US20120015148A1 - Alumina layer with enhanced texture - Google Patents
Alumina layer with enhanced texture Download PDFInfo
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- US20120015148A1 US20120015148A1 US13/135,339 US201113135339A US2012015148A1 US 20120015148 A1 US20120015148 A1 US 20120015148A1 US 201113135339 A US201113135339 A US 201113135339A US 2012015148 A1 US2012015148 A1 US 2012015148A1
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- cutting tool
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23B—TURNING; BORING
- B23B27/00—Tools for turning or boring machines; Tools of a similar kind in general; Accessories therefor
- B23B27/14—Cutting tools of which the bits or tips or cutting inserts are of special material
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical 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 deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/36—Carbonitrides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23B—TURNING; BORING
- B23B27/00—Tools for turning or boring machines; Tools of a similar kind in general; Accessories therefor
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
- C04B41/5031—Alumina
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical 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 deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical 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 deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/403—Oxides of aluminium, magnesium or beryllium
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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
- C23C30/00—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process
- C23C30/005—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process on hard metal substrates
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- 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
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24355—Continuous and nonuniform or irregular surface on layer or component [e.g., roofing, etc.]
- Y10T428/24372—Particulate matter
- Y10T428/24413—Metal or metal compound
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- 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
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24942—Structurally defined web or sheet [e.g., overall dimension, etc.] including components having same physical characteristic in differing degree
- Y10T428/2495—Thickness [relative or absolute]
- Y10T428/24967—Absolute thicknesses specified
- Y10T428/24975—No layer or component greater than 5 mils thick
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- 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
- Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
- Y10T428/252—Glass or ceramic [i.e., fired or glazed clay, cement, etc.] [porcelain, quartz, etc.]
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- 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
- Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
- Y10T428/263—Coating layer not in excess of 5 mils thick or equivalent
- Y10T428/264—Up to 3 mils
- Y10T428/265—1 mil or less
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- 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
- Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
- Y10T428/266—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension of base or substrate
Definitions
- the present invention relates to a coated cutting tool insert designed to be used in metal machining.
- the coating exhibits an excellent adhesion to the substrate covering all functional parts thereof.
- the coating is composed of one or more refractory layers of which at least one is an ⁇ -Al 2 O 3 layer strongly textured in the ⁇ 001> direction.
- ⁇ -Al 2 O 3 belongs to the trigonal crystal system and has a rhombohedrally centred hexagonal lattice, the space group symbol being R3 c.
- the crystal structure of ⁇ -Al 2 O 3 is often described as being composed of oxygen ions (A, B) in an approximate hcp (hexagonal close-packed) arrangement ( . . . ABAB . . .
- the aluminium cations can take three different vacancy positions in the oxygen lattice with the stacking sequence of . . . ⁇ . . . . These are usually referred to as c ⁇ , c ⁇ and c ⁇ .
- the unit cell of ⁇ -Al 2 O 3 comprises six layers of O and Al can be described in the following way: Ac ⁇ Bc 62 Ac ⁇ Bc ⁇ Ac ⁇ Bc ⁇ .
- texture has been controlled by modifying the chemistry of the nucleation surface.
- This approach does not provide complete nucleation control.
- the nucleation control is not complete, at least a portion of the produced ⁇ -Al 2 O 3 layers are formed via ⁇ -Al 2 O 3 ⁇ -Al 2 O 3 phase transformation.
- These kinds of ⁇ -Al 2 O 3 layers are composed of larger grains with transformation cracks. They exhibit much lower mechanical strength and ductility than textured ⁇ -Al 2 O 3 layers composed of ⁇ -Al 2 O 3 formed from 100% or near 100% nucleation. Consequently, there is a need to develop techniques to more precisely control the nucleation step and growth texture of ⁇ -Al 2 O 3 .
- 6,333,103 describes a modified method to control the nucleation and growth of ⁇ -Al 2 O 3 along the ⁇ 10(10)> direction.
- U.S. Pat. No. 6,869,668 describes a method to obtain a strong ⁇ 300> texture in ⁇ -Al 2 O 3 using a texture modifying agent (ZrCl 4 ).
- the prior-art processes discussed above all use deposition temperatures of about 1000° C.
- It is an object of the present invention is to provide an alumina layer providing improved physical properties to a cutting tool insert.
- a cutting tool insert comprising a substrate at least partially coated with a coating having a total thickness of from about 5 to about 40 ⁇ m, preferably 5-25 ⁇ m comprising one or more refractory layers of which at least one layer of which is an ⁇ -alumina layer wherein said ⁇ -alumina layer comprises columnar ⁇ -Al 2 O 3 grains with a ⁇ 001> growth direction.
- a method of making an ⁇ -Al 2 O 3 layer on a substrate which comprises the steps of nucleating said alumina in a temperature range of from about 750 to about 1000° C., and controlling both the nucleation and growth of ⁇ -alumina using sulphur-containing and at least one fluorine-containing precursor.
- FIG. 1 a shows SEM-image of a typical surface morphology of the layer according to this invention in 15000 ⁇ ;
- a coated cutting tool insert comprising a substrate and a coating to be used in metal machining. It has been surprisingly found that a ⁇ 001> texture can be deposited in a controlled way. It is characterised in the XRD pattern by a strong (006) peak. The alumina layer with strong ⁇ 001> texture outperforms prior art coatings with random or other controlled textures. Further, increased toughness can be obtained.
- the substrate comprises a hard material such as cemented carbide, cermets, ceramics, high speed steel or a superhard material such as cubic boron nitride (CBN) or diamond preferably cemented carbide or CBN.
- CBN cubic boron nitride
- the substrate is a cemented carbide with a binder phase enriched surface zone.
- ⁇ -Al 2 O 3 can be nucleated, for example, on Ti 2 O 3 surfaces, bonding layers of (Ti,Al)(C,O) or by controlling the oxidation potential using CO/CO 2 mixtures.
- the idea in all these approaches is that nucleation must not take place on the surfaces of TiC, TiN, Ti(C,N) or Ti(C,O,N) with fcc (face centered cubic) or in general on phases with cubic structure, otherwise ⁇ -Al 2 O 3 is obtained.
- the hard and wear resistant coating exhibits an excellent adhesion to the substrate covering all functional parts thereof. It is composed of one or more refractory layers of which at least one layer is a strongly textured ⁇ -Al 2 O 3 deposited on a bonding layer of (Ti,Al)(C,O,N) with increasing aluminium content towards the outer surface.
- the ⁇ -Al 2 O 3 layer is 1-45 ⁇ m composed of columnar grains with a strong ⁇ 001> texture.
- the length/width ratio of the alumina grains is from 2 to 15, preferably >5.
- the layer is characterised by a strong (006) diffraction peak, measured using XRD, and by low intensity of (012), (104), (113), (024) and (116) diffraction peaks.
- the texture coefficients (TC) for the ⁇ -Al 2 O 3 -layer is determined as follows:
- TC ⁇ ( hkl ) I ⁇ ( hkil ) I 0 ⁇ ( hkil ) ⁇ ⁇ 1 n ⁇ ⁇ I ⁇ ( hkil ) I 0 ⁇ ( hkil ) ⁇ - 1
- I 0 (hkl) standard intensity according to JCPDS card no 46-1212
- n number of reflections used in the calculation
- the (hkl) reflections used are: (012), (104), (110), (600), (113) and (116).
- the (024) reflection, which is the second-order reflection of (012), is omitted from the calculations.
- the texture of the alumina layer is defined as follows:
- TC(006)>1.4 preferably >3.0 and most preferably >4.0. This is a manifestation of a strong ⁇ 001> texture.
- the texture coefficients for (012), (104), (113), (024) and (116) diffraction peaks are less than 0.5, preferably less than 0.2 and most preferably less than 0.1.
- the coating comprises a first layer adjacent the substrate of CVD Ti(C,N), CVD TiN, CVD TiC, MTCVD Ti(C,N), MTCVD Zr(C,N), MTCVD Ti(B,C,N), CVD HfN or combinations thereof preferably of Ti(C,N) having a thickness of from 1 to 20 preferably from 1 to 10 ⁇ m.
- the ⁇ -Al 2 O 3 layer is the uppermost layer.
- this layer has a thickness of from about 1 to 20 ⁇ m, preferably 2 to 8 ⁇ m.
- the coating includes a layer of ⁇ -Al 2 O 3 and/or ⁇ -Al 2 O 3 preferably atop the ⁇ -Al 2 O 3 with a thickness of from 0.5 to 10, preferably from 1 to 5 ⁇ m.
- the present invention also relates to a refined method to produce textured ⁇ -Al 2 O 3 layers in a temperature range of 950-1000° C., preferably at 1000° C. with a controlled ⁇ 001> texture.
- the ⁇ -Al 2 O 3 layer is deposited on a bonding layer of (Ti,Al)(C,O,N) with increasing aluminium content towards the outer surface.
- Ti(C,O) layer is deposited with controlled O-content.
- a very thin titanium oxide nucleation layer is obtained in the similar way as used in ALD (Atomic Layer Deposition).
- the procedure is as follows: (i) exposure of a first precursor TiCl 4 , preferably together with AlC 3 , (ii) purge (N 2 ), (iii) exposure of the second precursor (H 2 O), (iv) purge (N 2 ).
- the duration of the steps (i) and (iii) is 1-5 min, preferably 2 min each and the steps (ii) and (iv) 2-10 min, preferably 5 min each.
- the deposition of the ⁇ -Al 2 O 3 is started with a relatively long 30-120 min, preferably 60 min, nucleation step without sulphur- or fluorine containing compounds.
- ⁇ -Al 2 O 3 is grown to its desired thickness using sulphur-containing compounds H 2 S, or SO 2 , preferably H 2 S, optionally together with fluorine-containing compounds SF 6 or HF, preferably SF 6 .
- ⁇ 001> texture could be obtained by careful control of the ratio of sulphur containing dopants to CO 2 /CO.
- a strong ⁇ 001> growth texture can be obtained in a controlled way.
- the correct ratios depend on the type of deposition equipment, flow rate etc.
- An important difference compared with the prior-art is that the texture is controlled, in addition to the nucleation procedure, also during the growth of ⁇ -Al 2 O 3 itself.
- the described texture is thereby obtained when both the nucleation and growth are controlled correctly.
- the lack of control of both nucleation and growth is a possible explanation for the fact that the ⁇ 001> texture [(006) diffraction peak)] has heretofore been unknown.
- Cemented carbide cutting inserts with a composition of 5.9% Co and balance WC (hardness about 1600 HV) were coated with a layer of MTCVD Ti(C,N).
- the thickness of the MTCVD layer was about 2 ⁇ m.
- an ⁇ -Al 2 O 3 layer consisting of about 10 ⁇ m.
- Coating a The detailed process data is given below:
- Step 3 (optional ALD steps): a)TiCl 4 treatment b) N 2 -purge c) H 2 O treatment d) N 2 -purge
- Step 4 Nucleation step
- Coating a) was studied using X-ray diffraction.
- the texture coefficients of the ⁇ -Al 2 O 3 layers were determined and are presented in Table 1.
- a SEM micrograph of Coating a) in top view with ⁇ 001> texture is shown in FIG. 1 a and in cross section in FIG. 1 b .
- the ⁇ -Al 2 O 3 layer was composed of columnar grains.
- the X-Ray diffraction pattern is shown in FIG. 2 .
- Coatings b) and c) with ⁇ 012> and ⁇ 104> textures were deposited according to the prior-art (coating thickness about 10 ⁇ m). The coatings were studied using X-ray diffraction. The texture coefficients of the ⁇ -Al 2 O 3 layers were determined and are presented in Table 2.
- Coating a), b) and c) deposited on Co-enriched substrates were tested with respect to toughness in longitudinal turning with interrupted cuts.
- Insert type CNMG120408-M3 Cutting speed: 140 m/min Feed: 0.1, 0.125, 0.16, 0.20, 0.25, 0.315, 0.4, 0.5, 0.63, 0.8 mm/rev gradually increased after 10 mm length of cut
- Tool life criteria Gradually increased feed until edge breakage. 10 edges of each variant were tested.
- the coatings a), b) and c) were tested with respect to edge chipping in longitudinal turning in cast iron.
- CBN Cubic boron nitride
- PCBN polycrystalline CBN
- Coating c) according to the invention shows the highest values of hardness and modulus, closely followed by coating c).
Abstract
The present invention relates to a coated cutting tool insert comprising a substrate and a coating to be used in metal machining. The hard and wear resistant coating exhibits an excellent adhesion to the substrate covering all functional parts thereof. The coating is composed of one or more refractory layers of which at least one layer is α-Al2O3 showing a strong growth texture along <001>. The α-Al2O3 layer has a thickness ranging from 1 to 20 μm and is composed of columnar grains with a length/width ratio of 2 to 15. The layer is characterised by a strong (006) diffraction peak, measured using XRD, and by low intensity of (012), (104), (113) (024) and (116) diffraction peaks. The <001>textured α-Al2O3 layers is deposited in a temperature range of 750-1000° C. The texture is controlled by a specific nucleation procedure combined with the use of sulphur- and fluorine containing dopants.
Description
- This application claims priority from Swedish application No. SE 0502115-9 filed Sep. 27, 2005 which is hereby incorporated by reference in its entirety.
- The present invention relates to a coated cutting tool insert designed to be used in metal machining. The coating exhibits an excellent adhesion to the substrate covering all functional parts thereof. The coating is composed of one or more refractory layers of which at least one is an α-Al2O3 layer strongly textured in the <001> direction.
- Techniques to deposit α-Al2O3 and κ-Al2O3 layers with nucleation control have been introduced on an industrial scale only recently, and it has clearly been shown that α-Al2O3 is the preferred phase in most metal cutting applications. According to the definition used in the International Tables of Crystallography, α-Al2O3 belongs to the trigonal crystal system and has a rhombohedrally centred hexagonal lattice, the space group symbol being R3 c. The crystal structure of α-Al2O3 is often described as being composed of oxygen ions (A, B) in an approximate hcp (hexagonal close-packed) arrangement ( . . . ABAB . . . ) with the aluminium anions occupying two thirds of the octahedral interstices. The aluminium cations can take three different vacancy positions in the oxygen lattice with the stacking sequence of . . . αβγαβγ . . . . These are usually referred to as cα, cβ and cγ. The unit cell of α-Al2O3 comprises six layers of O and Al can be described in the following way: AcαBc62 AcγBcαAcβBcγ. The JPDS card, defined hereinbelow, uses the hexagonal system and, consequently, four axes (hkil) are used where i=−(h+k). Often, the index i is omitted as done also in this case.
- It has been known in the art to use nucleation control in order to obtain various growth textures. As described in a recent publication (S. Ruppi, “Deposition, microstructure and properties of texture-controlled CVD α-Al2O3 coatings,” Int. J. Refractory Metals & Hard Materials 23(2005) pp.306-315) manipulation of the nucleation surfaces can be used to obtain the growth textures <012>, <104> or <003>. The commonly observed diffraction peaks from α-Al2O3 are (012), (104), (110), (113) and (116). However the diffraction peak (006), which is an indication of the <001> texture, is always missing, as indicated by its absence in XRD-patterns obtained from textured α-Al2O3 layers using known methods.
- Prior to the present invention, texture has been controlled by modifying the chemistry of the nucleation surface. This approach, however, does not provide complete nucleation control. When the nucleation control is not complete, at least a portion of the produced α-Al2O3 layers are formed via κ-Al2O3 →α-Al2O3 phase transformation. These kinds of α-Al2O3 layers are composed of larger grains with transformation cracks. They exhibit much lower mechanical strength and ductility than textured α-Al2O3 layers composed of α-Al2O3 formed from 100% or near 100% nucleation. Consequently, there is a need to develop techniques to more precisely control the nucleation step and growth texture of α-Al2O3.
- The control of the α-Al2O3 polymorph in industrial scale was achieved in the beginning of the 1990s with commercial products based on U.S. Pat. No. 5,137,774. Later modifications of this patent have been used to deposit α-Al2O3 with preferred textures. In U.S. Pat. No. 5,654,035 an alumina layer textured in the <012> direction and in U.S. Pat. No. 5,980,988 in the <110>direction are disclosed. In U.S. Pat. No. 5,863,640 a preferred growth either along <012>, or <104> or <110> is disclosed. U.S. Pat. No. 6,333,103 describes a modified method to control the nucleation and growth of α-Al2O3 along the <10(10)> direction. U.S. Pat. No. 6,869,668 describes a method to obtain a strong <300> texture in α-Al2O3 using a texture modifying agent (ZrCl4). The prior-art processes discussed above all use deposition temperatures of about 1000° C.
- US 2004/0028951A1 describes a technique to achieve a pronounced <012> texture. The commercial success of this kind of product demonstrates the importance to refine the CVD process of α-Al2O3 towards fully controlled textures.
- It is an object of the present invention is to provide an alumina layer providing improved physical properties to a cutting tool insert.
- It is another object of the invention to provide an alumina layer, as above, wherein the physical properties of the coated insert can be tailored through control of the nucleation and growth of an α-Al2O3 phase in the coating.
- These objects are achieved by a cutting tool insert comprising a substrate at least partially coated with a coating having a total thickness of from about 5 to about 40 μm, preferably 5-25 μm comprising one or more refractory layers of which at least one layer of which is an α-alumina layer wherein said α-alumina layer comprises columnar α-Al2O3 grains with a <001> growth direction.
- The objects of the invention are also achieved by a method of making an α-Al2O3 layer on a substrate which comprises the steps of nucleating said alumina in a temperature range of from about 750 to about 1000° C., and controlling both the nucleation and growth of α-alumina using sulphur-containing and at least one fluorine-containing precursor.
- For a fuller understanding of the invention, the following detailed description should be read in conjunction with the drawings, wherein:
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FIG. 1 a shows SEM-image of a typical surface morphology of the layer according to this invention in 15000×; - FIG 1 b shows the same layer in cross-section in 15000×; and FIG.2 shows an XRD pattern of an α-Al2O3-layer according to this invention for 2θ=20-70°.
- According to the present invention there is provided a coated cutting tool insert comprising a substrate and a coating to be used in metal machining. It has been surprisingly found that a <001> texture can be deposited in a controlled way. It is characterised in the XRD pattern by a strong (006) peak. The alumina layer with strong <001> texture outperforms prior art coatings with random or other controlled textures. Further, increased toughness can be obtained.
- The substrate comprises a hard material such as cemented carbide, cermets, ceramics, high speed steel or a superhard material such as cubic boron nitride (CBN) or diamond preferably cemented carbide or CBN. With CBN is herein meant a cutting tool material containing at least 40 vol-% CBN. In a preferred embodiment the substrate is a cemented carbide with a binder phase enriched surface zone.
- It has been experimentally confirmed that α-Al2O3 can be nucleated, for example, on Ti2O3 surfaces, bonding layers of (Ti,Al)(C,O) or by controlling the oxidation potential using CO/CO2 mixtures. The idea in all these approaches is that nucleation must not take place on the surfaces of TiC, TiN, Ti(C,N) or Ti(C,O,N) with fcc (face centered cubic) or in general on phases with cubic structure, otherwise κ-Al2O3 is obtained.
- Further, it has been noticed that enhanced performance can be obtained through optimising the texture of α-Al2O3. It is thus possible to enhance tool performance by tailoring the α-Al2O3 texture for different metal cutting applications and work piece materials.
- The hard and wear resistant coating exhibits an excellent adhesion to the substrate covering all functional parts thereof. It is composed of one or more refractory layers of which at least one layer is a strongly textured α-Al2O3 deposited on a bonding layer of (Ti,Al)(C,O,N) with increasing aluminium content towards the outer surface. The α-Al2O3 layer is 1-45 μm composed of columnar grains with a strong <001> texture. The length/width ratio of the alumina grains is from 2 to 15, preferably >5. The layer is characterised by a strong (006) diffraction peak, measured using XRD, and by low intensity of (012), (104), (113), (024) and (116) diffraction peaks. The texture coefficients (TC) for the α-Al2O3-layer is determined as follows:
-
- where
- I(hkl)=intensity of the (hid) reflection
- I0(hkl)=standard intensity according to JCPDS card no 46-1212
- n=number of reflections used in the calculation
- The (hkl) reflections used are: (012), (104), (110), (600), (113) and (116). The (024) reflection, which is the second-order reflection of (012), is omitted from the calculations.
- The texture of the alumina layer is defined as follows:
- TC(006)>1.4, preferably >3.0 and most preferably >4.0. This is a manifestation of a strong <001> texture. The texture coefficients for (012), (104), (113), (024) and (116) diffraction peaks are less than 0.5, preferably less than 0.2 and most preferably less than 0.1.
- More particularly, the coating comprises a first layer adjacent the substrate of CVD Ti(C,N), CVD TiN, CVD TiC, MTCVD Ti(C,N), MTCVD Zr(C,N), MTCVD Ti(B,C,N), CVD HfN or combinations thereof preferably of Ti(C,N) having a thickness of from 1 to 20 preferably from 1 to 10 μm. Preferably there is an intermediate layer of TiN between the substrate and said first layer with a thickness of <3 μm, preferably 0.5-2 μm.
- In one embodiment the α-Al2O3 layer is the uppermost layer. In another embodiment there is a layer of carbide, nitride, carbonitride or carboxynitride of one or more of Ti, Zr and Hf, having a thickness of from about 0.5 to 3 μm, preferably 0.5 to 1.5 μm atop the α-Al2O3 layer. Alternatively this layer has a thickness of from about 1 to 20 μm, preferably 2 to 8 μm.
- In yet another embodiment the coating includes a layer of κ-Al2O3 and/or γ-Al2O3 preferably atop the α-Al2O3 with a thickness of from 0.5 to 10, preferably from 1 to 5 μm.
- The present invention also relates to a refined method to produce textured α-Al2O3 layers in a temperature range of 950-1000° C., preferably at 1000° C. with a controlled <001> texture. The α-Al2O3 layer is deposited on a bonding layer of (Ti,Al)(C,O,N) with increasing aluminium content towards the outer surface. On to this layer a Ti(C,O) layer is deposited with controlled O-content. A very thin titanium oxide nucleation layer is obtained in the similar way as used in ALD (Atomic Layer Deposition). The procedure is as follows: (i) exposure of a first precursor TiCl4, preferably together with AlC3, (ii) purge (N2), (iii) exposure of the second precursor (H2O), (iv) purge (N2). The duration of the steps (i) and (iii) is 1-5 min, preferably 2 min each and the steps (ii) and (iv) 2-10 min, preferably 5 min each. The deposition of the α-Al2O3 is started with a relatively long 30-120 min, preferably 60 min, nucleation step without sulphur- or fluorine containing compounds. α-Al2O3 is grown to its desired thickness using sulphur-containing compounds H2S, or SO2, preferably H2S, optionally together with fluorine-containing compounds SF6 or HF, preferably SF6.
- It has been found, quite unexpectedly, that <001> texture could be obtained by careful control of the ratio of sulphur containing dopants to CO2/CO. When α-Al2O3 is nucleated correctly, followed by a deposition process using relatively low amounts of these dopants (0.5-1.2%) together with a CO+CO2 gas mixture where CO=0.5-2×CO2, a strong <001> growth texture can be obtained in a controlled way. The correct ratios depend on the type of deposition equipment, flow rate etc. An important difference compared with the prior-art is that the texture is controlled, in addition to the nucleation procedure, also during the growth of α-Al2O3 itself. The described texture is thereby obtained when both the nucleation and growth are controlled correctly. The lack of control of both nucleation and growth is a possible explanation for the fact that the <001> texture [(006) diffraction peak)] has heretofore been unknown.
- The following is a detailed description of a preferred sequence of nucleation steps.
-
- 1. Depositing a bonding layer 0.1-1 μm thick in a gas mixture of 2-3% TiCl4 and AlCl3 increasing from 0.5 to 6%, 3-10% CO, 1-3% CO2, 0.2-1.0% CH3CN, 0.2-1.0%, 2-10% N2 and balance H2 at about 750-1000° C., preferably at 800° C. and at a pressure of 50-200 mbar.
- 2. Purging by N2 for 5 min.
- 3. Treating the bonding layer in a gas mixture of 5-15% TiCl4 and 5-20% CO, 0.5-3% CO2 and 10-20% Ar in hydrogen for 5-15, preferably 10, minutes min at 950-1000° C., preferably at 1000° C. and at a pressure of 50-200 mbar.
- 4. Purging by N2 for 5 min.
- 5. Treating the bonding layer in a gas mixture of 8-15% TiCl4 and 0.5-2% AlCl3 in hydrogen for 5-15 min at about 950 to about 1000° C., preferably at about 1000° C. and at a pressure of from about 50 to about 200 mbar.
- 6. Treating in a gas mixture of 0.05 to 0.5% H2O, preferably 0.01%, balance H2.
- 7. Purging by N2 for 5 min.
- 8. Nucleation of the alumina layer at a temperature of 950-1000° C. with desired thickness according to known technique or depositing an alumina layer at 950-1000° C. without any catalysing precursors.
- 9. Deposition of the alumina layer at a temperature of 950-1000° C. to the desired thickness at 950-1000° C. at deposition pressures 50-200 mbar using 0.01-0.05% H2S or SO2, preferably H2S and 0.01-0.02% SF6 or HF, preferably SF6 as catalysing agents. CO2 1.0-4.5% is used as the oxygen donor together with CO, maintaining CO=2×CO2.
- Cemented carbide cutting inserts with a composition of 5.9% Co and balance WC (hardness about 1600 HV) were coated with a layer of MTCVD Ti(C,N). The thickness of the MTCVD layer was about 2 μm. On to this layer an α-Al2O3 layer consisting of about 10 μm. α-Al2O3 was deposited according to this invention referred to as Coating a). The detailed process data is given below:
- Step 1:
Bonding layer 1 -
Gas mixture TiCl4 = 2.8% CH3CN = 0.7% AlCl3 = increasing from 0.8 to 5.4% CO = 8.8% CO2 = 2.2% N2 . . . = 5% Balance: H2 Duration 40 min Temperature 1000° C. Pressure 100 mbar - Step 2: N2 purge
- Step 3:Bonding layer 2
-
Gas mixture TiCl4 = 8% CO = 12% CO2 = 1.2% Ar . . . = 5% Balance: H2 Duration 2-10 min Temperature 1000° C. Pressure 100 mbar - Step 3: (optional ALD steps): a)TiCl4 treatment b) N2-purge c) H2O treatment d) N2-purge
-
a) TiCl4 = 9% AlCl3 = 1% H2 = balance 5 min . . . c) H2O = 0.1% H2 = balance 2 min . . . b, d) N2 = 100% 5 min Temperature 1000° C. Pressure 50 mbar - Step 4: Nucleation step
-
Gas mixture AlCl3 = 1.2% HCl . . . = 2.0% CO2 = 1.0-1.5% CO = 0.5-2.4% Balance H2 Duration 60 min Temperature 1000° C. Pressure 50 mbar - Step 5: Deposition
-
Gas mixture AlCl3 = 2.8% HCl = 3% CO2 = 1.8-2.5% CO = 0.9-.5% H2S = 0.05-1.0% Balance: H2 Duration 630 min Temperature 1000° C. Pressure 70 mbar - Coating a) was studied using X-ray diffraction. The texture coefficients of the α-Al2O3 layers were determined and are presented in Table 1. A SEM micrograph of Coating a) in top view with <001> texture is shown in
FIG. 1 a and in cross section inFIG. 1 b. The α-Al2O3 layer was composed of columnar grains. The X-Ray diffraction pattern is shown inFIG. 2 . -
TABLE 1 hkl Coating a) 012 0.01 104 0.06 110 0.01 006 5.91 113 0.00 116 0.02 - For reference Coatings b) and c) with <012> and <104> textures were deposited according to the prior-art (coating thickness about 10 μm). The coatings were studied using X-ray diffraction. The texture coefficients of the α-Al2O3 layers were determined and are presented in Table 2.
-
TABLE 2 hkl Coating a), invention Coating b) Coating c) 012 0.03 5.15 0.16 104 0.06 0.13 4.27 110 0.01 0.10 0.08 600 5.88 0.00 0.09 113 0.00 0.18 0.66 116 0.02 0.44 0.74 - Coating a), b) and c) deposited on Co-enriched substrates were tested with respect to toughness in longitudinal turning with interrupted cuts.
- Work piece: Cylindrical slotted bar
- Insert type: CNMG120408-M3
Cutting speed: 140 m/min
Feed: 0.1, 0.125, 0.16, 0.20, 0.25, 0.315, 0.4, 0.5, 0.63, 0.8 mm/rev gradually increased after 10 mm length of cut - Remarks: dry turning
- Tool life criteria: Gradually increased feed until edge breakage. 10 edges of each variant were tested.
- The inserts were inspected after 2 and 4 minutes of cutting. As clear from Table 3 the edge toughness was considerably enhanced when the layer was produced according to this invention.
-
TABLE 3 Mean feed at Experimental coating breakage (mm/rev) Coating a (006), 0.50 according to the invention Coating b (012) 0.22 Coating c (104) 0.36 - The test results show (Table 3) that the coating according to the invention (Coating a) exhibited clearly better toughness behaviour than the prior-art (Coatings b and c).
- The coatings a), b) and c) were tested with respect to edge chipping in longitudinal turning in cast iron.
- Work piece: Cylindrical bar
- Material: SS0130
- Insert type: SNUN
- Cutting speed: 400 m/min
- Feed: 0.4 mm/rev
- Depth of cut: 2.0 mm
- Remarks: dry turning
- The inserts were inspected after 2 and 4 minutes of cutting. As clear from Table 4 the edge toughness of the prior art product was considerably enhanced when the coating was produced according to this invention.
-
TABLE 4 Flaking of the Flaking of the edge line (%) edge line (%) after 2 minutes after 6 minutes Coating a (Invention) 0 5 Coating b 0 18 Coating c 5 10 - Cubic boron nitride (CBN) insert containing about 90% of polycrystalline CBN (PCBN) were coated according to this invention and according to prior art Coating b). The coated CBN was compared with uncoated CBN insert in cutting of steel containing ferrite. It is known that B has a high affinity to ferrite and diffusion wear occurs at high cutting speeds.
- Work piece: Cylindrical bar
- Material: SS0130
- Insert type: SNUN
- Cutting speed: 800 m/min
- Feed: 0.4 mm/rev
- Depth of cut: 2.5 mm
- Remarks: dry turning
-
TABLE 5 Life time (min) Coated CBN, Invention 23 Coated CBN, prior art, 14 012 texture Uncoated CBN 9 - As is evident from Table 5 the coating according to this invention is superior to the prior art.
- The hardness and Young's modulus of the coatings a)-c) together with κ-Al2O3 and older prior-art α-Al2O3 were measured using nanoindentation. The results are shown in Table 6.
-
TABLE 6 Hardness Young's (GPa) Modulus (GPa) Coating a 28.92 444.42 Coating b 27.31 419.53 Coating c 28.81 441.17 Prior-art α-Al2O3 (no texture) 25.79 385.45 κ-Al2O3 23.64 339.51 - Coating c) according to the invention shows the highest values of hardness and modulus, closely followed by coating c).
Claims (20)
1. A cutting tool insert comprising a substrate at least partially coated with a coating having a total thickness of from about 5 to about 40 comprising one or more refractory layers of which at least one layer of which is an α-alumina layer wherein said α-alumina layer comprises columnar α-Al2O3 grains with a <001> growth direction with texture coefficients
a) TC(006)>1.4, preferably >3.0 and most preferably >4.0.
the texture coefficient TC(hkl) being defined as
wherein
I(hkl)=measured intensity of the (hkl) reflection
I0(hkl)=standard intensity according to JCPDS card no 46-1212
n=number of reflections used in the calculation
(hkl) reflections used are: (012), (104), (110), (006), (113) and (116).
2. Cutting tool insert according to claim 1 , wherein said at least one layer is an as deposited layer of α-alumina.
3. Cutting tool insert according to claim 1 , wherein said alumina columnar grains have a length/width ratio from about 2 to about 15.
4. Cutting tool insert according to claim 1 , wherein said substrate comprises cemented carbide with a binder phase enriched surface zone, CBN or sintered CBN alloy.
5. Cutting tool insert according to claim 1 , wherein the coating comprises a first layer adjacent the body of CVD Ti(C,N), CVD TiN, CVD TiC, MTCVD Ti(C,N), MTCVD Zr(C,N), MTCVD Ti(B,C.N), CVD HfN or combinations thereof preferably of Ti(C,N) having a thickness of from 1 to 20 μm, and said α-Al2O3 layer adjacent said first layer having a thickness of from about 1 to about 40 μm, preferably from about 1 to about 20 μm, most preferably from about 1 to about 10 μm.
6. Cutting tool insert according to claim 1 , wherein the α-Al2O3 layer is the uppermost layer.
7. Cutting tool insert according to claim 1 , wherein a layer of carbide, nitride, carbonitride or carboxynitride of one or more of Ti, Zr and Hf, having a thickness of from about 0.5 to 3 μm, preferably from about 0.5 to about 1.5 μm atop the α-Al2O3 layer.
8. Cutting tool insert according to claim 1 , wherein a layer of carbide, nitride, carbonitride or carboxynitride of one or more of Ti, Zr and Hf, having a thickness of from about 1 to 20 μm, preferably 2 to 8 μm atop the α-Al2O3 layer.
9. Cutting tool insert according to claim 1 , wherein a layer of κ-Al2O3 or γ-Al2O3 atop the α-Al2O3 with a thickness of from 0.5 to 10 μm, preferably from 1 to 5 μm.
10. Cutting tool insert according to claim 1 , wherein a layer of TiN between the substrate and said first layer with a thickness of <3 μm, preferably 0.5-2 μm.
11. Cutting tool insert according to claim 1 , wherein said coating has a total thickness of from about 5 to about 25 μm.
12. Cutting tool insert according to claim 1 , wherein said alumina columnar grains have a length/width ratio from about 5 to about 10.
13. Cutting tool insert according to claim 1 , wherein said first layer adjacent the body having a thickness of from 1 to 10 μm.
14. Cutting tool insert according to claim 1 , wherein said α-Al2O3 layer adjacent said first layer has a thickness of from about 1 to about 20 μm.
15. Cutting tool insert according to claim 1 , wherein said α-Al2O3 layer adjacent said first layer has a thickness of from about 1 to about 10 μm.
16. A cutting tool insert comprising a substrate at least partially coated with a coating having a total thickness of from about 5 to about 40 μm, preferably 5-25 μm comprising one or more refractory layers of which at least one layer of which is an α-alumina layer wherein said α-alumina layer comprises columnar α-Al2O3 grains with a <001> growth direction with texture coefficients
a) TC(006)>1.4, preferably >3.0 and most preferably >4.0.
the texture coefficient TC(hkl) being defined as
wherein
I(hkl)=measured intensity of the (hid) reflection
I0(hkl)=standard intensity according to JCPDS card no 46-1212
n=number of reflections used in the calculation
(hkl) reflections used are: (012), (104), (110), (006), (113) and (116), and
wherein said α-alumina layer is formed by controlling both the nucleation and growth of α-alumina using sulphur-containing and at least one fluorine-containing precursor.
17. Cutting tool insert according to claim 16 , wherein said at least one sulphur-containing precursor is selected from the group consisting of H2S, SF6, SO2, SF6 and mixtures thereof.
18. A method of making an α-Al2O3 layer on a substrate, comprising the steps of:
nucleating said alumina in a temperature range of from about 750 to about 1000° C., and controlling both the nucleation and growth of α-alumina using sulphur-containing and at least one fluorine-containing precursor.
19. Method according to claim 18 , wherein said at least one sulphur-containing precursor is selected from the group consisting of H2S, SF6, SO2, SF6 and mixtures thereof.
20. Method according to claim 18 , wherein said at least one sulphur-containing precursor comprises a mixture of H2S and SF6.
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Also Published As
Publication number | Publication date |
---|---|
CZ2006607A3 (en) | 2008-02-27 |
US7993742B2 (en) | 2011-08-09 |
CZ305851B6 (en) | 2016-04-13 |
SE0502115L (en) | 2007-03-28 |
BRPI0603957A (en) | 2007-08-21 |
CN1939715B (en) | 2010-06-23 |
US20070104945A1 (en) | 2007-05-10 |
KR101314504B1 (en) | 2013-10-07 |
CN1939715A (en) | 2007-04-04 |
SE529051C2 (en) | 2007-04-17 |
KR20070035454A (en) | 2007-03-30 |
JP2007125686A (en) | 2007-05-24 |
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