic phase layer and reduces the internal stress.
  • the support layer is a TiAlN/Al 2 O 3 layer having a thickness of 5 um to 10 um.
  • the support layer is formed by alternately depositing a hard TiAlN layer and an Al 2 O 3 layer.
  • Each layer of TiAlN layer has a thickness of 5-20 nm, and each layer of Al 2 O 3 has a thickness of 5-10 nm, and the number of alternately deposited layers reaches 4-1000 layers.
  • the Al 2 O 3 coating acts primarily as a thermal and chemical barrier to maintain the stability of the blade during processing.
  • the main constituent elements of Al 2 O 3 coating is Al, and O, depending on the deposition temperature, which may be amorphous, nanocrystalline or three-phase mixture of amorphous and nanocrystalline ⁇ -, ⁇ - or-Ab0 ⁇ .
  • the transition layer is an ⁇ -Al 2 O 3 layer having a thickness of 5 um to 10 um.
  • a gradient ultra-fine cemented carbide tool having an alumina-based composite coating, the TiAlN layer as a transition layer and the TiAlN layer in the support layer may each be reactively sputtered in a mixed atmosphere of N 2 or Ar and N 2 .
  • the alloy target is prepared.
  • the gas pressure during the deposition process is 0.1-2Pa, the substrate temperature is 300-700°C, and the asymmetric bidirectional pulse power supply with alternating positive and negative electrodes is used to increase the bias voltage.
  • the negative electrode change ratio is 2 -20%.
  • the Al 2 O 3 layer in the support layer is prepared by reactive sputtering of the Al target by bidirectional pulse DMS technology. Specifically, a symmetric bidirectional pulse power source is applied to both ends of the cathode target, and the cathode target material is a pure Al target, and the Al target is passed through the Al target. Reacting with O 2 in the atmosphere to form an Al 2 O 3 coating having a substrate temperature of 300-700 ° C or 1000-1015 ° C and a gas pressure of 0.1-2 Pa; a bidirectional pulse power supply with positive and negative bias applied to the cathode target The positive and negative bias ranges are 20-50V and 20-300V, respectively. Depending on the deposition temperature, an amorphous or nanocrystalline Al 2 O 3 coating is deposited.
  • the coating prepared at a substrate temperature of 300-500 ° C is mainly amorphous
  • the coating prepared at a substrate temperature of 500-700 ° C is mainly in a nanocrystalline state
  • the coating prepared at a substrate temperature of 1000-1015 ° C is ⁇ .
  • -Al 2 O 3 layer The thickness of the Al 2 O 3 coating is primarily adjusted by controlling the deposition time.
  • the ⁇ -Al 2 O 3 layer as a wear-resistant layer is prepared by reactive sputtering of an Al target by a bidirectional pulsed DMS technique, in particular, a symmetric bidirectional pulse power source is applied to both ends of the cathode target, and the material of the cathode target is a pure Al target.
  • the Al 2 O 3 coating is formed by reacting the Al target with O 2 in the atmosphere, the substrate temperature is 1000-1015 ° C, the gas pressure is 0.1-2 Pa, and the bidirectional pulse power source with positive and negative bias is applied to the cathode target.
  • the positive and negative bias ranges are 20-50V and 20-300V, respectively.
  • the gradient ultra-fine cemented carbide tool with the alumina-based composite coating has good bonding property between the tool base and the alumina composite coating, and the overall cutter has good wear resistance and temperature resistance.
  • a method for preparing a gradient ultra-fine cemented carbide tool having an alumina-based composite coating comprising preparing a tool base and preparing an alumina-based composite coating on a surface of the tool base is provided.
  • the cemented carbide substrate precursor is prepared by four steps of sintering.
  • cemented carbide precursor precursor after the finish grinding process is subjected to gradient sintering to prepare a cemented carbide tool base with surface cobalt-depleted and cubic phase-rich structure.
  • the preparation process of the alumina composite coating is as follows: a TiAlN layer as a transition layer is prepared on the surface of the tool substrate, a TiAlN/Al 2 O 3 layer as a support layer is deposited on the transition layer, and deposited on the support layer as wear resistance. a layer of ⁇ -Al 2 O 3 ;
  • the TiAlN layer as the transition layer and the TiAlN layer in the support layer are prepared by reactive sputtering of an Al-Ti alloy target in a mixed atmosphere of N 2 or Ar and N 2 , and the gas pressure during deposition is 0.1-2 Pa, the matrix
  • the temperature is 300-700 ° C, and the asymmetric bidirectional pulse power supply with alternating positive and negative poles is used to increase the bias voltage, wherein the negative electrode change ratio is 2-20%;
  • the Al 2 O 3 layer in the support layer is prepared by reactive sputtering of the Al target by bidirectional pulse DMS technology. Specifically, a symmetric bidirectional pulse power source is applied to both ends of the cathode target, and the cathode target material is a pure Al target, and the Al target is passed through the Al target. Reacting with O 2 in the atmosphere to form an Al 2 O 3 coating having a substrate temperature of 300-700 ° C or 1000-1015 ° C and a gas pressure of 0.1-2 Pa; a bidirectional pulse power supply with positive and negative bias applied to the cathode target The positive and negative bias ranges are 20-50V and 20-300V, respectively;
  • the ⁇ -Al 2 O 3 layer as a wear-resistant layer is prepared by reactive sputtering of an Al target by a bidirectional pulsed DMS technique, in particular, a symmetric bidirectional pulse power source is applied to both ends of the cathode target, and the material of the cathode target is a pure Al target.
  • the Al 2 O 3 coating is formed by reacting the Al target with O 2 in the atmosphere, the substrate temperature is 1000-1015 ° C, the gas pressure is 0.1-2 Pa, and the bidirectional pulse power source with positive and negative bias is applied to the cathode target.
  • the positive and negative bias ranges are 20-50V and 20-300V, respectively.
  • the gradient ultra-fine cemented carbide tool with the alumina-based composite coating prepared by the invention has good bonding property between the tool base and the alumina-based composite coating, and the overall cutter has good wear resistance and temperature resistance.
  • a method for preparing a gradient ultra-fine cemented carbide tool having an alumina-based composite coating comprising preparing a tool base and preparing an alumina-based composite coating on a surface of the tool base is provided.
  • the tool base is sintered from the following mass percent components: 5-15% TiC, 2-5% TaC, 10-15% alloy binder phase, and the balance is WC.
  • the alloy binder phase consists of the following mass percentages of powder: 0.5-5.5% Cr, 0.5-5.5% Mo, 0.5-5.5% B, 0.5-5.5% Al, 0.5-5.5% V, 0.5- 5.5% Y, 0.5-5.5% Si, the balance is Co, and the sum of the masses of Cr, Mo, B, Al, V, Y and Si in the alloy binder phase is 7-20 of the quality of the alloy binder phase. %.
  • the preparation method of the tool base comprises the following steps:
  • alloy binder phase Eight kinds of powders of Cr, Mo, B, Al, V, Y, Si and Co are weighed according to the mass percentage, and eight kinds of powders are uniformly mixed to obtain an alloy binder phase. Preferably eight powders are placed In the ball mill, the ball was ground by a cemented carbide ball for 72 hours, and the ball mill was suspended for 10 minutes after each ball mill for 1 hour to obtain an alloy binder phase.
  • the blank can be first press-molded by a molding machine to obtain a green body; and the green body is further pressed by a cold isostatic press to obtain a green body.
  • the blank is placed in a sintering furnace, heated to 1200-1250 ° C at a rate of 5-8 ° C / min, maintained for 18-22 min, and maintained at a vacuum below 10 -3 Pa; then into the sintering furnace Fill with nitrogen and raise the temperature to 1420-1450 ° C at 1-3 ° C / min, keep the pressure for 55-65 min and maintain the pressure above 0.2 MPa; then cool down to 1000-1200 ° C at 2-6 ° C / min, The temperature is maintained for 110-130 min, and the pressure of 0.2 MPa or more is maintained; then the green body is cooled with the furnace and maintained at a pressure of 0.2 MPa or more to obtain a surface hardened gradient cemented carbide.
  • a pre-sintering step is performed in which the green body is placed in a sintering furnace and sintered at 1400 ° C for 10 min under an inert gas atmosphere; the green body is refined with the furnace to refine the shape of the green body.
  • the cemented carbide substrate prepared by the method has excellent mechanical properties and improves the red hardness of the cemented carbide.
  • the grain in the cemented carbide matrix is small, which is the normal tissue layer; the surface layer of the cemented carbide is rich in cubic phase and the binder phase is lean in cobalt-rich cubic phase, and there is a transition layer rich in alloyed binder phase under the surface layer. Cobalt transition layer, so that the cemented carbide has excellent hardness, wear resistance and toughness.
  • the alloy substrate After the alloy substrate is prepared, it is chemically cleaned, and then an alumina-based composite coating is deposited on the surface thereof.
  • the preparation process of the alumina composite coating is as follows: a TiAlN layer as a transition layer is prepared on the surface of the tool substrate, a TiAlN/Al 2 O 3 layer as a support layer is deposited on the transition layer, and deposited on the support layer as wear resistance. layer ⁇ -Al 2 O 3 layer;
  • the TiAlN layer as the transition layer and the TiAlN layer in the support layer are prepared by reactive sputtering of an Al-Ti alloy target in a mixed atmosphere of N 2 or Ar and N 2 , and the gas pressure during deposition is 0.1-2 Pa, the matrix
  • the temperature is 300-700 ° C, and the asymmetric bidirectional pulse power supply with alternating positive and negative poles is used to increase the bias voltage, wherein the negative electrode change ratio is 2-20%;
  • the Al 2 O 3 layer in the support layer is prepared by reactive sputtering of the Al target by bidirectional pulse DMS technology. Specifically, a symmetric bidirectional pulse power source is applied to both ends of the cathode target, and the cathode target material is a pure Al target, and the Al target is passed through the Al target. Reacting with O 2 in the atmosphere to form an Al 2 O 3 coating having a substrate temperature of 300-700 ° C or 1000-1015 ° C and a gas pressure of 0.1-2 Pa; a bidirectional pulse power supply with positive and negative bias applied to the cathode target The positive and negative bias ranges are 20-50V and 20-300V, respectively;
  • the ⁇ -Al 2 O 3 layer as a wear-resistant layer is prepared by reactive sputtering of an Al target by a bidirectional pulsed DMS technique, in particular, a symmetric bidirectional pulse power source is applied to both ends of the cathode target, and the material of the cathode target is a pure Al target.
  • the Al 2 O 3 coating is formed by reacting the Al target with O 2 in the atmosphere, the substrate temperature is 1000-1015 ° C, the gas pressure is 0.1-2 Pa, and the bidirectional pulse power source with positive and negative bias is applied to the cathode target.
  • the positive and negative bias ranges are 20-50V and 20-300V, respectively.
  • the gradient ultra-fine cemented carbide tool with the alumina-based composite coating prepared by the invention has good bonding property between the tool base and the alumina-based composite coating, and the overall cutter has good wear resistance and temperature resistance.
  • An alumina-based composite coating for a gradient ultra-fine cemented carbide tool having the same structure as the alumina-based composite coating of any of embodiments 1-3, including for deposition on a surface of a tool substrate a TiAlN layer of the transition layer, a TiAlN/Al 2 O 3 layer deposited as a support layer on the transition layer, and an ⁇ -Al 2 O 3 layer deposited as a wear layer on the support layer, the TiAlN/Al 2 O 3 layer It is composed of a TiAlN layer and an Al 2 O 3 layer alternately.
  • Preparing an alumina composite coating comprising sequentially preparing a TiAlN layer as a transition layer on a surface of a tool substrate, depositing a TiAlN/Al 2 O 3 layer as a support layer on the transition layer, and depositing ⁇ as a wear layer on the support layer -Al 2 O 3 layer.
  • the TiAlN layer as the transition layer and the TiAlN layer in the support layer are prepared by reactive sputtering of an Al-Ti alloy target in a mixed atmosphere of N 2 or Ar and N 2 , and the gas pressure during deposition is 0.1-2 Pa, the matrix
  • the temperature is 300-700 ° C, and the asymmetric bidirectional pulse power supply with alternating positive and negative poles is used to increase the bias voltage, wherein the negative electrode change ratio is 2-20%.
  • the Al 2 O 3 layer in the support layer is prepared by reactive sputtering of the Al target by bidirectional pulse DMS technology. Specifically, a symmetric bidirectional pulse power source is applied to both ends of the cathode target, and the cathode target material is a pure Al target, and the Al target is passed through the Al target. Reacting with O 2 in the atmosphere to form an Al 2 O 3 coating having a substrate temperature of 300-700 ° C or 1000-1015 ° C and a gas pressure of 0.1-2 Pa; a bidirectional pulse power supply with positive and negative bias applied to the cathode target The positive and negative bias ranges are 20-50V and 20-300V, respectively.
  • the ⁇ -Al 2 O 3 layer as a wear-resistant layer is prepared by reactive sputtering of an Al target by a bidirectional pulsed DMS technique, in particular, a symmetric bidirectional pulse power source is applied to both ends of the cathode target, and the material of the cathode target is a pure Al target.
  • the Al 2 O 3 coating is formed by reacting the Al target with O 2 in the atmosphere, the substrate temperature is 1000-1015 ° C, the gas pressure is 0.1-2 Pa, and the bidirectional pulse power source with positive and negative bias is applied to the cathode target.
  • the positive and negative bias ranges are 20-50V and 20-300V, respectively.
  • the alumina-based composite coating prepared by the invention has good bonding property with the tool base, and the adhesion between the coating layers of the composite coating is good, and the high temperature resistance, corrosion resistance and wear resistance are good.

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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)
  • Inorganic Chemistry (AREA)
  • Cutting Tools, Boring Holders, And Turrets (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

La présente invention concerne un outil de coupe en alliage dur ultrafin à structure étagée pourvu d'un revêtement composite d'oxyde d'aluminium, comprenant un corps de base d'outil de coupe et un revêtement composite d'oxyde d'aluminium disposé sur le corps de base d'outil de coupe. Le corps de base d'outil de coupe comprend, depuis la couche intérieure jusqu'à la couche extérieure et dans cet ordre : une couche normalement organisée, une couche de transition riche en cobalt et une couche de phase riche en structures cubiques et pauvre en cobalt. Le revêtement composite d'oxyde d'aluminium comprend une couche de TiAlN déposée sur la surface de la phase riche en structures cubiques et pauvre en cobalt en tant que couche de transition, une couche de TiAlN/Al2O3 déposée sur la couche de transition comme couche de support, et une couche d'α-Al2O3 déposée sur la couche de support. La couche de TiAlN/Al2O3 est composée de couches alternées de TiAlN et d'Al2O3. L'invention concerne en outre un revêtement composite d'oxyde d'aluminium pour un outil de coupe en alliage dur ultrafin à structure étagée, un procédé de fabrication de l'outil de coupe en alliage dur ultrafin à structure étagée pourvu du revêtement composite d'oxyde d'aluminium, et un procédé de fabrication du revêtement composite d'oxyde d'aluminium.
PCT/CN2016/075333 2016-02-11 2016-03-02 Revêtement composite d'oxyde d'aluminium, outil de coupe en alliage dur ultrafin à structure étagée pourvu du revêtement composite et procédé de fabrication associé WO2017136968A1 (fr)

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CN117587405A (zh) * 2024-01-16 2024-02-23 宁波爱柯迪科技产业发展有限公司 一种压铸模具用防铝液黏附抗冲蚀复合涂层及其制备方法
CN117821913A (zh) * 2024-03-06 2024-04-05 欧优格(大连)切削工具有限公司 一种应用于合金刀具的多层多元纳米复合硬质涂层

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