CZ2000904A3 - Tool provided with protective layer system - Google Patents

Abstract

There is proposed a tool with a tool body and a wear resistant layer system, which layer system comprises at least one layer of MeX. Me comprises titanium and aluminium and X is a nitrogen or carbon. Thereby, in the MeX layer the quotient QI as defined by the ratio of the diffraction intensity I(200) to I(111) assigned respectively to the (200) and (111) plains in the X ray diffraction of the material using the THETA - THETA 2 method is selected to be. QI has a value QI <= 2. A tool is a solid carbide end mill or a solid carbide ball nose mill or a cemented carbide gear cutting tool. Further, the I(111) is at least twenty times larger than the intensity average noise value, both measured with a well-defined equipment and setting thereof.

Description

Tool equipped with a protective layer system

Technical area

The invention relates to a tool having a tool body and a protective layer system, the layer system comprising at least one MeX layer, wherein

- Me contains titanium and aluminum, and

X is at least one element from the group consisting of nitrogen and carbon.

Definition:

• The expression Q _x is defined as the ratio of the 1(200) to the 1(111) bending intensity, converted to the (200) and (111) planes of X-ray diffraction in the material, respectively, using the θ - 20 method. So,

Qi = I(200)/1(111).

The intensity values were measured using the following equipment and with the following settings or adjustments:

• · ·

Siemens diffractometer

Power consumption:

Aperture aperture:

Detector aperture: Time constant:

2θ angular velocity: Radiation:

D500

Operating voltage: 30 kV Operating current: 25 mA Aperture position I: 1° Aperture position II: 0.1° Soller slit with

0.05°/min

Cu-Kα (0.15406 nm)

When it is stated "measured in accordance with MS", reference is made to this equipment and to this setting or adjustment. Thus, all quantitative results for Ch and I in the description of this application were measured using MS.

• The term “tool body” refers to the uncoated tool.

• The term "hard material" means a material with which tools that are exposed to high mechanical and thermal loads during operation are coated for wear resistance purposes. Preferred examples of such materials are listed below as MeX materials.

From the prior art, it is generally known in the field of tool protection to apply wear-resistant layer systems that contain at least one layer of a hard material, defined as MeX.

The object of the present invention is to achieve a significant improvement in the service life of such tools. This is achieved by selecting for said at least one layer a value of Q _If for which the following holds:

Qi < 2, the tool being a solid carbide end mill, cylindrical cutter or a solid carbide ball mill or a cemented carbide gear cutting tool. In addition, the value 1(111) is at least 20 times higher than the average noise level measured in accordance with MS.

In accordance with the subject matter of the present invention, it has been found that the above-specified Qx values lead to a significantly high improvement in the wear resistance and thus the tool life, if the tool is of the type as mentioned above.

Until now, the application of wear-resistant layer systems made of hard MeX material has been carried out independently of the interaction between the tool body material and the mechanical and thermal loads to which the tool is exposed during operation.

The subject of the present invention is therefore based on the fact that it has been found that an excellent improvement in wear resistance is achieved when a specific Qx value is selectively combined with a specific type of tool, thereby realizing a 1(111) value higher by a factor of at least 20 than the average sound intensity level, both values being measured in accordance with MS.

The improvement achieved by the invention is even increased if the value of Qi is chosen to be at most 1, with further improvement being achieved if the value of Qi chosen is at most 0.5 or even at most 0.2. The greatest improvements are achieved if the value of Qi is at most 0.1.

It should be emphasized here that the value of Ch can drop to zero if the layer material is made with a uniform crystalline orientation in accordance with the zero bending intensity 1(200). Therefore, no lower limit is set for the value of Q _Iř which is determined only from a practical point of view.

As is well known to those skilled in the art, there is a relationship between the hardness of a layer and the stress or strain in that layer. The higher the stress or strain, the higher the hardness must be. However, as the strain increases, the adhesion to the tool body tends to decrease.

For the tool according to the invention, high hardness is more important than the highest possible adhesion. Therefore, the stress in the MeX layer is preferably chosen at the higher end of the stress range given below.

These circumstances limit the usable value of Qi in practice.

In a preferred embodiment of the tool according to the present invention, the MeX tool material is titanium aluminum nitride, titanium aluminum carbon nitride, or titanium aluminum boron nitride, the first two materials being currently preferred over titanium aluminum boron nitride.

• ·

In another embodiment of the tool according to the present invention, the metal Me in the layer material MeX may further contain at least one of the elements boron, zirconium, hafnium, yttrium, silicon, tungsten and chromium, with the use of yttrium and/or silicon and/or boron being preferred from the group mentioned.

The above-mentioned additional elements to titanium and aluminum are introduced into the layer material preferably in a content i, for which the following applies

0.05 at.% < i < 60 at.%, with Me being taken as 100 at.%.

A further improvement in all different embodiments of at least one MeX layer is achieved by inserting an additional titanium nitride layer between the MeX layer and the tool body with a thickness d, for which the following holds:

0.05^<d<5gm

In view of the general objective of the present invention, which is to design a new tool that could be manufactured at the lowest possible cost and thus as economically as possible, it was further proposed that this tool be provided with only one layer of MeX material and an additional layer that is placed between the MeX layer and the tool body.

In addition, the stress σ in the MeX material is chosen so that its magnitude lies within the range

GPa < σ < 8 GPa , and even more preferably in the range

GPa < σ < 6 GPa

The titanium content x in the metal component is preferably selected such that at % > x > 40 at %, so that in another preferred embodiment at % > x > 55 at %

On the other hand, the content y of aluminum in the metal component Me of the material MeX is preferably chosen such that at % < y < 60 at % , while in another preferred embodiment at % < y < 45 at %

In yet another preferred embodiment, both of these ranges, i.e. the range relating to titanium and the range relating to aluminum, are met.

The deposition of the MeX layer in particular can be carried out by any known vacuum deposition technique,

Me of the MeX layer is • « • ·

especially by means of reactive PVD coating techniques such as reactive cathodic arc evaporation or reactive sputtering. By appropriate control of the process parameters that affect the growth of the coating, advantageous exploitation of the ζΑ range is achieved.

In order to achieve excellent and repeatable adhesion of the layers to the tool body, a plasma etching technology based on argon plasma was used as a preparatory step, as described in US-A-5,709,784, which document is incorporated herein by reference, in terms of such etching and subsequent coating. This document is in accordance with US patent application No. 08/710,095 of the same inventor(s) and assignee as this application.

Example 1

An arc ion plating apparatus using magnetically controlled arc sources as described in US-A-5,709,784 was used under the operating conditions shown in Table 1 to deposit a MeX layer as also shown in Table 1 on 10 mm diameter solid carbide end mills, z = 6. The thickness of the MeX layer deposited was always 3 μπι. Thus, for samples Nos. 1 to 5, the Qi values determined according to the present invention were used,

while for comparison condition met. wasn't for samples no. 6 up to 10 this Value 1(111) was always significantly bigger, than twenty times the average noise values, measured in compliance with MS.

Coated end mills were used for milling for • · • · • · 4 · · • · · · « · · ····· • · · ·

the following conditions to determine the milling distance achievable until an average width of the knife ridge is worn down to 0.20 mm. The resulting milling distance, corresponding to the service life of such tools, is also given in Table 1.

Test cutting conditions:

- Tool:

- Machined material:

- Cutting conditions:

Solid carbide end mill with a diameter of 10 mm, z - 6

AISI D2 (DIN 1.2379) v _c = 20 m/min f _t = 0.031 mm a _p = 15 mm a _e = 1 mm dry continuous milling

From the data contained in Table 1, it is quite clear that end mills coated in accordance with the subject matter of the present invention are much more protected against chipping and wear than end mills coated under comparative conditions.

Example 2

The equipment used for coating in accordance with Example 1 was also used for coating samples Nos. 11 to 20 according to Table 2. Coated tools and test • · • ·

The test conditions were the same as in Example 1. The layer thickness is given in Table 2.

It can be seen here that in addition to the coating in accordance with Example 1, an intermediate layer of titanium nitride was applied between the MeX layer and the tool body, and an outer layer of the appropriate material, as shown in Table 2. The conditions in terms of the 1(111) value and the average noise level, measured in accordance with MS, were amply met.

It should be noted here that the use of an intermediate layer between the MeX layer and the tool body already results in further improvement. Additional improvement is achieved by using an outer layer of one of the materials, such as titanium carbon nitride, titanium aluminum oxynitride and especially in the case of an outer layer of aluminum oxide. Again, it can be seen that the use of the determined Qx values according to the present invention, compared to the comparative samples No. 16 to 20, leads to a significant improvement.

The outer layer of aluminum oxide, 0.3 pm thick, was formed by plasma CVD.

As mentioned above, the coated end mills were tested under the same cutting conditions as those of Example 1, and the Q _T value was measured in accordance with MS.

Example 3

The solid carbide end mills were again coated with a MeX layer using the apparatus of Example 1, as shown in Table 3, which still meets the Q _Ir conditions determined in accordance with the subject matter of the present invention, and the 1(111) condition regarding the average noise level measured in accordance with MS. Thus, one of the elements from the group consisting of zirconium, hafnium, yttrium, silicon and chromium was included in the metal layer Me, in the above-mentioned amount.

The coated end mills were placed in an air oven at 750° C. for thirty minutes for oxidation. The resulting oxide layer thickness was then measured. These results are also shown in Table 3. For comparison purposes, inserts coated in accordance with the present invention with MeX material with different Me compositions were tested in the same manner. It is clear that by adding any of the elements in accordance with samples 23 to 32 to Me, the thickness of the resulting oxide coating is significantly reduced. From an oxidation point of view, the best results were achieved by adding silicon or yttrium.

It should be emphasized here that it is well known to a person skilled in the art that for the MeX material of the wear-resistant layers: The better the oxidation resistance, as a result of which the resulting oxidation coating is thinner, the better the cutting properties.

Example 4

Again, the same coating equipment and method were used as was also used for the samples according to Example 1.

• ·

Solid carbide end mills with a diameter of 10 mm and six teeth were coated with a 3.0 pm thick MeX layer, with a 0.08 pm thick TiN interlayer arranged between the MeX layer and the tool body. The test conditions for the end mills were as follows:

Tool: solid carbide end mill, diameter 6 mm, z = 6

Material: AISI D2 (DIN 1.2379)

HRC

Cutting parameters: v _c = 20 m/min f _t = 0.031 mm a _p = 15 mm a _e = 1 mm continuous dry milling

Solid carbide end mills were used until an average width of 0.20 mm was achieved on the knife edge. The results are shown in Table 4. Again, the 1(111) noise condition, measured in accordance with MS, was clearly met for sample No. 35, while the 1(200) noise condition was met for sample No. 34.

Example 5

The coating apparatus and method of Example 1 were used again.

Solid carbide ball end mills were coated with a 3.1 pm thick MeX layer and a 3.1 pm thick TiN interlayer. The steels were experimentally formed.

tested

00 0 0 ·

0 ·

0 · 0

I 0 0

0 0 0

0.07 μm. Coated tools through milling hardened

The test conditions were as follows:

Tool: - solid carbide ball nose cutter

J97 (Jabro), R4 (0 8 x 65 mm)

Material: forged steel H 11 (DIN 1.2343)

HRC 49.5

Cutting parameters: v _c = 220 m/min and _p = 0.5 mm without coolant

Tool life was evaluated in minutes.

The illustration according to Fig. 1 shows a graph showing the magnitude of the partial pressure of nitrogen as a function of the prestress of the tool body, which dependence is applied for reactive cathodic arc evaporation in the reactive PVD plating method used to implement the above-mentioned examples.

All process parameters of the cathodic arc evaporation method, in particular

- arc current, operating temperature, plating intensity, evaporated material, strength and arrangement of the magnetic field near the arc source, • · geometry and dimensions of the plated tool, operating chamber and were kept constant.

The remaining process parameters, in particular the partial pressure of the reactive gas (or total pressure) and the bias of the tool body to be plated as a workpiece, as well as with respect to a predetermined electrical reference potential, such as the ground potential of the chamber wall, were varied.

Under these conditions, titanium and aluminum nitride were deposited. Depending on the partial pressure of the reactive gas and the preload of the tool body, different operating points were established, and the resulting Qi values of the deposited hard material layers were measured in accordance with MS.

It should be emphasized here that in the graph shown in Fig. 1 there is a region P which extends in a first approximation linearly from at least the adjacent origin of the graph coordinates, the resulting layer leading to very low values of 1(200) and 1(111) XRD intensities. It is quite clear that to accurately determine the limits of the P region, a large number of measurements are necessary. Thus, none of the values of 1(200) and 1(111) intensities is as large as twenty times the average noise level measured in accordance with MS.

On one side of said region P, as shown in the representation according to Fig. 1, Qi is greater than 1, while in the other region Q _T is less than 1, with respect to the region Ρ. In both of these regions, at least one of the values 1(200) and 1(111) « ·

greater than twenty times the average noise level, measured in accordance with MS.

As shown by the arrows in the illustration of FIG. 1 , decreasing the partial pressure of the reactive gas (or the total pressure if it is practically equal to said partial pressure) and/or increasing the prestress of the plated tool body leads to a decrease in Qi.

Thus, a method for manufacturing a tool comprising a tool body and a wear-resistant layer system according to the present invention, which layer system comprises at least one layer of hard material, comprises the steps of reactive PVD depositing at least one layer of hard material in a vacuum chamber, then preselecting process parameter values for the PVD deposition process step, in addition to one or both of two process parameters, in particular the partial pressure of the reactive gas and the prestressing of the tool body.

It is one of these two parameters or both of these parameters which are then adjusted in order to achieve the desired Qx values, so that in accordance with the subject matter of the present invention the bias voltage is reduced and/or the partial pressure of the reactive gas is increased in order to achieve Qi values which, as mentioned above, have a value of at most 2, preferably at most 1 or even at most 0.5 or even at most 0.2. The most preferred value is

Qi < 0.1

In addition to the Qx value used in this invention, in the “right region” with respect to P, the 1(111) value is larger, namely • · · · · · · · · · · · · · · · · · · · · · · · · · · «·» ·· · · · · * · usually much larger than twenty times the average noise intensity level measured in accordance with MS.

The figure according to Fig. 2 shows a typical intensity versus angle 2Θ plot for a titanium aluminum nitride hard material layer deposited in the region Qi > 1 according to the present invention and according to Fig. 1, resulting in a Qi value of 5.4. The average noise level N* is much less than 1(200)/20. The measurement was carried out in accordance with MS.

The figure in Fig. 3 shows a graph analogous to that in Fig. 2, but where the deposition of titanium and aluminum nitride was controlled by means of bias voltage and nitrogen partial pressure in order to achieve a result of Qi < 1. The resulting value of Q _x has a magnitude of 0.03. Here, the value of 1(111) is greater than twenty times the average noise intensity level measured in accordance with MS.

It should be noted here that in the illustration according to Fig. 1, the respective Qx values in the respective regions are indicated at each operating point, measured in accordance with MS.

The illustration in Fig. 4 shows a graph that is analogous to the graphs in Fig. 2 and Fig. 3, and that applies to the operating point Ρχ in Fig. 1. It can be seen here that the intensities 1(200) and 1(111) are significantly reduced compared to the intensities in the region outside P. None of the values of 1(200) and 1(111) reach twenty times the average noise level N*.

Thus, by simply adjusting at least one of the two parameters Q _x controlling the reactive PVD process, namely the partial pressure of the reactive gas and the prestress of the workpiece, the value of Qi used according to the present invention is controlled.

The illustration according to Fig. 1 generically shows for dQs. < 0 the adjustment direction for decreasing Q _x , whereby it is clear that in the opposite direction of adjusting the two parameters for controlling the given process, an increase in Q i is achieved.

• · • · to Αί i—I 3 Λ fO H

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• · • · · · · · · · · · • · ·· ···*· * · • » · · · · · · · • · · · · # ·· ·“» ·♦

Table

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PATENTED

Claims (17)

Claims Tool with a tool body and a wear-resistant coating system, said coating system comprising at least one MeX layer, characterized in that: Me contains titanium and aluminum, X is at least one of nitrogen and carbon, said layer having a Qx value, defined as the ratio of bending intensity 1 (200) to bending intensity 1 (111), converted to X-ray diffraction planes (200) and (111) respectively in the material, using the θ - 2Θ method, whereupon the intensity values are measured using the following equipment and settings: Diffractometer Siemens Hole aperture: Detector diaphragm: Time constant: 2θ angular velocity: Radiation: wherein Q _T has a value D500 Operating voltage: 30 kV Operating current: 25 mA Aperture I position: 1 ° Aperture II position: 0.1 ° Soller slit 4 s 0.05 ° / min Cu-Ka (0.15406 nm) Qi <2 • · and wherein said tool is one of the following tool groups: solid carbide end milling cutter, solid carbide end milling cutter, cemented carbide cutting tool, the value of 1 (111) being at least 20 times the average noise intensity value . Tool according to claim 1, characterized in that for said Qi: Qi < 1 preferably then Q 1 - 0.5, and particularly preferably Qx < 0.2 and particularly preferably Qi <0.1 ♦ · · · · · ······· 9 9 9 9 9 9 · · · · Tool according to one of claims 1 or 2, characterized in that said MeX material is one of the group consisting of titanium and aluminum nitride, titanium, aluminum and carbon nitride, titanium, aluminum and boron nitride, and preferably one of the group , containing titanium nitride and aluminum and titanium nitride, aluminum and carbon. Tool according to one of claims 1 to 3, characterized in that Me further comprises at least one other element selected from the group consisting of boron, zirconium, hafnium, yttrium, silicon, tungsten, chromium, preferably at least one of the group , containing yttrium and silicon and boron. Tool according to claim 4, characterized in that said further element containing i is contained in Me 0,05 at. % <i <60 at. %, the Ti content being taken as 100 at. %. The tool of any one of claims 1 to 5, further comprising a further layer of titanium nitride between said at least one layer and said tool body, said further layer having a thickness d to which it applies 0.05 pm <d <5.0 pm The tool of claim 6, wherein said layer system is comprised of said at least one layer and said additional layer. Tool according to one of claims 1 to 7, characterized in that the stress σ in the at least one layer is 2 GPa <σ <8 GPa, preferably 4 GPa <σ <6 GPa. Tool according to one of claims 1 to 8, characterized in that the x content of titanium in Me is: 70 at. %> x> 40 at. %, preferably Tool according to one of claims 1 to 9, characterized in that the aluminum content y in said Me is: 30 at. % <y <60 at. preferably then 35 at. % <y <45 at. %. A method of manufacturing a tool comprising a tool body and layered system, resistant to wear, which contains at least one layer hard material, marked following u j i c steps: i like you m that contains reactive PVD deposition of at least one MeX layer on said body, wherein Me comprises titanium and aluminum, and x is at least one of nitrogen and carbon elements, selecting predetermined process parameter values for said PVD deposition, and in addition at least one of two parameters, relating to a partial pressure of the reactive gas in said vacuum chamber and biasing the tool body relative to a predetermined reference potential, adjusting at least said partial pressure and / or said bias to realize said layer with a desired Qi value which may be greater than or less , and to realize the magnitude of at least one of 1 (200) and 1 (111) to be at least twenty times greater than the average noise intensity value, and exploiting the fact that said Ch value as a function of partial pressure and preload decreases decreasing partial pressure and with increasing preload, wherein the value of Qi is defined as the ratio of the bending intensity 1 (200) to the bending intensity 1 (111) converted respectively to the X-ray bending planes (111) and (111) by the method Θ. - 2θ, then the intensity values are measured using the following equipment and setting: · · «· Diffractometer Siemens Hole aperture: Detector diaphragm: Time constant: 2θ angular velocity: Radiation: D500 Operating voltage: 30 kV Operating current: 25 mA Aperture I position: 1 ° Aperture II position: 0.1 ° Soller slit 4 p 0.05 ° / min Cu-Ka (0.15406 nm). The method of claim 11, further comprising the step of performing said reactive PVD deposition by reactive cathode arc evaporation. The method of claim 12, comprising the step of magnetic control of said arc evaporation. The method according to any one of claims 11 to 13, further comprising the step of depositing a MeX layer on said tool body, wherein Me comprises titanium and aluminum, and X is at least one of nitrogen and carbon comprising: is introduced into said PVD deposition by means of a reactive gas. Method according to one of Claims 11 to 14, characterized in that said tool is one of the following group: solid carbide end milling cutter, solid carbide end milling cutter, sintered carbide cutting tool, after which said tool is selected. value of Qi so that it holds Qx <2 by adjusting at least one of said reactive pressure and from said bias for said reactive PVD deposition. Method according to claim 15, characterized in that said value Qi is then selected to be valid Qx < 1, preferably then Qx <0.5, or even Qx <0.2 · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 17. The method of wherein said Q value _{of T,} such that in claim 16, it then selects