Tool having CVD coating

Patent metadata

Field	Value
Publication number	US-9976213-B2
Application number	US-201414781622-A
Country	US
Kind code	B2
Filing date	Apr 16, 2014
Priority date	Apr 26, 2013
Publication date	May 22, 2018
Grant date	May 22, 2018

Abstract

A tool having a base body of carbide, cermet, ceramic, steel or high speed steel and a single-layer or multi-layer wear-protection coating applied thereto in a CVD process, wherein the wear-protection coating has at least one Ti 1-x Al x C y N z layer having stoichiometry coefficients 0.70≤x<1.0≤y<0.25 and 0.75≤z<1.15 wherein the Ti 1-x Al x C y N z layer is of a thickness of 1 μm to 25 μm and has a crystallographic preferential orientation, which is characterized by a ratio of the intensities of the X-ray diffraction peaks of the crystallographic {111} plane and the {200} plane, wherein I{111}/I{200}>1+h (ln h) 2 , wherein h is the thickness of the Ti 1-x Al x C y N z layer in micrometer.

First claim

The invention claimed is:

1. A process for the production of a tool having a base body of carbide, cermet, ceramic, steel or high speed steel and a single-layer or multi-layer wear-protection coating applied thereto in a CVD process, wherein the wear-protection coating has at least one Ti 1-x Al x C y N z layer having stoichiometry coefficients 0.70<x<1, 0<y<0.25 and 0.75≤z<1.15 and of a thickness in the range of 1 μm to 25 μm, wherein for production of the Ti 1-x Al x C y N z layer
a) the bodies to be coated are placed in a substantially cylindrical CVD reactor designed for an afflux flow on the bodies to be coated with the process gases in a direction substantially radially relative to the longitudinal axis of the reactor,
b) two precursor gas mixtures (VG1) and (VG2) are provided, wherein the first precursor gas mixture (VG1) contains
0.005% to 0.2 vol-% TiCl 4 ,
0.025% to 0.5 vol-% AlCl 3 and
as a carrier gas hydrogen (H 2 ) or a mixture of hydrogen and nitrogen (H 2 /N 2 ), and

wherein the second precursor gas mixture (VG2) contains
0.1 to 3.0 vol-% of at least one N-donor selected from ammonia (NH 3 ) and hydrazine (N 2 H 4 ), and
as a carrier gas hydrogen (H 2 ) or a mixture of hydrogen and nitrogen (H 2 /N 2 ), and

wherein the first precursor gas mixture (VG1) and/or the second precursor gas mixture (VG2) optionally contains a C-donor selected from acetonitrile (CH 3 CN), ethane (C 2 H 6 ), ethene (C 2 H 4 ) and ethyne (C 2 H 2 ) and mixtures thereof, wherein the total vol-% proportion of N-donor and C-donor in the precursor gas mixtures (VG1, VG2) is in the range of 0.1 to 3.0 vol-%,
c) the two precursor gas mixtures (VG1, VG2) are kept separate before passing into the reaction zone and are introduced substantially radially relative to the longitudinal axis of the reactor at a process temperature in the CVD reactor in the range of 600° C. to 850° C. and a process pressure in the CVD reactor in the range of 0.2 to 18 kPa,
wherein the ratio of the volume gas flows ({dot over (V)}) of the precursor gas mixtures (VG1, VG2){dot over (V)}(VG1)/{dot over (V)}(VG2) is less than 1.5.

2. A process according to claim 1 , wherein the process includes at least one of: the process temperature in the CVD reactor is in the range of 650° C. to 800° C. and the process pressure in the CVD reactor is in the range of 0.2 to 7 kPa.

3. A process according to claim 1 , wherein the ratio of the volume gas flows ({dot over (V)}) of the precursor gas mixtures (VG1, VG2){dot over (V)}(VG1)/{dot over (V)}(VG2) is less than 1.25.

4. A process according to claim 1 , wherein the concentration of TiCl 4 in the precursor gas mixture (VG1) and the concentration of N-donor in the precursor gas mixture (VG2) are so set that the molar ratio of Ti to N in the volume gas flows {dot over (V)}(VG1) and {dot over (V)}(VG2) introduced into the reactor in stage c) is ≤0.25.

5. A process according to claim 1 , wherein the second precursor gas mixture (VG2) contains ≤1.0 vol-% of the N-donor.

6. A process according to claim 1 , wherein the N-donor is ammonia (NH 3 ).

7. A process according to claim 1 , wherein the wear-protection coating is subjected to a blasting treatment with a particulate blasting agent under conditions such that the Ti 1-x Al x C y N z layer after the blasting treatment has residual stresses in the range of +300 to −5000 MPa.

8. A tool having
a base body of carbide, cermet, ceramic, steel or high speed steel and
a single-layer or multi-layer wear-protection coating applied thereto in a CVD process,
wherein the wear-protection coating includes at least one Ti 1-x Al x C y N z layer having stoichiometry coefficients 0.70≤x<1, 0<y<0.25 and 0.75≤z<1.15, and
wherein the Ti 1-x Al x C y N z layer is of a thickness of 1 μm to 25 μm and has a crystallographic preferential orientation, which is characterised by a ratio of the intensities of the X-ray diffraction peaks of the crystallographic {111} plane and the {200} plane, wherein I{111}/I{200}>1+h (ln h) 2 , wherein h is the thickness of the Ti 1-x Al x C y N z layer in micrometers.

9. A tool according to claim 8 , wherein the full-width half-maximum (FWHM) of the X-ray diffraction peak of the {111} plane of the Ti 1-x Al x C y N z layer is <1%.

10. A tool according to claim 8 , wherein the Ti 1-x Al x C y N z layer has at least 90 vol-% Ti 1-x Al x C y N z phase with a cubically face-centred (fcc) lattice.

11. A tool according to claim 8 , wherein the Ti 1-x Al x C y N z layer has stoichiometry coefficients 0.70≤x<1, y=0 and 0.95≤z<1.15.

12. A tool according to claim 8 , wherein the Ti 1-x Al x C y N z layer has a thickness in the range of 3 μm to 20 μm.

13. A tool according to claim 8 , wherein the ratio of the intensities of the X-ray diffraction peaks of the crystallographic {111} plane and the {200} plane of the Ti 1-x Al x C y N z layer is >1+(h+3)x(ln h) 2 .

14. A tool according to claim 8 , wherein the Ti 1-x Al x C y N z layer has a Vickers hardness (HV)>2300 HV.

15. A tool according to claim 8 , wherein the wear-protection coating includes at least one of:
arranged between the base body and the Ti 1-x Al x C y N z layer, at least one layer selected from a TiN layer, a TiCN layer deposited by means of high temperature CVD (CVD) or medium temperature CVD (MT-CVD), an Al 2 O 3 layer and combinations thereof, and
arranged over the Ti 1-x Al x C y N z layer, at least one hard material layer.

16. A tool according to claim 8 , wherein an absolute maximum, measured radiographically or by means of EBSD, of the diffraction intensity of the crystallographic {111} planes of the fcc Ti 1-x Al x C y N z layer is within an angle range of α=±10°, starting from the normal direction of the sample surface.

17. A tool including a base body of carbide, cermet, ceramic, steel or high speed steel and a single-layer or multi-layer wear-protection coating applied thereto in a CVD process, wherein the wear-protection coating includes at least one Ti 1-x Al x C y N z layer having stoichiometry coefficients 0.70<x<1, 0<y<0.25 and 0.75<z<1.15, and wherein the Ti 1-x Al x C y N z layer is of a thickness of 1 μm to 25 μm and has a crystallographic preferential orientation, which is characterised by a ratio of the intensities of the X-ray diffraction peaks of the crystallographic {111} plane and the {200} plane, wherein l{111}/l{200}>1+h (ln h) 2 , wherein h is the thickness of the Ti 1-x Al x C y N z layer in micrometers, produced according to claim 1 .

18. A process according to claim 2 , wherein the process includes at least one of: the process temperature in the CVD reactor is in the range of 657° C. to 750° C. and the process pressure in the CVD reactor is in the range of 0.4 to 1.8 kPa.

19. A process according to claim 5 , wherein the second precursor gas mixture (VG2) contains <0.6 vol-% of the N-donor.

20. A process according to claim 7 , wherein the Ti 1-x Al x C y N z layer after the blasting treatment has residual stresses in the range of −1 to −3500 MPa.

21. A tool according to claim 9 , wherein the full-width half-maximum (FWHM) of the X-ray diffraction peak of the {111} plane of the Ti 1-x Al x C y N z layer is <0.6%.

22. A tool according to claim 10 , wherein the Ti 1-x Al x C y N z layer has at least 98 vol-% Ti 1-x Al x C y N z phase with a cubically face-centred (fcc) lattice.

23. A tool according to claim 14 , wherein the Ti 1-x Al x C y N z layer has a Vickers hardness (HV) in the range of 27

Assignees

• Walter Ag

Inventors

• Stiens Dirk
• Ruppi Sakari
• Manns Thorsten

Classifications

• C23C16/44

  characterised by the method of coating (C23C16/04 takes precedence) · CPC title

• C23C16/34 Primary

  Nitrides {(C23C16/303 takes precedence)} · CPC title

• C23C16/45508

  Radial flow · CPC title