CVD COATED CUTTING TOOL WITH TEXTURED k-Al2O3 LAYER

Abstract

The present disclosure relates to a coated cutting tool having a substrate and a coating, wherein the coating includes at least one layer of κ-Al.sub.2O.sub.3 with a thickness of 1-20 μm deposited by chemical vapour deposition (CVD). A χ-scan from −80° to 80° over the (0 0 6) reflection of the κ-Al.sub.2O.sub.3 layer shows the strongest peak centered around 0° and the full width half maximum (FWHM) of the peak is <25°.

Claims

1. A coated cutting tool comprising a substrate and a coating, wherein the coating comprises at least one layer of κ-Al.sub.2O.sub.3 with a thickness of 1-20 μm deposited by chemical vapor deposition, wherein a χ-scan from −80° to 80° over a (0 0 6) reflection of said κ-Al.sub.2O.sub.3 layer shows the strongest peak centered around 0° and wherein a FWHM of said peak is <25°.

2. The coated cutting tool in accordance with claim 1, wherein the strongest peak from the κ-Al.sub.2O.sub.3 layer in an X-ray diffractogram from 15° to 140° is a (0 0 2) reflection.

3. The coated cutting tool in accordance with claim 2, wherein the second strongest peak from the κ-Al.sub.2O.sub.3 layer in an X-ray diffractogram from 15° to 140° is a (0 0 4) reflection.

4. The coated cutting tool in accordance with claim 3, wherein the third strongest peak from the κ-Al.sub.2O.sub.3 layer in an X-ray diffractogram from 15° to 140° is the (0 0 6) reflection.

5. The coated cutting tool in accordance with claim 1, wherein an average thickness of the κ-Al.sub.2O.sub.3 layer is 2-10 μm.

6. The coated cutting tool in accordance with claim 1, wherein the coating further comprises an α-Al.sub.2O.sub.3 layer.

7. The coated cutting tool in accordance with claim 6, wherein said α-Al.sub.2O.sub.3 layer is located between said κ-Al.sub.2O.sub.3 layer and the substrate.

8. The coated cutting tool in accordance with claim 1, wherein the thickness of said α-Al.sub.2O.sub.3 layer is 0.5-2 μm or 0.7-1 μm.

9. The coated cutting tool in accordance with claim 1, wherein the coating further comprises one or more layers of TiN, TiCN, TiC, TiCO, TiAlCO and TiCNO.

10. The coated cutting tool in accordance with claim 1, wherein a layer of one or more of TiN, TiC, TiCN, TiCO, TiCNO, TiAlCO is located between said α-Al.sub.2O.sub.3 layer and said κ-Al.sub.2O.sub.3 layer.

11. The coated cutting tool of claim 10, wherein the thickness of said layer of one or more of TiN, TiC, TiCN, TiCO, TiCNO, TiAlCO is ≦0.5 μm.

12. The coated cutting tool in accordance with claim 1, wherein the coating comprises layers in the following order as seen from the surface of the substrate TiN, TiCN, TiCNO, α-Al.sub.2O.sub.3, TiN and κ-Al.sub.2O.sub.3.

13. The coated cutting tool in accordance with claim 1, wherein the coating comprises an outermost wear indicating color layer.

Description

BRIEF DESCRIPTION OF DRAWINGS

[0024] FIG. 1 is a θ-2θ XRD diffractogram from Sample B with no corrections applied on the intensities.

[0025] FIG. 2 is a θ-2θ XRD diffractogram from Sample A with no corrections applied on the intensities.

[0026] FIG. 3 is a θ-2θ XRD diffractogram from Sample C with no corrections applied on the intensities.

[0027] FIG. 4 is a χ-scan from the (0 0 6) plane of the κ-Al.sub.2O.sub.3 layer of Sample B. Thin film correction is applied to the intensities.

[0028] FIG. 5 is a χ-scan from the (0 0 6) plane of the κ-Al.sub.2O.sub.3 layer of Sample C. Thin film correction is applied to the intensities.

[0029] FIG. 6 is a (0 0 6) pole figure of Sample B wherein −80°≦χ≦80° and 0°≦φ≦360°.

[0030] FIG. 7 is a χ-scan from the (0 0 12) plane of the α-Al.sub.2O.sub.3 layer of Sample B. Notice that no correction is applied to the intensities.

DETAILED DESCRIPTION

XRD Examination

[0031] In order to investigate the texture of the κ-Al.sub.2O.sub.3 layer X-ray diffraction (XRD) was conducted on the flank face using a PANalytical CubiX3 diffractometer equipped with a PIXcel detector. The coated cutting tools were mounted in sample holders to ensure that the flank face of the samples were parallel to the reference surface of the sample holder and also that the flank face was at appropriate height. Cu-Kα radiation was used for the measurements, with a voltage of 45 kV and a current of 40 mA. Anti-scatter slit of ½ degree and divergence slit of ¼ degree were used. The diffracted intensity from the coated cutting tool was measured in the range 15° to 140° 2θ, i.e. over an incident angle θ range from 7.5 to 70°.

[0032] A common way to analyze the texture of a polycrystalline film is to calculate texture coefficients (TC) based on Harris formula and standard intensity PDF cards. The out of plane texture for κ-Al.sub.2O.sub.3 alumina is however hard to determine from calculation of texture coefficients since the crystal structure of κ-Al.sub.2O.sub.3 has a low symmetry and therefore there are many peaks of low intensity in the diffractogram. Also there are a lot of overlapping peaks. Therefore the peak of the highest intensity of the κ-Al.sub.2O.sub.3 layer is selected here as a measure of the texture of the layer. Selected κ-Al.sub.2O.sub.3 XRD peaks which had no (or very limited) peak overlap in the XRD diffractogram and are either strong in the κ-layer of the invention or are strong in a randomly oriented powder according to PDF card 00-52-0803 were used to evaluate the texture of the κ-Al.sub.2O.sub.3 layer (κ-Al.sub.2O.sub.3 peaks: (0 0 2), (0 1 3), (1 2 2), (0 0 4) and (0 0 6)).

[0033] Since the κ-Al.sub.2O.sub.3 layer was a finitely thick film the relative intensities of peaks at different 2θ angles are different than they are for bulk samples, due to the differences in path length through the layer. Therefore, thin film correction was applied to the peak intensities, taken into account the linear absorption coefficient of the layer. Since possible further layers above for example the κ-Al.sub.2O.sub.3 layer will affect the X-ray intensities entering the κ-Al.sub.2O.sub.3 layer and exiting the whole coating, corrections need to be made for these as well, taken into account the linear absorption coefficient for the respective compound in a layer. Any further layers, such as TiN, above an alumina layer can be removed by a method that does not substantially influence the XRD measurement results, e.g. chemical etching.

Pole Figure and χ-Scan

[0034] Textured κ-Al.sub.2O.sub.3 layers were analyzed by XRD on a PANalytical MRD diffractrometer with an Euler cradle. The diffractrometer was operated in point focus and was equipped with a primary polycapillary lens and a cross slit. The cross slit was set to 2×2 mm. The diffracted side optics was a 0.18° parallel plate collimator and a flat graphite monocromator. A point detector was used.

[0035] Pole figure was extracted from the (0 0 6) plane and measured on the clearance side on a CNMG1208-PM insert. The step size in φ was 5° and the χ step size was 5°. The measurement time/step was 1.5 seconds. The scan range was 0-360° in φ and −0 to 80 in χ.

[0036] To evaluate the intensity distribution as a function of χ a scan in the χ axis was performed. The measurement was performed symmetric around χ=0° with a scan range of 70°, a step size of 2.5° and a time/step of 10 seconds.

[0037] The FWHM of the peak in the χ scan is a measure of alignment of planes {h k l} in parallel with the surface. i.e a single crystal will have a broadening equal to the instrument resolution and a randomly oriented material will not show any peak in the χ scan. The χ scan can be considered as a cut in the χ direction in the (0 0 6) pole figure.

[0038] The pole figure and χ-scan analyze of the α-Al.sub.2O.sub.3 layer was made in the corresponding way on the α-Al.sub.2O.sub.3 (0 0 12) plane.

[0039] Also in the case of pole figure and χ scan thin film correction needs to be applied to the intensities, taken into account the linear absorption coefficient of layer. Since the layer is of finite thickness the path length of the X-ray beam in the sample will vary as a function of the χ angle.

EXAMPLES

[0040] Embodiments of the present invention will be disclosed in more detail in connection with the following examples. The examples are to be considered as illustrative and not limiting embodiments. In the following examples coated cutting tools (inserts) were manufactured, analyzed and evaluated in cutting tests.

Example 1—Sample Preparation

[0041] Three types of coatings have been deposited in a radial Ion Bond type CVD reactor 530 size capable of housing 10.000 half-inch size cutting inserts. The three type of samples are called Sample A (invention), Sample B (invention) and Sample C (reference). The samples were inserts with the ISO type geometry CNMG 120408-PM.

[0042] The process parameters regarding the inner layer are identical in all three coatings. The inner layer includes TiN (approx. 0.4 μm), MT-TiCN (approx. 8 μm) and bonding layer (approx. 0.7 μm).

[0043] The inserts were first coated with a thin approximately 0.4 μm TiN-layer then with an approximately 8 μm TiCN layer (TiCN inner+TiCN outer) by employing the well-known MTCVD technique using TiCl.sub.4, CH.sub.3CN, N.sub.2, HCl and H.sub.2 at 885° C. The details of the TiN and the TiCN deposition are shown in Table 1.

TABLE-US-00001 TABLE 1 Process parameters TiN and MT-TiCN MT CVD of TiN and TiCN Pressure H.sub.2 N.sub.2 HCl TiCl.sub.4 CH.sub.3CN (885° C.): [mbar] [vol %] [vol %] [vol %] [vol %] [vol %] TiN 400 balance 48.8 — 2.4 — TiCN inner 55 balance 37.6 — 2.9 0.5 TiCN outer 55 balance 7.8 7.8 2.4 0.6

[0044] Deposition time for TiCN inner and TiCN outer was 10 and 240 minutes, respectively. On top of the MTCVD TiCN layer a 0.7 μm bonding layer was deposited at 1000° C. by a process consisting of four separate reaction steps. First a HTCVD TiCN step using TiCl.sub.4, CH.sub.4, N.sub.2, HCl and H.sub.2 at 400 mbar, then a second step (TiCNO-1) using TiCl.sub.4, CH.sub.3CN, CO, HCl, N.sub.2 and H.sub.2 at 70 mbar, then a third step (TiCNO-2) using TiCl.sub.4, CH.sub.3CN, CO, N.sub.2 and H.sub.2 at 70 mbar and finally a fourth step (TiN) using TiCl.sub.4, N.sub.2 and H.sub.2 at 70 mbar. During the third and fourth deposition step some of the gases were continuously changed as indicated by a first start level and a second stop level presented in Table 2.

TABLE-US-00002 TABLE 2 Bonding layer Bonding layer Press H.sub.2 N.sub.2 CH.sub.4 HCl CO TiCl.sub.4 CH.sub.3CN CO.sub.2 (1000° C.) [mbar] [vol %] [vol %] [vol %] [vol %] [vol %] [vol %] [vol %] [vol %] HTCVD- 400 balance 25.5 3.4 1.7 — 1.5 — — TiCN TiCNO-1 70 balance 12   — 1.2 1.2 1.5 0.4 — TiCNO-2 70 balance 31.5-30.6 — — 1.6-4.6 3.15-3.06 0.66-0.62 — TiN 70 balance 32.2 — — — 3.2 — —

Sample A

[0045] On top of the inner layer a layer structure of {0 0 1}-textured α-alumina, TiN and {0 0 1}-textured κ-alumina were subsequently deposited in accordance with the following:

[0046] Initially the bonding layer (the inner layer) was oxidized for 4 minutes in a mixture of CO.sub.2, CO, N.sub.2 and H.sub.2. The details of the bonding layer oxidation deposition are shown in Table 3.

TABLE-US-00003 TABLE 3 Oxidation Pressure H.sub.2 N.sub.2 CO CO.sub.2 [mbar] [vol %] [vol %] [vol %] [vol %] Oxidation 55 balance 30 12.5 3.7

[0047] On top of the oxidized bonding layer an α-Al.sub.2O.sub.3 layer was then deposited, see Table 4. The α-Al.sub.2O.sub.3 layer was deposited at 1000° C. and 55 mbar in two steps. The first step using 1.2 vol-% AlCl.sub.3, 4.7 vol-% CO.sub.2, 1.8 vol-% HCl and balance H.sub.2 giving about 0.1 μm α-Al.sub.2O.sub.3 and a second step using 1.2% AlCl.sub.3, 4.7% CO.sub.2, 2.9% HCl, 0.58% H.sub.2S and balance H.sub.2 giving a total α-Al.sub.2O.sub.3 layer thickness of about 1 μm.

TABLE-US-00004 TABLE 4 α-Al.sub.2O.sub.3 layer deposition α-Al2O3 Pressure H.sub.2 HCl CO.sub.2 H.sub.2S AlCl.sub.3 (1000° C.): [mbar] [vol %] [vol %] [vol %] [vol %] [vol %] Al.sub.2O.sub.3-1 55 balance 1.8 4.7 — 1.2 Al.sub.2O.sub.3-2 55 balance 2.9 4.7 0.6 1.2

[0048] On top of the α-Al.sub.2O.sub.3 layer a thin TiN-layer of approximately 0.1 μm was deposited, see Table 5. This was done at 55 mbar and 1000° C. using 1.4% TiCl.sub.4, 41.1% N.sub.2 and balance H.sub.2.

TABLE-US-00005 TABLE 5 TiN layer deposition TiN-layer Pressure H.sub.2 N.sub.2 TiCl.sub.4 (1000° C.): [mbar] [vol %] [vol %] [vol %] TiN-layer 55 balance 41.1 1.4

[0049] On top of the thin TiN-layer, a κ-Al.sub.2O.sub.3 layer was deposited, see Table 6. The κ-Al.sub.2O.sub.3 layer was deposited at 1000° C. and 55 mbar in two steps. The first step using 1.2 vol-% AlCl.sub.3, 4.7 vol-% CO.sub.2, 1.8 vol-% HCl and balance H.sub.2 giving about 0.1 μm Al.sub.2O.sub.3 and a second step using 1.2% AlCl.sub.3, 4.7% CO.sub.2, 2.9% HCl, 0.58% H.sub.2S and balance H.sub.2 giving a total κ-Al.sub.2O.sub.3 layer thickness of about 4 μm.

TABLE-US-00006 TABLE 6 κ-Al.sub.2O.sub.3 layer deposition on Sample A. κ-Al2O3 Pressure H.sub.2 HCl CO.sub.2 H.sub.2S AlCl.sub.3 (1000° C.): [mbar] [vol %] [vol %] [vol %] [vol %] [vol %] Al.sub.2O.sub.3-1 55 balance 1.8 4.7 — 1.2 Al.sub.2O.sub.3-2 55 balance 2.9 4.7 0.6 1.2

Sample B

[0050] Sample A and Sample B differs in the process parameters for the κ-Al.sub.2O.sub.3 layer deposition. All other process parameters were identical. For Sample B the κ-Al.sub.2O.sub.3 layer was deposited at 1000° C. and 55 mbar in two steps. The first step using 2.3 vol-% AlCl.sub.3, 4.6 vol-% CO.sub.2, 1.7 vol-% HCl and balance H.sub.2 giving about 0.1 μm κ-Al.sub.2O.sub.3 and a second step using 2.2% AlCl.sub.3, 4.4% CO.sub.2, 5.5% HCl, 0.33% H.sub.2S and balance H.sub.2 giving a total κ-Al.sub.2O.sub.3 layer thickness of about 4 μm. The process parameters are given in Table 7.

TABLE-US-00007 TABLE 7 κ-Al.sub.2O.sub.3 layer deposition on Sample B. κ-Al2O3 Pressure H.sub.2 HCl CO.sub.2 H.sub.2S AlCl.sub.3 (1000° C.): [mbar] [vol %] [vol %] [vol %] [vol %] [vol %] Al.sub.2O.sub.3-1 55 balance 1.7 4.6 — 2.3 Al.sub.2O.sub.3-2 55 balance 5.5 4.4 0.3 2.2

Sample C

[0051] A κ-Al.sub.2O.sub.3 layer of approximately 5 μm was deposited directly on the bonding layer (the inner layer) using the process parameters given in Table 7.

[0052] The layer thicknesses were analyzed in a light optical microscope by studying a cross section of each coating at 1000× magnification. The layer thicknesses are presented in Table 8.

TABLE-US-00008 TABLE 8 Layer thicknesses Inner layer structure Al.sub.2O.sub.3 layer structure TiN TiCN Bonding α-Al.sub.2O.sub.3 TiN κ-Al.sub.2O.sub.3 Sample A 9.1 μm 5.4 μm 0.4 μm 8.0 μm 0.7 μm 1.2 μm 0.1 μm 4.1 μm Sample B 9.7 μm 4.8 μm 0.4 μm 8.6 μm 0.7 μm 1.0 μm 0.1 μm 3.7 μm Sample C 9.7 μm 4.5 μm 0.4 μm 8.6 μm 0.7 μm — — 4.5 μm

Example 2—XRD Examination

[0053] The peak intensities in an XRD diffractogram was provided in accordance with the method described above. Thin film correction was applied to the intensities.

[0054] Diffractograms (no applied correction) from Sample A and Sample B are shown in FIG. 2 and FIG. 1, respectively. The peaks originating from the {0 0 1} planes show a strong intensity at 20=19.85°, 40.33° and 62.24° for (0 0 2), (0 0 4) and (0 0 6) planes respectively. Compared to ICDD's PDF card No. 00-052-0803 these peaks are supposed to have 11% 8% and 7% intensity for the (0 0 2), (0 0 4) and (0 0 6) planes respectively. The strongest peak according to PDF card 00-052-0803 is the (1 1 2) plane which is hardly observable in FIG. 1. The second strongest peak in PDF card 00-052-0803 is the (0 1 3) which can be observed as a weak peak in FIG. 1 and in FIG. 2. Thus, it is clear that the κ-Al.sub.2O.sub.3 layers of Sample A and Sample B show a strong texture with the {0 0 1} planes in parallel with the surface.

[0055] A diffractogram from Sample C is shown in FIG. 3. The peak originating from the κ-Al.sub.2O.sub.3 with the strongest intensity for Sample C is the (1 2 2) peak.

[0056] Table 9 lists the 20 values for the κ-Al.sub.2O.sub.3 peaks that were used to determine the texture of the κ-Al.sub.2O.sub.3 layer of Sample A, B and C and table 10 lists the corrected intensities of these peaks.

TABLE-US-00009 TABLE 9 2θ values of peaks of κ-Al.sub.2O.sub.3 h k l 2θ (°) 0 0 2 19.85° 0 1 3 31.89° 1 2 2 34.81° 0 0 4 40.34° 0 0 6 62.30°

TABLE-US-00010 TABLE 10 Peak intensities from the κ-Al.sub.2O.sub.3 XRD diffractogram, normalized such that the highest peak is set to 100 in intensity. Peak (h k l) Sample A Sample B Sample C (0 0 2) 100.0 100.0 1.1 (0 1 3) 38.6 13.9 21.2 (1 2 2) 5.3 3.9 100.0 (0 0 4) 93.7 97.4 not visible (0 0 6) 51.7 52.8 not visible

Example 3—Pole Figure and χ-Scan Examination

[0057] The samples Sample B and Sample C were evaluated using {0 0 6} pole figures and χ-scan with the method as disclosed above. The pole figure of Sample B showed one peak centered around χ=0°, see FIG. 6. No such peak close to χ=0° was found in the pole figure of the reference Sample C.

[0058] In the χ scan of the κ-Al.sub.2O.sub.3 (0 0 6) plane of Sample B one single sharp peak is noted which indicates a strong {0 0 1} texture and a high alignment of the {0 0 1} planes in parallel with the surface of the substrate. The χ scan of the Sample B is shown in FIG. 4. The one peak is centered around χ=0° with a FWHM of about 16.5°.

[0059] A χ scan from the κ-Al.sub.2O.sub.3 (0 0 6) plane in the reference Sample C is shown in FIG. 5. As can be observed no sharp peak is observed centered around χ=0° rather two local maxima at roughly χ=±20° is shown.

[0060] In the χ scan of the α-Al.sub.2O.sub.3 (0 0 12) plane of Sample B one single peak is noted around χ=0° which indicates a strong {0 0 1} texture and a high alignment of the {0 0 1} planes in parallel with the surface of the substrate. The χ scan of the Sample B is shown in FIG. 7. The one peak is centered around χ=0° with a FWHM of about 17°.

Example 4—Crater Wear Test

[0061] The coated cutting tools, i.e. Samples A, B and C were tested in longitudinal turning in ball bearing steel (Ovako 825B) using the following cutting data;

[0062] Cutting speed v.sub.c: 220 m/min

[0063] Cutting feed, f: 0.3 mm/revolution

[0064] Depth of cut, ap: 2 mm

[0065] Insert style: CNMG120408-PM

[0066] Water miscible metal working fluid was used.

[0067] One cutting edge per cutting tool was evaluated.

[0068] In analyzing the crater wear, the area of exposed substrate was measured, using a light optical microscope. When the surface area of the exposed substrate exceeded 0.2 mm.sup.2 the life time of the tool was considered to be reached. The wear of each cutting tool was evaluated after 2 minutes cutting in the light optical microscope. The cutting process was then continued with a measurement after each 2 minutes run, until the tool life criterion was reached. When the size of the crater area exceeded 0.2 mm.sup.2 the time until the tool life criterion was met was estimated based on an assumed constant wear rate between the two last measurements. Beside crater wear, flank wear was also observed, but did not in this test influence the tool life. The average results of two parallel tests are shown in Table 11.

TABLE-US-00011 TABLE 11 Crater wear resistance Sample Sample A Sample B Sample C Life time 31 34 22 (min)

[0069] While the invention has been described in connection with the above exemplary embodiments, it is to be understood that the invention is not to be limited to the disclosed exemplary embodiments; on the contrary, it is intended to cover various modifications and equivalent arrangements within the appended claims.