U.S. patent application number 13/135339 was filed with the patent office on 2012-01-19 for alumina layer with enhanced texture.
This patent application is currently assigned to SECO TOOLS AB. Invention is credited to Sakari Ruppi.
Application Number | 20120015148 13/135339 |
Document ID | / |
Family ID | 37930325 |
Filed Date | 2012-01-19 |
United States Patent
Application |
20120015148 |
Kind Code |
A1 |
Ruppi; Sakari |
January 19, 2012 |
Alumina layer with enhanced texture
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 .alpha.-Al.sub.2O.sub.3 showing a strong growth texture
along <001>. The .alpha.-Al.sub.2O.sub.3 layer has a
thickness ranging from 1 to 20 .mu.m 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 .alpha.-Al.sub.2O.sub.3
layers is deposited in a temperature range of 750-1000.degree. C.
The texture is controlled by a specific nucleation procedure
combined with the use of sulphur- and fluorine containing
dopants.
Inventors: |
Ruppi; Sakari; (Fagersta,
SE) |
Assignee: |
SECO TOOLS AB
Fagersta
SE
|
Family ID: |
37930325 |
Appl. No.: |
13/135339 |
Filed: |
July 1, 2011 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
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11527711 |
Sep 27, 2006 |
7993742 |
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13135339 |
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Current U.S.
Class: |
428/148 ;
423/625 |
Current CPC
Class: |
Y10T 428/265 20150115;
Y10T 428/24413 20150115; C23C 16/36 20130101; C23C 30/005 20130101;
Y10T 428/24975 20150115; C23C 16/403 20130101; Y10T 428/252
20150115; Y10T 428/266 20150115 |
Class at
Publication: |
428/148 ;
423/625 |
International
Class: |
B32B 5/16 20060101
B32B005/16; C01F 7/02 20060101 C01F007/02 |
Foreign Application Data
Date |
Code |
Application Number |
Sep 27, 2005 |
SE |
0502115-9 |
Claims
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 .alpha.-alumina layer wherein said
.alpha.-alumina layer comprises columnar .alpha.-Al.sub.2O.sub.3
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 TC ( hkl ) = I ( hkil ) I 0 ( hkil ) { 1 n I ( hkil ) I 0 ( hkil
) } - 1 ##EQU00002## wherein I(hkl)=measured intensity of the (hkl)
reflection I.sub.0(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 .alpha.-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 .mu.m, and said .alpha.-Al.sub.2O.sub.3 layer adjacent
said first layer having a thickness of from about 1 to about 40
.mu.m, preferably from about 1 to about 20 .mu.m, most preferably
from about 1 to about 10 .mu.m.
6. Cutting tool insert according to claim 1, wherein the
.alpha.-Al.sub.2O.sub.3 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 .mu.m,
preferably from about 0.5 to about 1.5 .mu.m atop the
.alpha.-Al.sub.2O.sub.3 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 .mu.m,
preferably 2 to 8 .mu.m atop the .alpha.-Al.sub.2O.sub.3 layer.
9. Cutting tool insert according to claim 1, wherein a layer of
.kappa.-Al.sub.2O.sub.3 or .gamma.-Al.sub.2O.sub.3 atop the
.alpha.-Al.sub.2O.sub.3 with a thickness of from 0.5 to 10 .mu.m,
preferably from 1 to 5 .mu.m.
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 .mu.m, preferably 0.5-2 .mu.m.
11. Cutting tool insert according to claim 1, wherein said coating
has a total thickness of from about 5 to about 25 .mu.m.
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
.mu.m.
14. Cutting tool insert according to claim 1, wherein said
.alpha.-Al.sub.2O.sub.3 layer adjacent said first layer has a
thickness of from about 1 to about 20 .mu.m.
15. Cutting tool insert according to claim 1, wherein said
.alpha.-Al.sub.2O.sub.3 layer adjacent said first layer has a
thickness of from about 1 to about 10 .mu.m.
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 .mu.m, preferably 5-25 .mu.m comprising one or more
refractory layers of which at least one layer of which is an
.alpha.-alumina layer wherein said .alpha.-alumina layer comprises
columnar .alpha.-Al.sub.2O.sub.3 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 TC ( hkl ) = I ( hkil ) I 0 ( hkil ) { 1 n
I ( hkil ) I 0 ( hkil ) } - 1 ##EQU00003## wherein I(hkl)=measured
intensity of the (hid) reflection I.sub.0(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 .alpha.-alumina layer is
formed by controlling both the nucleation and growth of
.alpha.-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 H.sub.2S, SF.sub.6, SO.sub.2, SF.sub.6 and mixtures
thereof.
18. A method of making an .alpha.-Al.sub.2O.sub.3 layer on a
substrate, comprising the steps of: nucleating said alumina in a
temperature range of from about 750 to about 1000.degree. C., and
controlling both the nucleation and growth of .alpha.-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 H.sub.2S, SF.sub.6, SO.sub.2, SF.sub.6 and mixtures thereof.
20. Method according to claim 18, wherein said at least one
sulphur-containing precursor comprises a mixture of H.sub.2S and
SF.sub.6.
Description
CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims priority from Swedish application
No. SE 0502115-9 filed Sep. 27, 2005 which is hereby incorporated
by reference in its entirety.
FIELD OF THE INVENTION
[0002] 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 .alpha.-Al.sub.2O.sub.3 layer
strongly textured in the <001> direction.
BACKGROUND OF THE INVENTION
[0003] Techniques to deposit .alpha.-Al.sub.2O.sub.3 and
.kappa.-Al.sub.2O.sub.3 layers with nucleation control have been
introduced on an industrial scale only recently, and it has clearly
been shown that .alpha.-Al.sub.2O.sub.3 is the preferred phase in
most metal cutting applications. According to the definition used
in the International Tables of Crystallography,
.alpha.-Al.sub.2O.sub.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 .alpha.-Al.sub.2O.sub.3
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 . . . .alpha..beta..gamma..alpha..beta..gamma. . . . .
These are usually referred to as c.sup..alpha., c.sup..beta. and
c.sup..gamma.. The unit cell of .alpha.-Al.sub.2O.sub.3 comprises
six layers of O and Al can be described in the following way:
Ac.sup..alpha.Bc.sup.62
Ac.sup..gamma.Bc.sup..alpha.Ac.sup..beta.Bc.sup..gamma.. 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.
[0004] 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 .alpha.-Al.sub.2O.sub.3 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 .alpha.-Al.sub.2O.sub.3
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 .alpha.-Al.sub.2O.sub.3 layers using known
methods.
[0005] 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 .alpha.-Al.sub.2O.sub.3 layers are formed via
.kappa.-Al.sub.2O.sub.3 .fwdarw..alpha.-Al.sub.2O.sub.3 phase
transformation. These kinds of .alpha.-Al.sub.2O.sub.3 layers are
composed of larger grains with transformation cracks. They exhibit
much lower mechanical strength and ductility than textured
.alpha.-Al.sub.2O.sub.3 layers composed of .alpha.-Al.sub.2O.sub.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 .alpha.-Al.sub.2O.sub.3.
[0006] The control of the .alpha.-Al.sub.2O.sub.3 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
.alpha.-Al.sub.2O.sub.3 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 .alpha.-Al.sub.2O.sub.3 along the
<10(10)> direction. U.S. Pat. No. 6,869,668 describes a
method to obtain a strong <300> texture in
.alpha.-Al.sub.2O.sub.3 using a texture modifying agent
(ZrCl.sub.4). The prior-art processes discussed above all use
deposition temperatures of about 1000.degree. C.
[0007] 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
.alpha.-Al.sub.2O.sub.3 towards fully controlled textures.
OBJECTS AND SUMMARY OF THE INVENTION
[0008] It is an object of the present invention is to provide an
alumina layer providing improved physical properties to a cutting
tool insert.
[0009] 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 .alpha.-Al.sub.2O.sub.3 phase in the coating.
[0010] 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 .mu.m,
preferably 5-25 .mu.m comprising one or more refractory layers of
which at least one layer of which is an .alpha.-alumina layer
wherein said .alpha.-alumina layer comprises columnar
.alpha.-Al.sub.2O.sub.3 grains with a <001> growth
direction.
[0011] The objects of the invention are also achieved by a method
of making an .alpha.-Al.sub.2O.sub.3 layer on a substrate which
comprises the steps of nucleating said alumina in a temperature
range of from about 750 to about 1000.degree. C., and controlling
both the nucleation and growth of .alpha.-alumina using
sulphur-containing and at least one fluorine-containing
precursor.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] For a fuller understanding of the invention, the following
detailed description should be read in conjunction with the
drawings, wherein:
[0013] FIG. 1a shows SEM-image of a typical surface morphology of
the layer according to this invention in 15000.times.;
[0014] FIG 1b shows the same layer in cross-section in
15000.times.; and FIG.2 shows an XRD pattern of an
.alpha.-Al.sub.2O.sub.3-layer according to this invention for
2.theta.=20-70.degree..
DETAILED DESCRIPTION OF THE INVENTION
[0015] 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.
[0016] 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.
[0017] It has been experimentally confirmed that
.alpha.-Al.sub.2O.sub.3 can be nucleated, for example, on
Ti.sub.2O.sub.3 surfaces, bonding layers of (Ti,Al)(C,O) or by
controlling the oxidation potential using CO/CO.sub.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 .kappa.-Al.sub.2O.sub.3 is obtained.
[0018] Further, it has been noticed that enhanced performance can
be obtained through optimising the texture of
.alpha.-Al.sub.2O.sub.3. It is thus possible to enhance tool
performance by tailoring the .alpha.-Al.sub.2O.sub.3 texture for
different metal cutting applications and work piece materials.
[0019] 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 .alpha.-Al.sub.2O.sub.3 deposited on a
bonding layer of (Ti,Al)(C,O,N) with increasing aluminium content
towards the outer surface. The .alpha.-Al.sub.2O.sub.3 layer is
1-45 .mu.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 .alpha.-Al.sub.2O.sub.3-layer is
determined as follows:
TC ( hkl ) = I ( hkil ) I 0 ( hkil ) { 1 n I ( hkil ) I 0 ( hkil )
} - 1 ##EQU00001##
[0020] where
[0021] I(hkl)=intensity of the (hid) reflection
[0022] I.sub.0(hkl)=standard intensity according to JCPDS card no
46-1212
[0023] n=number of reflections used in the calculation
[0024] 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.
[0025] The texture of the alumina layer is defined as follows:
[0026] 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.
[0027] 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 .mu.m. Preferably there is an intermediate
layer of TiN between the substrate and said first layer with a
thickness of <3 .mu.m, preferably 0.5-2 .mu.m.
[0028] In one embodiment the .alpha.-Al.sub.2O.sub.3 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 .mu.m, preferably
0.5 to 1.5 .mu.m atop the .alpha.-Al.sub.2O.sub.3 layer.
Alternatively this layer has a thickness of from about 1 to 20
.mu.m, preferably 2 to 8 .mu.m.
[0029] In yet another embodiment the coating includes a layer of
.kappa.-Al.sub.2O.sub.3 and/or .gamma.-Al.sub.2O.sub.3 preferably
atop the .alpha.-Al.sub.2O.sub.3 with a thickness of from 0.5 to
10, preferably from 1 to 5 .mu.m.
[0030] The present invention also relates to a refined method to
produce textured .alpha.-Al.sub.2O.sub.3 layers in a temperature
range of 950-1000.degree. C., preferably at 1000.degree. C. with a
controlled <001> texture. The .alpha.-Al.sub.2O.sub.3 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 TiCl.sub.4, preferably together
with AlC.sub.3, (ii) purge (N.sub.2), (iii) exposure of the second
precursor (H.sub.2O), (iv) purge (N.sub.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 .alpha.-Al.sub.2O.sub.3 is started with a relatively long
30-120 min, preferably 60 min, nucleation step without sulphur- or
fluorine containing compounds. .alpha.-Al.sub.2O.sub.3 is grown to
its desired thickness using sulphur-containing compounds H.sub.2S,
or SO.sub.2, preferably H.sub.2S, optionally together with
fluorine-containing compounds SF.sub.6 or HF, preferably
SF.sub.6.
[0031] It has been found, quite unexpectedly, that <001>
texture could be obtained by careful control of the ratio of
sulphur containing dopants to CO.sub.2/CO. When
.alpha.-Al.sub.2O.sub.3 is nucleated correctly, followed by a
deposition process using relatively low amounts of these dopants
(0.5-1.2%) together with a CO+CO.sub.2 gas mixture where
CO=0.5-2.times.CO.sub.2, 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
.alpha.-Al.sub.2O.sub.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.
[0032] The following is a detailed description of a preferred
sequence of nucleation steps. [0033] 1. Depositing a bonding layer
0.1-1 .mu.m thick in a gas mixture of 2-3% TiCl.sub.4 and
AlCl.sub.3 increasing from 0.5 to 6%, 3-10% CO, 1-3% CO.sub.2,
0.2-1.0% CH.sub.3CN, 0.2-1.0%, 2-10% N2 and balance H2 at about
750-1000.degree. C., preferably at 800.degree. C. and at a pressure
of 50-200 mbar. [0034] 2. Purging by N.sub.2 for 5 min. [0035] 3.
Treating the bonding layer in a gas mixture of 5-15% TiCl.sub.4 and
5-20% CO, 0.5-3% CO.sub.2 and 10-20% Ar in hydrogen for 5-15,
preferably 10, minutes min at 950-1000.degree. C., preferably at
1000.degree. C. and at a pressure of 50-200 mbar. [0036] 4. Purging
by N.sub.2 for 5 min. [0037] 5. Treating the bonding layer in a gas
mixture of 8-15% TiCl.sub.4 and 0.5-2% AlCl.sub.3 in hydrogen for
5-15 min at about 950 to about 1000.degree. C., preferably at about
1000.degree. C. and at a pressure of from about 50 to about 200
mbar. [0038] 6. Treating in a gas mixture of 0.05 to 0.5% H.sub.2O,
preferably 0.01%, balance H.sub.2. [0039] 7. Purging by N.sub.2 for
5 min. [0040] 8. Nucleation of the alumina layer at a temperature
of 950-1000.degree. C. with desired thickness according to known
technique or depositing an alumina layer at 950-1000.degree. C.
without any catalysing precursors. [0041] 9. Deposition of the
alumina layer at a temperature of 950-1000.degree. C. to the
desired thickness at 950-1000.degree. C. at deposition pressures
50-200 mbar using 0.01-0.05% H.sub.2S or SO.sub.2, preferably
H.sub.2S and 0.01-0.02% SF.sub.6 or HF, preferably SF.sub.6 as
catalysing agents. CO.sub.2 1.0-4.5% is used as the oxygen donor
together with CO, maintaining CO=2.times.CO.sub.2.
EXAMPLE 1
[0042] 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
.mu.m. On to this layer an .alpha.-Al.sub.2O.sub.3 layer consisting
of about 10 .mu.m. .alpha.-Al.sub.2O.sub.3 was deposited according
to this invention referred to as Coating a). The detailed process
data is given below:
[0043] Step 1:Bonding layer 1
TABLE-US-00001 Gas mixture TiCl.sub.4 = 2.8% CH.sub.3CN = 0.7%
AlCl.sub.3 = increasing from 0.8 to 5.4% CO = 8.8% CO.sub.2 = 2.2%
N.sub.2 . . . = 5% Balance: H.sub.2 Duration 40 min Temperature
1000.degree. C. Pressure 100 mbar
[0044] Step 2: N.sub.2 purge
[0045] Step 3:Bonding layer 2
TABLE-US-00002 Gas mixture TiCl.sub.4 = 8% CO = 12% CO.sub.2 = 1.2%
Ar . . . = 5% Balance: H.sub.2 Duration 2-10 min Temperature
1000.degree. C. Pressure 100 mbar
[0046] Step 3: (optional ALD steps): a)TiCl.sub.4 treatment b)
N.sub.2-purge c) H.sub.2O treatment d) N.sub.2-purge
TABLE-US-00003 a) TiCl.sub.4 = 9% AlCl.sub.3 = 1% H.sub.2 = balance
5 min . . . c) H.sub.2O = 0.1% H.sub.2 = balance 2 min . . . b, d)
N.sub.2 = 100% 5 min Temperature 1000.degree. C. Pressure 50
mbar
[0047] Step 4: Nucleation step
TABLE-US-00004 Gas mixture AlCl.sub.3 = 1.2% HCl . . . = 2.0%
CO.sub.2 = 1.0-1.5% CO = 0.5-2.4% Balance H.sub.2 Duration 60 min
Temperature 1000.degree. C. Pressure 50 mbar
[0048] Step 5: Deposition
TABLE-US-00005 Gas mixture AlCl.sub.3 = 2.8% HCl = 3% CO.sub.2 =
1.8-2.5% CO = 0.9-.5% H.sub.2S = 0.05-1.0% Balance: H.sub.2
Duration 630 min Temperature 1000.degree. C. Pressure 70 mbar
EXAMPLE 2
[0049] Coating a) was studied using X-ray diffraction. The texture
coefficients of the .alpha.-Al.sub.2O.sub.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. 1a and in cross
section in FIG. 1b. The .alpha.-Al.sub.2O.sub.3 layer was composed
of columnar grains. The X-Ray diffraction pattern is shown in FIG.
2.
TABLE-US-00006 TABLE 1 hkl Coating a) 012 0.01 104 0.06 110 0.01
006 5.91 113 0.00 116 0.02
EXAMPLE 3
[0050] For reference Coatings b) and c) with <012> and
<104> textures were deposited according to the prior-art
(coating thickness about 10 .mu.m). The coatings were studied using
X-ray diffraction. The texture coefficients of the
.alpha.-Al.sub.2O.sub.3 layers were determined and are presented in
Table 2.
TABLE-US-00007 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
EXAMPLE 4
[0051] 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
Material: SS1672
[0052] 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
Depth of cut: 2.5 mm
[0053] Remarks: dry turning
[0054] Tool life criteria: Gradually increased feed until edge
breakage. 10 edges of each variant were tested.
[0055] 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-US-00008 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
[0056] 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).
EXAMPLE 5
[0057] The coatings a), b) and c) were tested with respect to edge
chipping in longitudinal turning in cast iron.
[0058] Work piece: Cylindrical bar
[0059] Material: SS0130
[0060] Insert type: SNUN
[0061] Cutting speed: 400 m/min
[0062] Feed: 0.4 mm/rev
[0063] Depth of cut: 2.0 mm
[0064] Remarks: dry turning
[0065] 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-US-00009 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
EXAMPLE 6
[0066] 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.
[0067] Work piece: Cylindrical bar
[0068] Material: SS0130
[0069] Insert type: SNUN
[0070] Cutting speed: 800 m/min
[0071] Feed: 0.4 mm/rev
[0072] Depth of cut: 2.5 mm
[0073] Remarks: dry turning
TABLE-US-00010 TABLE 5 Life time (min) Coated CBN, Invention 23
Coated CBN, prior art, 14 012 texture Uncoated CBN 9
[0074] As is evident from Table 5 the coating according to this
invention is superior to the prior art.
EXAMPLE 7
[0075] The hardness and Young's modulus of the coatings a)-c)
together with .kappa.-Al.sub.2O.sub.3 and older prior-art
.alpha.-Al.sub.2O.sub.3 were measured using nanoindentation. The
results are shown in Table 6.
TABLE-US-00011 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 .alpha.-Al.sub.2O.sub.3 (no texture) 25.79 385.45
.kappa.-Al.sub.2O.sub.3 23.64 339.51
[0076] Coating c) according to the invention shows the highest
values of hardness and modulus, closely followed by coating c).
* * * * *