Coated cutting tool
09725811 · 2017-08-08
Assignee
Inventors
Cpc classification
B23B27/148
PERFORMING OPERATIONS; TRANSPORTING
C23C30/00
CHEMISTRY; METALLURGY
International classification
B23B27/14
PERFORMING OPERATIONS; TRANSPORTING
Abstract
A coated cutting tool has a substrate and a coating layer. At least one layer of the coating layer is a coarse grain layer with an average layer thickness of 0.2 to 10 μm and an average grain diameter in excess of 200 nm measured at the direction parallel to the interface of the coating layer. A composition of the layer is represented by (Al.sub.aTi.sub.bM.sub.c)X, wherein M represents at least one of Zr, Hf, V, Nb, Ta, Cr, Mo, W, Y, B and Si, X represents at least one of C, N and O, and a, b and c represents atomic ratios of Al, Ti and M relative to one another such that 0.30≦a≦0.65, 0.35≦0.70, 0≦c≦0.20 and a+b+c=1.
Claims
1. A coated cutting tool which comprises a substrate and a coating layer formed on a surface of the substrate, at least one layer of the coating layer being a coarse grain layer having an average grain diameter Lx measured at a direction parallel to an interface of the coating layer and the substrate exceeding 200 nm, and a composition of which being represented by (Al.sub.aTi.sub.bM.sub.c)X, wherein: a grain diameter ratio (Ly/Lx) of an average grain diameter Ly of the coarse grain layer measured at a direction perpendicular to an interface between the coating layer and the substrate to said average grain diameter Lx of the coarse grain layer measured at a direction parallel to an interface between the coating layer and the substrate is 0.7 or more and less than 1.5, M represents at least one kind of an element(s) selected from the group consisting of Zr, Hf, V, Nb, Ta, Cr, Mo, W, Y, B and Si, X represents at least one kind of an element(s) selected from the group consisting of C, N and O, a represents an atomic ratio of an Al element based on a total of the Al element, a Ti element and an M element, b represents an atomic ratio of a Ti element based on a total of an Al element, the Ti element and an M element, c represents an atomic ratio of an M element based on a total of an Al element, a Ti element and the M element, a, b and c each satisfy 0.30≦a≦0.65, 0.35≦b≦0.70, 0≦c≦0.20 and a+b+c=1, and an average layer thickness of the coarse grain layer being 0.2 to 10 μm.
2. The coated cutting tool according to claim 1, wherein a, b and c each satisfy 0.30≦a≦0.50, 0.50≦b≦0.70, 0≦c≦0.20 and a+b+c=1.
3. The coated cutting tool according to claim 1, wherein X of the coarse grain layer represents N.
4. The coated cutting tool according claim 1, wherein an average grain diameter Lx of the coarse grain layer measured at a direction parallel to an interface of the coating layer and the substrate is in the range of 400 nm to 1,000 nm.
5. The coated cutting tool according to claim 1, wherein the coarse grain layer is cubic.
6. The coated cutting tool according to claim 5, wherein a full width at half maximum intensity (FWHM) of an X-ray diffraction peak of a (200) plane of the coarse grain layer is 0.6° or less.
7. The coated cutting tool according to claim 1, wherein the coating layer contains a lower layer formed on a surface of the substrate and a coarse grain layer formed on a surface of the lower layer, and the lower layer is a single layer or a multilayer containing at least one kind of a material(s) selected from a metal containing at least one kind of metallic elements selected from the group consisting of Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Y, Al and Si, and a compound containing at least one kind of these metallic elements and at least one kind of nonmetallic elements selected from the group consisting of carbon, nitrogen, oxygen and boron.
8. The coated cutting tool according to claim 1, wherein the coarse grain layer is an uppermost layer.
9. A coated cutting tool which comprises a substrate and a coating layer formed on a surface of the substrate, at least one layer of the coating layer being a coarse grain layer having an average grain diameter Lx measured at a direction parallel to an interface between the coating layer and the substrate exceeding 200 nm, and a composition of which being represented by (Al.sub.dCr.sub.eL.sub.f)Z, wherein: a grain diameter ratio (Ly/Lx) of an average grain diameter Ly of the coarse grain layer measured at a direction perpendicular to an interface between the coating layer and the substrate to said average grain diameter Lx of the coarse grain layer measured at a direction parallel to an interface between the coating layer and the substrate is 0.7 or more and less than 1.5, L represents at least one kind of an element(s) selected from the group consisting of Ti, Zr, Hf, V, Nb, Ta, Mo, W, Y, B and Si, Z represents at least one kind of an element(s) selected from the group consisting of C, N and O, d represents an atomic ratio of an Al element based on a total of the Al element, a Cr element and an L element, e represents an atomic ratio of a Cr element based on a total of an Al element, the Cr element and an L element, f represents an atomic ratio of an L element based on a total of an Al element, a Cr element and the L element, d, e and f each satisfy 0.25≦d≦0.70, 0.30≦e≦0.75, 0≦f<0.20 and d+e+f=1, and an average layer thickness of the coarse grain layer being 0.2 to 10 μm.
10. The coated cutting tool according to claim 9, wherein d, e and f each satisfy 0.40≦d≦0.70, 0.30≦e≦0.50, 0≦f≦0.20, d≧e and d+e+f=1.
11. The coated cutting tool according to claim 9, wherein Z of the coarse grain layer represents N.
12. The coated cutting tool according to claim 9, wherein an average grain diameter Lx of the coarse grain layer measured at a direction parallel to an interface between the coating layer and the substrate is in the range of 400 nm to 1,000 nm.
13. The coated cutting tool according to claim 9, wherein the coarse grain layer is cubic.
14. The coated cutting tool according to claim 13, wherein a full width at half maximum intensity (FWHM) of an X-ray diffraction peak at a (200) plane of the coarse grain layer is 0.6° or less.
15. The coated cutting tool according to claim 9, wherein the coating layer contains a lower layer formed on a surface of the substrate and a coarse grain layer formed on a surface of the lower layer, and the lower layer is a single layer or a multilayer containing at least one kind of a material(s) selected from a metal containing at least one kind of metallic elements selected from the group consisting of Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, W, Y, Al and Si, and a compound containing at least one kind of these metallic elements and at least one kind of nonmetallic elements selected from the group consisting of carbon, nitrogen, oxygen and boron.
16. The coated cutting tool according to claim 9, wherein the coarse grain layer is an uppermost layer.
Description
BRIEF EXPLANATION OF THE DRAWINGS
(1)
(2)
(3)
(4)
(5)
EXAMPLE 1
(6) As a substrate, a cemented carbide corresponding to P20 having an insert shape of ISO standard SEKN1203AGTN was prepared. In a reaction vessel of an arc ion plating device, a metal evaporation source which became a starting material of a coating layer shown in Table 1 and Table 2 was set, and the substrate was attached to a sample holder in the reaction vessel of the arc ion plating device. A pressure in the reaction vessel was made vacuum of 1×10.sup.31 2 Pa or less, and the substrate was heated to a temperature of 500° C. by a heater in the vessel. After the temperature of the substrate became 500° C., an Ar gas was introduced until a pressure in the reaction vessel became 5 Pa, and an atmosphere in the reaction vessel was made an Ar atmosphere. A pressure in the reaction vessel was made 5 Pa, and an Ar ion bombardment treatment was subjected to the substrate under ion bombardment conditions in which a bias voltage of −1000V was applied.
(7) After the Ar ion bombardment treatment, the Ar gas was discharged and a pressure in the reaction vessel was made vacuum of 1×10.sup.31 2 Pa or less. With regard to Sample Nos. 1 to 16 and 19 to 36, an N.sub.2 gas was introduced into the reaction vessel to make a nitrogen atmosphere with a pressure of 3 Pa in the reaction vessel. With regard to Sample Nos. 17 and 18, a mixed gas in which an N.sub.2 gas and a CH.sub.4 gas were mixed so that a partial pressure ratio thereof became N.sub.2:CH.sub.4=1:1 was introduced into the reaction vessel to make a mixed gas atmosphere with a pressure of 3 Pa in the reaction vessel. Next, the substrate was heated until a temperature of the substrate became those shown in Table 1 and Table 2 by a heater in the vessel. A bias voltage applied to the substrate was made −50V, a magnetic flux density at the center of the metal evaporation source was made the magnetic flux density shown in Table 1 and Table 2, and a coating layer shown in Table 1 and Table 2 was each formed on the surface of the substrate under the coating conditions in which an arc current was made 150A. After forming the coating layer, the sample was cooled, and the temperature of the sample became 100° C. or lower, then, the sample was taken out from the reaction vessel.
(8) TABLE-US-00001 TABLE 1 Coating layer Average Average grain grain diameter diameter Lx at Ly at Coating direction direction Grain conditions parallel perpendicular diameter Magnetic to interface to interface ratio Average flux Substrate of of (Ly/Lx) layer Sample density temperature substrate substrate of Ly to thickness No. (mT) (° C.) Composition (nm) (nm) Lx (μm) Present 1 10 500 (Al.sub.0.30Ti.sub.0.70)N 620 180 0.29 0.2 product 2 10 500 (Al.sub.0.30Ti.sub.0.70)N 620 456 0.74 0.5 3 10 500 (Al.sub.0.30Ti.sub.0.70)N 620 614 0.99 3.0 4 10 500 (Al.sub.0.30Ti.sub.0.70)N 620 883 1.42 10.0 5 10 500 (Al.sub.0.50Ti.sub.0.50)N 570 562 0.99 3.0 6 10 500 (Al.sub.0.25Cr.sub.0.75)N 590 168 0.28 0.2 7 10 500 (Al.sub.0.25Cr.sub.0.75)N 590 420 0.71 0.5 8 10 500 (Al.sub.0.25Cr.sub.0.75)N 590 576 0.98 3.0 9 10 500 (Al.sub.0.25Cr.sub.0.75)N 590 828 1.40 10.0 10 10 500 (Al.sub.0.50Cr.sub.0.50)N 450 468 1.04 3.0 11 10 500 (Al.sub.0.50Ti.sub.0.45W.sub.0.05)N 510 492 0.96 3.0 12 10 500 (Al.sub.0.50Cr.sub.0.45W.sub.0.05)N 480 398 0.83 3.0 13 10 500 (Al.sub.0.50Ti.sub.0.45Y.sub.0.05)N 430 396 0.92 3.0 14 10 500 (Al.sub.0.50Cr.sub.0.45Y.sub.0.05)N 410 324 0.79 3.0 15 10 500 (Al.sub.0.50Ti.sub.0.45Si.sub.0.05)N 430 408 0.95 3.0 16 10 500 (Al.sub.0.50Cr.sub.0.45Si.sub.0.05)N 410 336 0.82 3.0 17 10 500 (Al.sub.0.30Ti.sub.0.70)CN 550 564 1.03 3.0 18 10 500 (Al.sub.0.25Cr.sub.0.75)CN 550 540 0.98 3.0 19 10 700 (Al.sub.0.50Ti.sub.0.50)N 480 456 0.95 3.0 20 10 700 (Al.sub.0.50Cr.sub.0.50)N 370 420 1.14 3.0 21 10 700 (Al.sub.0.50Ti.sub.0.45W.sub.0.05)N 390 396 1.02 3.0 22 10 700 (Al.sub.0.50Cr.sub.0.45W.sub.0.05)N 370 360 0.97 3.0 23 10 700 (Al.sub.0.50Ti.sub.0.45Y.sub.0.05)N 240 276 1.15 3.0 24 10 700 (Al.sub.0.50Cr.sub.0.45Y.sub.0.05)N 220 240 1.09 3.0 25 10 700 (Al.sub.0.50Ti.sub.0.45Si.sub.0.05)N 240 288 1.20 3.0 26 10 700 (Al.sub.0.50Cr.sub.0.45Si.sub.0.05)N 220 252 1.15 3.0
(9) TABLE-US-00002 TABLE 2 Coating layer Average Average grain grain diameter diameter Lx at Ly at Coating direction direction Grain conditions parallel perpendicular diameter Magnetic to interface to interface ratio Average flux Substrate of of (Ly/Lx) layer Sample density temperature substrate substrate of Ly to thickness No. (mT) (° C.) Composition (nm) (nm) Lx (μm) Comparative 27 10 500 (Al.sub.0.70Ti.sub.0.30)N 70 48 0.69 3.0 product 28 10 500 (Al.sub.0.75Cr.sub.0.25)N 180 122 0.68 3.0 29 20 800 (Al.sub.0.50Ti.sub.0.50)N 130 64 0.49 3.0 30 20 700 (Al.sub.0.50Cr.sub.0.50)N 150 96 0.64 3.0 31 20 700 (Al.sub.0.50Ti.sub.0.45W.sub.0.05)N 120 80 0.67 3.0 32 20 700 (Al.sub.0.50Cr.sub.0.45W.sub.0.05)N 110 68 0.62 3.0 33 20 700 (Al.sub.0.50Ti.sub.0.45Y.sub.0.05)N 80 44 0.55 3.0 34 20 700 (Al.sub.0.50Cr.sub.0.45Y.sub.0.05)N 60 28 0.47 3.0 35 20 700 (Al.sub.0.50Ti.sub.0.45Si.sub.0.05)N 80 48 0.60 3.0 36 20 700 (Al.sub.0.50Cr.sub.0.45Si.sub.0.05)N 60 32 0.53 3.0
(10) With regard to the obtained samples, the layer thicknesses of the coating layer were measured at the 5 portions by using an optical microscope and FE-SEM at the position of 50 μm toward the center portion of the surface from the edge of a blade of a surface opposed to the metal evaporation source, and the averaged value thereof was made an average layer thickness of the coating layer. The composition of the coating layer was measured by using an FE-SEM-attached EDS and an FE-SEM-attached WDS.
(11) With regard to the obtained samples, from the surface to the depth of 100 nm of the coating layer was grinded by a diamond paste, and further polished to a minor surface by using colloidal silica. The surface structure of the coating layer which became a mirror surface was observed by an EBSD, and an average grain diameter Lx of the coating layer was measured. The EBSD was so set that a boundary having a step size of 0.01 μm, a measurement range of 2 μm×2 μm, and an orientation difference of 5° or more was regarded as a grain boundary. A diameter of a circle having an area equal to the area of a certain crystal grain of the coarse grain layer was made a grain diameter of the crystal grain. According to the same method, grain diameters of the crystal grains contained in the observed surface structure were obtained. Thereafter, a grain size distribution comprising the horizontal axis showing a grain diameter divided with an interval of 5 nm, and the vertical axis showing an area ratio of the whole crystal grains contained in a division of an interval of 5 nm was prepared, and a center value of the division with the interval of 5 nm and the area ratio of the whole crystal grains contained in the division were multiplied. The value in which all the values obtained by multiplying the center value of the division with the interval of 5 nm and the area ratio of the whole crystal grains contained in the division had been summed was made an average grain diameter Lx of the coarse grain layer.
(12) A cross section of the sample obtained by cutting with a cutter was grinded by a diamond paste, and further polished to a minor surface by using colloidal silica. The cross section of the coating layer which became a minor surface was observed by an EBSD, and the average grain diameter Ly of the coating layer measured at a direction perpendicular to an interface between the coating layer and the substrate was measured. At this time, the EBSD was so set that a boundary with a step size of 0.01 μm, a measurement range of 2 μm×2 μm and an orientation difference of 5° or more is regarded as grain boundary. To an image of the cross-sectional structure of the coating layer enlarged to 5,000 to 50,000-fold by the EBSD were drawn ten straight lines to a direction perpendicular to an interface between the coating layer and the substrate with an interval of 500 nm. A length from the interface of the coating layer at the substrate side or an interface of the coating layer at the surface side to the point at which the straight line and the grain boundary were crossed, or a length from the point at which the straight line and the grain boundary are crossed to the next point at which the straight line and the grain boundary were crossed was made Ln (n=1, 2, 3, . . .). Also, when the straight line and the grain boundary were not crossed, a length from the interface of the coating layer at the substrate side to the interface of the coarse grain layer at the surface side was made Ln. An average value of these Ln's was made an average grain diameter Ly.
(13) With regard to the obtained samples, the X-ray diffraction measurement was carried out under the conditions that the target: Cu, tube voltage: 50 kV, tube current: 250 mA, Cu-Kα line, scanning axis: 2θ/θ, a solar slit on an incident side: 5°, a divergence longitudinal slit: 2/3°, a divergence longitudinal restriction slit: 5 mm, scattering slit: 2/3°, a solar slit on light receiving side: 5°, a light receiving slit: 0.30 mm, a light receiving monochromatic slit: 0.8 mm, monochromation of X-ray: a graphite light receiving monochromatic meter (bending mode), sampling width: 0.01°, scanning speed: 4°/min, and a measurement range of Bragg angle (2θ) of 30° to 70°. As a result, it could be found that all the crystal system of the obtained coating layer were cubic. A composition of the coating layer, an average grain diameter Lx at a direction parallel to an interface between the coating layer and the substrate, an average grain diameter Ly at a direction perpendicular to an interface between the coating layer and the substrate, a grain diameter ratio (Ly/Lx) of the average grain diameter Ly to the average grain diameter Lx, and an average layer thickness of the whole coating layer are shown in Table 1 and Table 2.
(14) The obtained sample was attached to the following mentioned milling cutter and Machining test 1 was carried out. Processing distances until the samples reach to the tool life were shown in Table 3 and Table 4.
(15) [Machining Test 1]
(16) Work piece material: S45C.,
(17) Cutting speed: 200 m/min,
(18) Feed: 0.2 mm/tooth,
(19) Depth of cut: 2.0 mm,
(20) Width of cut: 50 mm,
(21) Cutter effective diameter: φ100 mm,
(22) Coolant: Not used (dry processing),
(23) Judgement of tool life: When a maximum flank wear width reached to 0.2 mm, then the time was the end of tool life.
(24) TABLE-US-00003 TABLE 3 Processing distance until sample reaches to Sample No. tool life (m) Present product 1 3.6 2 9.1 3 12.3 4 14.1 5 11.2 6 3.4 7 8.4 8 11.5 9 13.2 10 9.4 11 9.8 12 8.0 13 7.9 14 6.5 15 8.2 16 6.7 17 11.3 18 10.8 19 9.1 20 8.4 21 7.9 22 7.2 23 5.5 24 4.8 25 5.8 26 5.0
(25) TABLE-US-00004 TABLE 4 Processing distance until sample reaches to Sample No. tool life (m) Comparative 27 1.0 product 28 2.4 29 1.3 30 1.9 31 1.6 32 1.4 33 0.9 34 0.6 35 1.0 36 0.6
(26) As shown in Table 3 and Table 4, Present products having large average grain diameters Lx at a direction parallel to an interface between the coating layer and the substrate are excellent in wear resistance so that the processing distances until the samples reach to the tool life were longer than those of Comparative products.
EXAMPLE 2
(27) As a substrate, a cemented carbide corresponding to P20 having an insert shape of ISO standard SEKN1203AGTN was prepared. In a reaction vessel of an arc ion plating device, a metal evaporation source which became a starting material of coating layer shown in Table 5 was set, the substrate was attached to a sample holder in the reaction vessel of the arc ion plating device and an Ar ion bombardment treatment was carried out under the same conditions as in Example 1. After the Ar ion bombardment treatment, the Ar gas was discharged and a pressure in the reaction vessel was made vacuum of 1×10.sup.−2 Pa or less. An N.sub.2 gas was introduced into the reaction vessel to make a pressure in the reaction vessel a nitrogen atmosphere at 3 Pa. After the substrate was heated to a temperature as shown in Table 5 by a heater in the vessel, a bias voltage to be applied to the substrate was made −50V, a magnetic flux density at the center of the metal evaporation source was made a magnetic flux density as shown in Table 5, and the coating layer shown in Table 5 was formed on the surface of the substrate under the coating conditions that an arc current was made 150A. After forming the coating layer, the sample was cooled, and after the temperature of the sample became 100° C. or lower, the sample was taken out from the reaction vessel.
(28) TABLE-US-00005 TABLE 5 Coating layer Average Average grain grain diameter diameter Ly at Lx at direction Coating direction perpendicular Grain conditions parallel to diameter Magnetic to interface interface ratio Average flux Substrate of of (Ly/Lx) layer Sample density temperature substrate substrate of Ly to thickness No. (mT) (° C.) Composition (nm) (nm) Lx (μm) Present 37 10 500 (Al.sub.0.30Ti.sub.0.70)N 620 456 0.74 0.5 product 38 10 500 (Al.sub.0.30Ti.sub.0.70)N 620 614 0.99 3.0 39 10 500 (Al.sub.0.30Ti.sub.0.70)N 620 883 1.42 10.0 40 10 500 (Al.sub.0.25Cr.sub.0.75)N 590 420 0.71 0.5 41 10 500 (Al.sub.0.25Cr.sub.0.75)N 590 576 0.98 3.0 42 10 500 (Al.sub.0.25Cr.sub.0.75)N 590 828 1.40 10.0 Comparative 43 10 500 (Al.sub.0.30Ti.sub.0.70)N 620 993 1.60 12.0 product 44 10 500 (Al.sub.0.25Cr.sub.0.75)N 590 934 1.58 12.0 45 20 850 (Al.sub.0.30Ti.sub.0.70)N 180 294 1.63 3.0 46 20 850 (Al.sub.0.25Cr.sub.0.75)N 160 258 1.61 3.0
(29) With regard to the obtained samples, the crystal system, the composition, the average grain diameter Lx at a direction parallel to an interface between the coating layer and the substrate, the average grain diameter Ly at a direction perpendicular to an interface between the coating layer and the substrate, the grain diameter ratio (Ly/Lx) of the average grain diameter Ly to the average grain diameter Lx of the coating layer, and the average layer thickness of the whole coating layer were measured under the same measurement conditions as in Example 1. These results are shown in Table 5. Incidentally, all the coating layers of the obtained samples were cubic.
(30) The obtained sample was attached to the following mentioned milling cutter and Machining tests 2 and 3 were carried out. Processing distances until the samples reach to the tool life were shown in Table 6. Incidentally, Machining test 2 is a test mainly evaluating wear resistance and Machining test 3 is a test mainly evaluating fracture resistance.
(31) [Machining Test 2]
(32) Work piece material: S45C.,
(33) Cutting speed: 250 m/min,
(34) Feed: 0.1 mm/tooth,
(35) Depth of cut: 2.0 mm,
(36) Width of cut: 50 mm,
(37) Cutter effective diameter: φ100 mm,
(38) Coolant: Not used (dry processing),
(39) Judgement of tool life: When a maximum flank wear width reached to 0.2 mm, then the time was the end of tool life.
(40) [Machining Test 3]
(41) Work piece material: SCM440,
(42) Cutting speed: 250 m/min,
(43) Feed: 0.4 mm/tooth,
(44) Depth of cut: 2.0 mm,
(45) Width of cut: 105 mm,
(46) Cutter effective diameter: φ125 mm,
(47) Coolant: Not used (dry processing),
(48) Judgement of tool life: When the sample fractured, then the time was the end of tool life.
(49) TABLE-US-00006 TABLE 6 Machining test 2 Machining test 3 Processing distance Processing distance until sample reaches to until sample reaches to Sample No. tool life (m) tool life (m) Present product 37 9.1 6.9 38 12.3 6.4 39 14.1 5.3 40 8.4 6.7 41 11.5 6.1 42 13.2 5.1 Comparative 43 7.9 3.2 product 44 7.5 3.0 45 2.4 2.8 46 2.1 2.6
(50) As shown in Table 6, Present products having large average grain diameters Lx at a direction parallel to an interface between the coating layer and the substrate are excellent in wear resistance and fracture resistance, so that the processing distances until the samples reach to the tool life were longer than those of Comparative products.
EXAMPLE 3
(51) As a substrate, a cemented carbide corresponding to P20 having an insert shape of ISO standard SEKN1203AGTN was prepared. In a reaction vessel of an arc ion plating device, a metal evaporation source which became a starting material of coating layer shown in Table 7 was set, the substrate was attached to a sample holder in the reaction vessel of the arc ion plating device and an Ar ion bombardment treatment was carried out under the same conditions as in Example 1. After the Ar ion bombardment treatment, the Ar gas was discharged and a pressure in the reaction vessel was made vacuum of 1×10.sup.−2 Pa or less. An N.sub.2 gas was introduced into the reaction vessel to make a pressure in the reaction vessel a nitrogen atmosphere at 3 Pa. After the substrate was heated to a temperature as shown in Table 7 by a heater in the vessel, a bias voltage to be applied to the substrate was made −50V, a magnetic flux density at the center of the metal evaporation source was made a magnetic flux density as shown in Table 7, and the coating layer shown in Table 7 was formed on the surface of the substrate under the coating conditions that an arc current was made 150A. After forming the coating layer, the sample was cooled, and after the temperature of the sample became 100° C. or lower, the sample was taken out from the reaction vessel.
(52) TABLE-US-00007 TABLE 7 Coating layer Average Average grain grain diameter diameter Ly at Lx at direction Full Coating direction perpendicular Grain width conditions parallel to diameter at Magnetic to interface interface ratio half Average flux Substrate of of (Ly/Lx) maximum layer Sample density temperature substrate substrate of Ly to intensity thickness No. (mT) (° C.) Composition (nm) (nm) Lx (° C.) (μm) Present 47 10 550 (Al.sub.0.30Ti.sub.0.70)N 600 588 0.98 0.30 3.0 product 48 10 550 (Al.sub.0.50Ti.sub.0.50)N 550 528 0.96 0.58 3.0 Comparative 49 20 850 (Al.sub.0.50Ti.sub.0.50)N 110 56 0.51 0.68 3.0 product 50 10 550 (Al.sub.0.70Ti.sub.0.30)N 60 40 0.67 0.80 3.0
(53) With regard to the obtained samples, the crystal system, the composition, the average grain diameter Lx at a direction parallel to an interface between the coating layer and the substrate, the average grain diameter Ly at a direction perpendicular to an interface between the coating layer and the substrate, the grain diameter ratio (Ly/Lx) of the average grain diameter Ly to the average grain diameter Lx of the coating layer, and the average layer thickness of the coating layer was measured under the same measurement conditions as in Example 1. Incidentally, all the coating layers of the obtained samples were cubic. Further, with regard to the X-ray diffraction peak at the (200) plane of the coarse grain layer, using XRD analysis software JADE ver.6 manufactured by MDI (Materials Data Inc.), background processing and Kα2 peak removal were carried out by using cubic spline, and profile fitting was carried out by using Pearson-VII function, then, peak position was obtained by the peak top method, whereby the full width at half maximum intensity (FWHM) was led out. These results are shown in Table 7.
(54) The obtained sample was attached to the following mentioned milling cutter and Machining test 4 was carried out. Processing distances until the samples reach to the tool life were shown in Table 8.
(55) [Machining Test 4]
(56) Work piece material: SCM440,
(57) Cutting speed: 200 m/min,
(58) Feed: 0.1 mm/tooth,
(59) Depth of cut: 2.0 mm,
(60) Width of cut: 50 mm,
(61) Cutter effective diameter: φ100 mm,
(62) Coolant: Not used (dry processing),
(63) Judgement of tool life: When a maximum flank wear width reached to 0.2 mm, then the time was the end of tool life.
(64) TABLE-US-00008 TABLE 8 Machining test 4 Processing distance until sample Sample No. reaches to tool life (m) Present product 47 9.4 48 8.4 Comparative 49 3.4 product 50 2.4
(65) As shown in Table 8, Present products having large average grain diameters Lx at a direction parallel to an interface between the coating layer and the substrate and small full widths at half maximum intensity (FWHM) of the X-ray diffraction peak at the (200) plane of the coating layer are excellent in wear resistance so that the processing distances until the samples reach to the tool life were longer than those of Comparative products.
EXAMPLE 4
(66) As a substrate, a cemented carbide corresponding to P20 having an insert shape of ISO standard SEKN1203AGTN was prepared. In a reaction vessel of an arc ion plating device, a metal evaporation source which became a starting material of coating layer shown in Table 9 was set, the substrate was attached to a sample holder in the reaction vessel of the arc ion plating device and an Ar ion bombardment treatment was carried out under the same conditions as in Example 1. After the Ar ion bombardment treatment, the Ar gas was discharged and a pressure in the reaction vessel was made vacuum of 1×10.sup.31 2 Pa or less. An N.sub.2 gas was introduced into the reaction vessel to make a pressure in the reaction vessel a nitrogen atmosphere at 3 Pa. After the substrate was heated until a temperature became 700° C. by a heater in the vessel, Layer A and Layer B shown in Table 9 were alternately formed under the coating conditions of a bias voltage to be applied to the substrate of −50V, a magnetic flux density at the center of the metal evaporation source of 20 mT and an arc current of 150A, to form the lower layers with an alternately laminated structure on the surface of the substrate.
(67) Subsequently, the sample was heated by a heater in the vessel until a temperature became the temperature of an uppermost layer shown in Table 9, and the uppermost layer shown in Table 10 was formed on the surface of the lower layer under the coating conditions of a bias voltage to be applied to the substrate of −50V, a magnetic flux density at the center of the metal evaporation source of the magnetic flux density of the uppermost layer of Table 9 and an arc current of 150A. After forming the uppermost layer, the sample was cooled, and after the temperature of the sample became 100° C. or lower, the sample was taken out from the reaction vessel.
(68) TABLE-US-00009 TABLE 9 Coating layer Lower layer (alternately laminated structure) Average layer Repeated thickness Layer A Layer B times of Average Average A + B of whole layer layer laminating laminating lower thickness thickness period period layer Sample No. Composition (nm) Composition (nm) (nm) (times) (μm) Present 51 (Al.sub.0.70Ti.sub.0.30)N 100 (Al.sub.0.50Ti.sub.0.50)N 100 200 10 2.0 product 52 (Al.sub.0.70Ti.sub.0.30)N 100 (Al.sub.0.50Cr.sub.0.50)N 100 200 10 2.0 53 (Al.sub.0.70Ti.sub.0.30)N 100 (Al.sub.0.50Ti.sub.0.50)N 100 200 10 2.0 54 (Al.sub.0.70Ti.sub.0.30)N 100 (Al.sub.0.50Cr.sub.0.50)N 100 200 10 2.0 Comparative 55 (Al.sub.0.70Ti.sub.0.30)N 100 (Al.sub.0.50Ti.sub.0.50)N 100 200 10 2.0 product 56 (Al.sub.0.70Ti.sub.0.30)N 100 (Al.sub.0.50Cr.sub.0.50)N 100 200 10 2.0 57 (Al.sub.0.70Ti.sub.0.30)N 100 (Al.sub.0.50Ti.sub.0.50)N 100 200 10 2.0 58 (Al.sub.0.70Ti.sub.0.30)N 100 (Al.sub.0.50Cr.sub.0.50)N 100 200 10 2.0 Coating layer Uppermost layer Average Average layer layer Coating thickness thickness conditions of of Magnetic upper- whole flux Sample most coating density temperature layer layer Sample No. (mT) (° C.) Composition (μm) (μm) Present 51 10 550 (Al.sub.0.30Ti.sub.0.70)N 2.0 4.0 product 52 10 550 (Al.sub.0.30Ti.sub.0.70)N 2.0 4.0 53 10 550 (Al.sub.0.50Ti.sub.0.50)N 2.0 4.0 54 10 550 (Al.sub.0.50Ti.sub.0.50)N 2.0 4.0 Comparative 55 20 850 (Al.sub.0.50Ti.sub.0.50)N 2.0 4.0 product 56 20 850 (Al.sub.0.50Ti.sub.0.50)N 2.0 4.0 57 10 550 (Al.sub.0.70Ti.sub.0.30)N 2.0 4.0 58 10 550 (Al.sub.0.70Ti.sub.0.30)N 2.0 4.0
(69) With regard to the obtained samples, the composition and the average layer thickness of Layer A and Layer B of the lower layer, the laminating period in which the layer thickness of Layer A of the lower layer and the layer thickness of Layer B of the lower layer are summed, the number of repeating times of the laminating period, the composition and the average layer thickness of the uppermost layer, and the average layer thickness of the whole coating layer were measured at the position of 50 μm from the surface of an edge of a blade opposed to the metal evaporation source toward the center portion of the surface by using an optical microscope, an FE-SEM and a TEM. Incidentally, with regard to the respective layer thicknesses of Layer A of the lower layer, Layer B of the lower layer, the uppermost layer and the whole coating layer, each measured at 5 portions, and these were averaged to make an average layer thickness of the respective layers. Also, the respective compositions of Layer A of the lower layer, Layer B of the lower layer and the uppermost layer were measured by using an FE-SEM-attached EDS, an FE-SEM-attached WDS, a TEM-attached EDS and a TEM-attached WDS. These results are shown in Table 9. With regard to the obtained samples, an X-ray diffraction measurement was carried out under the same measurement conditions as in Example 1, whereby the crystal system of the uppermost layer was measured. Incidentally, the uppermost layers of the obtained samples were all cubic. In addition, the average grain diameter Lx of the uppermost layer at a direction parallel to an interface between the coating layer and the substrate, the average grain diameter Ly of the uppermost layer at a direction perpendicular to an interface between the coating layer and the substrate and the grain diameter ratio (Ly/Lx) of the average grain diameter Ly to the average grain diameter Lx were measured under the same measurement conditions as in Example 1. These results are shown in Table 10 .
(70) TABLE-US-00010 TABLE 10 Uppermost layer Average grain Average grain diameter Lx diameter Ly Grain at direction at direction diameter parallel to perpendicular to ratio interface of interface of (Ly/Lx) Sample No. substrate (nm) substrate (nm) of Ly to Lx Present 51 550 576 1.05 product 52 530 528 1.00 53 500 516 1.03 54 480 456 0.95 Comparative 55 100 48 0.48 product 56 90 40 0.44 57 55 32 0.58 58 50 24 0.48
(71) The obtained sample was attached to the following mentioned milling cutter and Machining test 5 was carried out. Processing distances until the samples reach to the tool life were shown in Table 11.
(72) [Machining test 5]
(73) Work piece material: SCM440,
(74) Cutting speed: 250 m/min,
(75) Feed: 0.1 mm/tooth,
(76) Depth of cut: 2.0 mm,
(77) Width of cut: 50 mm,
(78) Cutter effective diameter: φ100 mm,
(79) Coolant: Not used (dry processing),
(80) Judgement of tool life: When a maximum flank wear width reached to 0.2 mm, then the time was the end of tool life.
(81) TABLE-US-00011 TABLE 11 Machining test 5 Processing distance until sample Sample No. reaches to tool life (m) Present product 51 9.2 52 8.4 53 8.3 54 7.3 Comparative 55 2.9 product 56 2.4 57 1.9 58 1.4
(82) As shown in Table 11, Present products having large average grain diameters Lx at a direction parallel to an interface between the coating layer and the substrate are excellent in wear resistance so that the processing distances until the samples reach to the tool life were longer than those of Comparative products.
EXPLANATION OF REFERENCE NUMERALS
(83) 1: Crystal grain of coating layer
(84) 2: The state where crystal grain of coating layer dropped
(85) 3: Coating layer
(86) 4: Substrate
(87) 5: Interface at surface side
(88) 6: Interface at substrate side