MXPA00002589A - Tool having a protective layer system - Google Patents
Tool having a protective layer systemInfo
- Publication number
- MXPA00002589A MXPA00002589A MXPA/A/2000/002589A MXPA00002589A MXPA00002589A MX PA00002589 A MXPA00002589 A MX PA00002589A MX PA00002589 A MXPA00002589 A MX PA00002589A MX PA00002589 A MXPA00002589 A MX PA00002589A
- Authority
- MX
- Mexico
- Prior art keywords
- tool
- layer
- titanium
- voltage
- aluminum
- Prior art date
Links
- 239000011241 protective layer Substances 0.000 title description 3
- 239000000463 material Substances 0.000 claims abstract description 37
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000007787 solid Substances 0.000 claims abstract description 13
- 239000010936 titanium Substances 0.000 claims abstract description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 10
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminum Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- 210000001331 Nose Anatomy 0.000 claims abstract description 5
- 229910052799 carbon Chemical group 0.000 claims abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000002441 X-ray diffraction Methods 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 32
- 238000001704 evaporation Methods 0.000 claims description 18
- -1 titanium-aluminum Chemical compound 0.000 claims description 16
- 210000000188 Diaphragm Anatomy 0.000 claims description 12
- 238000000151 deposition Methods 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 229910052796 boron Inorganic materials 0.000 claims description 5
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 5
- 229910052727 yttrium Inorganic materials 0.000 claims description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 4
- NRTOMJZYCJJWKI-UHFFFAOYSA-N titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 4
- 229910002483 Cu Ka Inorganic materials 0.000 claims description 3
- VBJZVLUMGGDVMO-UHFFFAOYSA-N Hafnium Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 3
- 239000011651 chromium Substances 0.000 claims description 3
- 229910052735 hafnium Inorganic materials 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 230000001276 controlling effect Effects 0.000 claims description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 239000010937 tungsten Substances 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 abstract description 10
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 abstract 1
- 238000000034 method Methods 0.000 description 97
- 238000000576 coating method Methods 0.000 description 63
- 239000011248 coating agent Substances 0.000 description 60
- 238000010891 electric arc Methods 0.000 description 52
- 239000010410 layer Substances 0.000 description 42
- 210000002381 Plasma Anatomy 0.000 description 28
- 239000000126 substance Substances 0.000 description 25
- 238000009826 distribution Methods 0.000 description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 14
- 239000000758 substrate Substances 0.000 description 14
- 238000005516 engineering process Methods 0.000 description 13
- 150000002500 ions Chemical class 0.000 description 11
- 229910052756 noble gas Inorganic materials 0.000 description 11
- 229910052786 argon Inorganic materials 0.000 description 8
- 238000010586 diagram Methods 0.000 description 6
- 238000005096 rolling process Methods 0.000 description 6
- 230000000875 corresponding Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 238000004544 sputter deposition Methods 0.000 description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N tin hydride Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 5
- 230000001133 acceleration Effects 0.000 description 4
- 238000003486 chemical etching Methods 0.000 description 4
- 238000010849 ion bombardment Methods 0.000 description 4
- 238000005530 etching Methods 0.000 description 3
- 238000011068 load Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000002800 charge carrier Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000010192 crystallographic characterization Methods 0.000 description 2
- 239000012212 insulator Substances 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003071 parasitic Effects 0.000 description 2
- 238000001771 vacuum deposition Methods 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- 229910001208 Crucible steel Inorganic materials 0.000 description 1
- 240000001441 Fragaria vesca Species 0.000 description 1
- 241000890403 Ligustrum virus A Species 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 241000196252 Ulva Species 0.000 description 1
- OMTZRXWMULHIFQ-UHFFFAOYSA-N [Al].B#[Ti] Chemical compound [Al].B#[Ti] OMTZRXWMULHIFQ-UHFFFAOYSA-N 0.000 description 1
- 238000005296 abrasive Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N al2o3 Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000001808 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000004059 degradation Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 230000002349 favourable Effects 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000004301 light adaptation Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000002835 noble gases Chemical class 0.000 description 1
- 230000002093 peripheral Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 235000021012 strawberries Nutrition 0.000 description 1
- 230000000576 supplementary Effects 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 238000009489 vacuum treatment Methods 0.000 description 1
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 aluminum and X is a nitrogen or carbon. The tool is a solid carbide end mill, a solid carbide ball nose mill or a cemented carbide gear cutting tool. 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&thgr;-2&thgr;method is selected to be=2. 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 WITH PROTECTIVE LAYER SYSTEM
DESCRIPTION OF THE INVENTION
This description has an Appendix A. The present invention is directed to a tool with a tool body and a protective layer system, wherein the layer system comprises at least one layer of MeX, wherein: I comprises titanium or aluminum, • X is at least one of nitrogen and carbon.
Definition • The term Q? is defined as the ratio of the intensities of diffraction 1 (200) to 1 (111), assigned respectively to the planes (200) and (111) in the X-ray diffraction of a material using the T-2T method. In this way, it is valid Q, = l (200) / l (111). The
• intensity values were measured with the following equipment and with the following parameters: 20 Siemens D500 diffractometer Power: Operating voltage: 30 kV Operating current: 25 mA Opening diaphragms: Diaphragm position I: 1st Diaphragm position II: 0.1 ° 25 Detector Diaphragm: Soller Slot
Time constant: 4 s Angular speed 2 ?: 0.05 ° / min. Radiation: Cu-Ka (0.15406 nm) When referring to "measured according to MS", this equipment and these parameters are referred to. In this way, all the quantitative results for Q | and I through this application have been measured through MS. • "Tool body" means the uncoated tool. 10 • "Hard material" means a material with which the tools, which are mechanically and thermally loaded in high form during operation, are coated for wear resistance. Preferred examples of such materials are referred to below as MeX materials. It is well known in the tool protection art to provide wear resistant layer systems, which comprise at least one layer of a hard material, as defined by MeX. The present invention has the object of significantly improving the life time of said tools. This is solved by selecting for this layer a value of Q ?, for which Q is valid? > In accordance with the present invention, it has been recognized that the 25 Qi values as specified lead to an improvement
^^^ JjJ ^^^^^ & ^^^^^^ exceptionally high wear resistance, and thus a tool's lifetime, if such a tool is of the specified type. Up to now, the application of systems of a wear resistant layer of MeX hard material was carried out without considering the interaction between the material of the tool body and the mechanical and thermal load of the tool to which it is subjected during operation. The present invention in this manner resides in the fact that it has been recognized that an extraordinary improvement in wear resistance can be achieved when the value of Q? with the specific type of tools, thus providing a value of 1 (200) greater by a factor of at least 20 than the level of the average noise intensity, both measured with MS. The improvement achieved by the invention is even increased if Q? is selected to be at least 1, and still a further improvement is made by selecting Q? so that at most it is 0.5 or even at a lot of 0.2. The greatest improvements are achieved if Q? it's at about 0.1. It must be established that Q? it can fall to zero, if the layer material is achieved with a single crystal orientation according to a fading diffraction intensity 1 (200). Therefore, no lower limit has been set for Q ?, which has only been fixed by practical aspects. As is known to those skilled in the art, there is a correlation between the hardness of a layer and its tension. The more
High is the tension, the higher the hardness. However, with high tension, adhesion to the tool body tends to decrease. • For the tool according to the present invention, a high hardness is much more important than the best possible adhesion. Therefore, the tension in the MeX layer is advantageously selected rather at the upper end of the voltage scale given below. These considerations limit in practice the value of Q | that can be exploited. In a preferred embodiment of the tool of the invention,
• The MeX material of the tool is titanium-aluminum nitride, titanium-aluminum carbonitride or titanium-aluminum-boron nitride, so the first two materials mentioned today are preferred over titanium-aluminum nitride- boron. In a further form of the embodiment of the tool of the invention, Me of the MeX layer material may further comprise at least one of the elements of the group consisting of boron, zirconium, hafnium, yttrium, silicon, tungsten, chromium, therefore, outside this group, it is preferred to use yttrium and / or silicon and / or boron. Saying
additional element to the titanium and aluminum is introduced into the layer material, preferably with a content i, for which is valid 0.05 to% < i < 60 to%, taking Me as 100 in%. A further improvement in all the different modalities of
at least one layer of MeX is achieved by introducing a layer
riataMrikÉj ^ | -MtaBMk ^ Additional éf of titanium nitride between the MeX layer and the tool body with a thickness d, for which the validity is 0.05 μm < d < .5 μm. • In view of the general object of the present invention, which is to propose that the tool of the invention can be manufactured at costs as low as possible and thus more economically, it is further proposed that the tool has only one layer of material of MeX and the additional layer, which is deposited between the MeX layer and the tool body. 10 In addition, the voltage s in MeX is preferably selected
• to be 2 GPa < _ s < _ 8 GPa, so most preferably within the 4 GPa < s < 6 GPa. The content of x of titanium in the Me component of the MeX layer is preferably selected to be 70 to% > _ x > _ 40 to%, so in a further preferred embodiment within the scale 65 to% > x > 55 to%. On the other hand, the content of y of aluminum in the Me component of the MeX material is preferably selected to be 30 to% < and < 60 to%, in a preferred additional mode where 35 a < and < 45 to% 25 In another more preferred modality, both scales, that is, with
* E *? M? M &? ßfc ~ A **** < ,, *. * - > * - '- r * 8 ^ 1 ^^^ JÉ3tU J__LL? ^ __ -L ^^ J ^ l ^ J ^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^ with respect to aluminum, they are satisfied. The deposition, especially of the MeX layer, can be carried out by any known vacuum deposition technique, especially by means of a coating technique with reactive PVD, for example, reactive cathodic arc evaporation or reactive cathodic deposition. By properly controlling the parameters of the process, which have an influence on the development of the coating, the Q scale is obtained? exploited by the invention. To achieve an excellent adhesion and capable of being reproduced
of the layers to the tool body, a technology of
• plasma chemical attack, as a preparatory step, based on an argon plasma as described in Appendix A, said document is integrated to this description by reference, with respect to said chemical attack and subsequent coating. East
document in accordance with the request of E.U.A. No. 08 / 710,095 of the same inventor (two inventors) and the applicant of the present application. •
Example 1 An arc ion deposition apparatus was used, using magnetically controlled arc sources, as described in Appendix A, operated as shown in Table 1 to deposit the MeX layer also as set forth in Table 1. on solid carbide terminal laminates with a diameter of 10 mm,
z = 6. The thickness of the deposited MeX layer was always 3
da¡¡ ^ úaÉÉü «Ui & mm. So, in samples Nos. 1 to 5, the values of Q? Established by the invention were obtained, while, by comparison, in samples Nos. 6 to 10, this condition was not satisfied. The value of 1 (111) was always significantly greater than 20 times the value of the average noise intensity, measured according to MS. The coated terminal laminates were used for lamination under the conditions set forth below to find the rolling distance that can be obtained to achieve an average width of the flank wear of
0.20 mm. The resulting rolling distance according to the duration of said tools is also shown in Table 1. Test cut conditions: Tool: solid carbide terminal laminate, diameter 10 mm, z = 6 15 Material to be cut: AISI D2 (DIN 1.2379) Cutting parameters: Vc = 20 m / min. ft = 0.031 mm ap = 15 mm aP = 1 mm 20 concurrent, dry laminate It can be clearly recognized from Table 1 that the terminal laminates, coated according to the present invention, are significantly more protected against delamination and wear than the laminates. coated laminates of
according to the comparison conditions.
Table 1 co
Example 2 The apparatus that was used for coating according to Example 1 was also used to coat samples Nos. 11 to
• 20 of Table 2. The coated tools and the conditions of
The test was identical to Example 1. The thickness of the layers is indicated in Table 2. It can be seen that in addition to the coating according to Example 1, an intermediate layer of titanium nitride was applied between the layer of MeX and the tool body and an outermost layer 10 of the respective material as set forth in Table 2. The condition with respect to 1 (111) and average noise level, measured according to MS, was greatly satisfied. It can be seen that the provision of the intermediate layer between the MeX layer and the tool body already resulted in a further improvement. A further improvement was obtained by providing an outermost layer of one of the materials of titanium carbonitride, titanium-aluminum oxynitride and especially with an outermost layer of aluminum oxide, again, it can be seen that obtaining the values of Q? established by the invention with
like those of Example 1, Q? it was measured according to MS
* i. ... ,, > .....,,. **. * .... ..... ...., _ ****. ** **. * .. ^ x ** ^ *** ^ *, .., ^ _ ^^^? *? _ L ¿»ux * * * Table 2
Example 3 Again, cemented carbide inserts were coated with the apparatus of Example 1 with the MeX layer as set forth in
• Table 3, again the conditions of Q are satisfied? established by the invention and, further, the condition of 1 (200) with respect to the average noise level, measured in accordance with MS. In this way one of zirconium, hafnium, yttrium, silicon and chromium was introduced, with the amount established above, in Me. The coated inserts were kept in an air oven at 10 750 ° C for 30 minutes for oxidation. Then, the resulting thickness of the oxide layer was measured. These results are also shown in Table 3. For comparison, inserts coated with the invention were also tested with different Me compounds from the MeX material. It became evident that by adding any of the elements according to samples 23 to 32 to Me, the thickness of the resulting oxide film was significantly reduced. With respect to oxidation, the best results were obtained by adding silicon or yttrium. It is a signal that is known to those skilled in the art that the wear-resistant layers of the MeX material is valid: the better the oxidation resistance, the thinner the resulting oxide film is, and the better the cutting performance.
.- **** siM - * - i.x ¿tme * - *** - **
Table 3
?
Example 4 Again an apparatus and a coating method such as those for the samples of Example 1 were used. Solid carbide end laminates with a diameter of 10 mm with 6 teeth were coated with a MeX layer of 3.0 μm. An intermediate layer of titanium nitride with a thickness of 0.08 μm between MeX and the tool body was provided. The test conditions for the terminal laminates were: Tool: solid carbide terminal laminate, diameter 10 10 mm, z = 6 Material: AISI D2 (DIN 1.2379) 60 HRC Cutting parameters: vc = 20 m / min. f, = 0.031 mm 15 ap = 15 mm ae = 1 mm concurrent laminate, dry The solid carbide terminal laminates were used until an average flank wear width of 20 0.20 mm was obtained. The result is shown in Table 4. Again, the condition of 1 (111) to noise, measured with MS, was clearly satisfied for sample No. 35, for sample No. 34, the condition of 1 (200) The noise was not satisfied.
^ c ^^^ Afc. - -,. - ihfüNt ---, - -T- t i n.-i, - n rr i (MMI ^^^^^^ M ^^^ MJÍÍ ^ É •
Table 4
n
Example 5 The apparatus and the coating method according to Example 1 were used. Solid carbide ball nose laminates were coated with
MeX of 3.1 μm and an intermediate layer of TiN with the thickness of 0.07 μm. The coated tools were tested with the lamination of a hardened mold steel. Test conditions: Tool: J97 laminated solid carbide ball nose 10 (Jabro), R4 (O 8 x 65 mm) • Material: Cast steel H 11 (DIN 1.2343), HRC 49.5 Cutting parameters: vc = 220 m / min ap = 0.5 mm 15 without cooler The life of the tool was evaluated in minutes.
Table 5
^ l
In Figure 1, it is shown, with a line plotting a partial pressure diagram of nitrogen versus tool body deflection voltage as applied for reactive cathode arc evaporation as the reactive PVD deposition method used to carry out the examples that they were discussed earlier. All parameters of the cathodic arc evaporation process, mainly: - arc current; process temperature; deposition speed; evaporated material; resistance and configuration of the magnetic field adjacent to the arc source; geometry and dimensions of the process chamber and the workpiece tool that will be treated, were kept constant. The remaining process parameters, mainly the partial pressure of the reactive gas, or total pressure, and the deflection voltage of the tool body that will be coated as a workpiece and with respect to a predetermined electrical reference potential, such as the potential to ground of the chamber wall, were variable. In this way, the titanium-aluminum nitride was deposited. With respect to the partial pressure of reactive gas and the deviation voltage of the tool body, different working points were established and the values of Q? resulting in deposited hard material layers were measured according to MS.
• It turns out that there exists in the diagram according to Figure 5 1, an area P, which extends in a first approximation linearity from at least adjacent to the origin of the coordinates of the diagram, where the resulting layer leads to very low XRD intensity values of 1 (200) and 1 (111). It is evident that to determine exactly the limits of P, one will have to
perform a high number of measurements. So, none of the
• values of intensity 1 (200) and 1 (111) is as large as 20 times the average level of noise, measured according to MS. On one side of this area P and as shown in Figure 1, Q, is greater than 1, in the other area with respect to P, Q? is less than 1. 15 In both areas at least one of the values 1 (200), 1 (111) is greater than 20 times the average noise level, measured according to MS. • As shown by the arrows in Figure 1, the reduction of the partial pressure of the reactive gas, or of the total pressure if
practically equal to said partial pressure, and / or the elevation of the deflection voltage of the tool body being coated, leads to the reduction of Q |. In this way, the method of the invention for producing a tool comprising a tool body and a resistant layer system
to wear, the latter comprises at least one layer of hard material, comprises the steps of depositing reactive PVD in at least one layer of hard material in a vacuum chamber, thus preselecting the values of the process parameter for the passage of PVD deposition process in addition to either or both of the two process parameters, mainly the partial pressure of the reactive gas and the deflection voltage of the tool body. Is one of these two parameters or both the ones that later adjust to produce the Q values? desired, in this manner, and in accordance with the present invention, the deviation voltage is increased and / or the partial reactive gas pressure is reduced to obtain the values of Q (, which are, as explained above, as a lot of 2, preferably at most 1 or even at a lot of 0.5 or even at a lot of 0.2 Very preferred is Q | <; _ 0.1. In addition, the Q value, exploited by the invention, in this area "on the right hand", with respect to P, 1 (111) is greater, much larger than 20 times the average intensity level of the noise, measured in accordance with MS In Figure 2, a diagram of intensity versus angle 2T typical for the hard material layer of titanium-aluminum nitride deposited in the region of Q? > 1 of figure 1, resulting in a value for Q? of 5.4. The average noise level N * is much lower than l (200) / 20. The measurement was made according to MS. In Figure 3, a diagram is shown in analogy with that of Figure 2, but deposition of titanium-aluminum nitride- ~ * H > --.- * - ~ - - -'ni i? "?, a-jw ÉáHáaamM? k * s¡_ ^.
being controlled by the deviation voltage and the partial pressure of nitrogen to result, in the form of the invention, Q? < _ 1. The value of Q, resulting is 0.03. Here, again the value of 1 (111) is greater than 20 times the average noise intensity level, both measured according to MS. Please observe in Figure 1 the values of Q? respective in the respective regions that are observed in each work point measured (according to MS). In Figure 4, a diagram is illustrated in analogy with that of Figures 2 and 3 to work point P < of Figure 1. It can be seen that the intensities 1 (200) and 1 (111) are significantly reduced, compared with those in the external area of P. None of the values of 1 (200) and 1 (111) reaches the value of 20 times the average noise level, N *. In this way, simply by adjusting at least one of the two QD control reactive PVD process parameters mainly the partial pressure of the reactive gas and the workpiece by-pass voltage, the value of Q is controlled? exploited in the invention. In Figure 1 is shown generically < 9Q? < 0, the adjustment direction to reduce Q ?, and it is obvious that in the opposite direction of adjustment of the two control process parameters, and an increase of Q?
-,.
"APPENDIX A" PROCESS AND APPARATUS FOR COATING A WORKPIECE DESCRIPTION OF THE INVENTION • The present invention relates to a coating arrangement according to the generic manufacture of claim 1, as well as a process for coating work pieces of the invention. According to the generic specification of claim 14. In many vacuum treatment processes, the cleaning of the workpiece surface is carried out before the vacuum coating. In addition, the workpieces can be heated to the desired temperature before or after the cleaning step. These steps are mainly necessary to ensure adequate resistance to the adhesion of the coating that will be deposited. This is especially important in applications where work pieces, in particular tools, are to be coated with a wear protection coating. In tools such as drills, milling cutters, traction reamers and forming dies, these coatings are subjected to very high mechanical and abrasive stress. An extremely good bond with the substrate is, therefore, essential for the useful and economical use. An improved method for pre-treating such tools is heating with electron bombardment, and chemical attack through ion attack, for example, sputtering attack. The heating by bombardment of electrons from a plasma discharge is known, for example, from DE 33
* ^ - ~ ^ * á *** HU * -A. . -. i í *. * A-AL! < * - *. . *. .,. *** t -. * .. * .- 4f-f ..-^ __ ^ L ^^ M_; _ ^ ¡| ^ jjjj ggi ^ 30 144. A discharge path of plasma to create heavy noble gas ions, for example, argon ions, which are accelerated from this plasma to the workpiece or
the substrate on which it causes the sputtering attack as described in DE 2823 876. In addition to the sputtering attack, another known technique is to operate plasma discharges with additional reactive gases and chemically attack the work pieces, without
However, process techniques are also reliable that combine
• Reactive chemical attack and sputtering attack. The object of these pretreatment processes is to prepare the surface of the workpiece in such a way that the subsequently deposited coating adheres very well to the substrate. For the generation of plasma, the aforementioned arrangements use a low-voltage arc discharge that is arranged in the central axis of the apparatus, while the pieces of
• Work is arranged at a certain distance around this arch along a cylindrical surface. The coating subsequently
is deposited through thermal evaporation or cathodic deposition. Depending on the handling of the process, an additional ion bombardment is generated during the coating through a corresponding substrate displacement, a technique that is known as ionic sedimentation. The advantage of this provision
is that large ion currents with a small energy of
particle can be extracted from the low voltage arc, which offers a moderate treatment of the work piece. However, the disadvantage is that the work pieces must be arranged in a zone defined radially to the discharge and that as a rule they must
to rotate around the central axis as well as its own axis in order to obtain uniform results and capable of being reproduced. Another disadvantage is that due to the relatively narrow width of the admissible cylindrical processing band, both the
size of the workable workpiece is limited as the size
• the lot is limited to a large number of small workpieces, which severely limits the cost effectiveness of the known provisions. This limitation is due to the fact that the low voltage arc discharge, which centrally penetrates the
process chamber, requires a certain dimension for itself. In order to produce good and reproducible results, the work pieces must have an adequate distance from the
• discharge, which means that a large portion of the central processing chamber space can not be used. The arrangements of cathodic deposition with so-called diode discharges are also known. These diode discharges are operated with high voltages up to 1000 volts and even higher. Diode attack devices have proven not to be suitable for applications with demand requirements. On the one hand,
obtainable chemical attack regimes and consequently the
efficiency is low, and on the other hand these high voltages can produce defects on sensitive substrates. In particular, work pieces that require three-dimensional processing such as tools, can not be easily processed through said arrangement. For example, the tools are designed with a number of thin cutting edges on which said discharges tend to concentrate, resulting in uncontrolled effects such as overheating and even destruction of the functional edge may occur at the fine edges and points. In the patent application DE 41 25 365, an aspect to solve the aforementioned problem is described. It is assumed that the coating is deposited through a so-called arc evaporation process. In order to produce good adhesion coating with said evaporators, the arc of the same evaporator was used before the actual coating in such a way that the ions produced in the arc, particularly the metal ions, are accelerated out of the evaporation objective towards the workpieces through a negative acceleration voltage typically of > 500 volts, but usually also on the scale of 800 to 1000 volts, so that more material is deposited cathodically on the work piece than the one deposited. After this chemical attack process, the evaporator is operated as a coating source. The description mentions that in the usual processes based on arc coating technology, such high
1 . «. . . TO**.-*.. *.*.. . .- - «-. - * - *- .. TO, .... . • ^^ * M ^ _L? Ai &jÉ! ¿- - voltages are necessary to produce coatings of good adhesion through the process of arc evaporation. In order to avoid the problem of overheating or chemical attack on the uneven mass distribution or on fine work piece geometries, the description proposes to operate, in addition to the arc plasma, an auxiliary discharge path with high voltage that causes the supplementary ionization, which is coupled to the evaporation arc. An additional DC source causes the ions to be extracted from the plasma and accelerated to the workpiece and
thus produce the desired chemical attack effect. An additional anode with another discharge path operated from a separate power supply is considered to increase the effect. During the chemical attack process, the arc evaporator is operated with a closed shutter, so that the substrate is
protected from the direct effect of the evaporator, thus avoiding so-called drops on the substrate. The disadvantage of the previous arrangement is that it also requires a high voltage, that only limited processing homogeneities can be obtained, and that also through
of the coupling of the different plasma trajectories also the adjustment capacities in the operating environments are limited. Furthermore, this arrangement is very complicated and consequently very expensive to develop and operate, which seriously damages the economy of a production system.
using voltage in excess of 1000 volts requires
Additional safety precautions. Systems based on current technology are not very suitable for high productions, if a high quality of processing is also required. Systems that adapt widths
coating of up to 1000 mm and more, can be developed only with great difficulty, if not all. The purpose of the present invention is to eliminate the aforementioned disadvantages of current technology, in particular by creating a coating arrangement and proposing a process
that is suitable for depositing coatings of good adhesion
• on a large number of workpieces, or on individual large workpieces with an uneven mass distribution, without damaging the fine structures, but with the desired homogeneity and the highly economical processing regime, required. This is achieved by designing the process arrangement mentioned at the beginning in accordance with the characterization portion of claim 1, and by the designed coating process of
• according to the characterization portion of claim 14. Accordingly, the workpiece surface that will be
The coated coating is exposed to a plasma source designed as a hot cathode low voltage arc discharge arrangement conveying it inversely to the linear degree of the last discharge path. The work piece is connected to a negative voltage, so that the pieces are extracted from the arc discharge and
accelerated towards the work piece, causing the latter to be attacked by sputtering. Subsequently, the workpiece is coated on the same side from which the low voltage arc discharge was effective. The preferred design variants of the coating arrangement according to the invention are described in the subsidiary claims 2 to 13, and the preferred design variants of the process in claims 14 to 17. The chemical etching with an arc discharge arrangement Low-voltage hot cathode as the ion source is particularly advantageous since said arc discharges can be operated with discharge voltages of < 200 volts, which means that this process is not obstructed by the disadvantages of high-voltage chemical attack. Chemical attack with low voltage arc discharges is also particularly non-hazardous for the workpiece, that is, thin structures in larger workpieces, such as cutting edges, are not adversely affected by thermal overload nor because of the edge rounding caused by the high-energy ion bombardment. Despite the relatively low discharge voltage in the working range of 30 to 200 volts DC but preferably within the range of 30 to 120 volts, a very high discharge current of 10 to 100 amps, preferably 100 to 300 amps, is reliable. amperes. This means that this type of discharge is capable of producing a very high ion current at low energy. Due to the high current available, high speed can be achieved
ii) Finish the chemical attack on the substrate at a relatively low acceleration voltage, and as mentioned above, with moderate treatment of the workpiece. The extraction voltage
• or the acceleration voltage on the substrate is within the range of -50 volts to -300 volts, preferably within the range of -100 volts to -200 volts. The ionic current expelled to the work pieces achieves values of 5 to 20 amperes, with a preferred working scale of 8 to 16 amperes. The processing width for the workpiece or work pieces can be
of up to 1000 mm. With a slightly more elaborate computer design, also larger processing widths are reliable. The values obtainable depend not only on the operating values for the arc discharge, but also on its geometrical disposition in relation to the work piece, as well as
at the selected working pressure. Typical working pressures are of the order of 10 3 mbars.To operate the arc discharge, a noble gas is used as the working gas, preferably a heavy noble gas such as argon. low bow
The voltage was rotated symmetrically, which means that the arc discharge was arranged in the center and the workpieces were rotated around this arc discharge located on the central axis. The assumption was that the symmetric arrangement of rotation with the centrally arranged arc discharge could offer the best
possible result with respect to the uniformity and speed of
a ^ MMÍHÍ ^^ AÉriÍ chemical attack operation. Surprisingly, it has been shown, however, that the asymmetric arrangement provided by the invention is above all much more advantageous than the above-mentioned symmetrical rotation arrangement. With a provision
symmetric rotation with the discharge of arc in the central axis, the placement of workpieces of large volume is restricted towards the center by the same arc discharge. Furthermore, said workpieces have to be rotated not only around the central axis, but also around their own axis so that
After the etching process, the attacked workpiece surfaces can be immediately coated with the coating sources disposed on the chamber wall. Only in this way is the proper distribution of the etching process achieved and the coating thickness secured. It has also been shown that the distance of the work piece from the arc discharge is more critical in a symmetrical rotation arrangement than in an asymmetric arrangement where the work piece is exposed only from one side towards the arc discharge. In the apparatus according to the invention, it is possible to pass large-volume workpieces in front of the arc discharge without additional rotation, with the result that the size of the process chamber can be kept within reasonable limits and the handling of heavy workpieces is enormously
simplified. This has a major influence on the economy of
production systems. The arrangement according to the invention is advantageous not only for high-volume workpieces, but it is also possible to accommodate and simultaneously process a correspondingly large number of smaller workpieces. Another advantage of the arrangement according to the invention is that the chemical etching apparatus no longer has to be constructed as an integral part of the process chamber, since it only needs to be disposed in the area of the process chamber wall. which means that it can be arranged as a smaller, elongated discharge chamber on the external wall of the latter, so that a greater freedom in the design of the process chamber is achieved. It has further been found that this arrangement is less critical with respect to the distance between the arc discharge and the workpiece surface, which means that a superior reproducibility of the results is achieved with greater separation variations that typically occur with larger work pieces. The total ionic current that can be extracted from the arc discharge still advantageously reaches high values and can be concentrated entirely on the workpieces, thus producing the desired high etch rates. The actual separation of the low-voltage arc discharge or the plasma source from the process chamber or from the treatment zone also offers a greater degree of freedom in the design of this source and consequently much more adaptation.
. i *,. - * .-. - - - »» - .. > -. - * - > - -, i i.i.A'ía? tÁr-íA i, flexible of the source design for the process requirements that in the case with the symmetric arrangement of integral rotation with discharge in the central axis of the equipment. To deposit a good adhesion coating r the etching process, one or more additional evaporation sources acting from the same side are disposed on the chamber wall of the process. Particularly suitable are sources that can be arranged in such a way that, like the elongated low voltage discharge, they coat the work pieces
transported in front of them through an area
• correspondingly enlarged. Sources such as sources of cathodic deposition or sources of arc evaporation are suitable. The practice has shown that the so-called cathode spark gap evaporators or arc evaporators are particularly
suitable, since coatings of good adhesion through these and the preceding chemical etching process can be economically produced. The test tools processed through this arrangement achieved a useful life that was significantly and reproducibly longer than that obtained from
through known arc evaporator coatings with the preceding high-voltage chemical etching. For example, the useful life of cutting tools such as strawberries was improved by a factor of at least 1.5; particularly in favorable cases even by a multiple on conventional techniques. In addition, it was achieved
a much more homogeneous chemical attack distribution, which
it depends less on the geometry of the work piece and also allows the mixing of different substrates in a batch. With the proposed arrangement, it is also easily possible to implement processes not only with noble gases, but also with chemically active gases, since the low-voltage arc discharge activates gases such as N2, H2, very well. Unwanted parasitic discharges produced by insulating surfaces can be easily controlled with low voltage discharge. The low voltage arc discharge is preferably operated with a separate cathode chamber or ionization chamber, which adapts a hot cathode and communicates with the discharge chamber or process chamber only through a small opening. The gases are preferably admitted through this cathode chamber. This results in some gas separation between the process chamber and the coating sources, which reduces or eliminates the objective contamination problem. With this arrangement, it is also possible to activate the workpiece with different process gases during the actual coating phase. The desired working conditions can be established by selecting a corresponding positive negative voltage on the work piece. Since the workpieces generally have to pass in front of the sources several times during a process step in order to achieve the necessary depth of chemical attack or coating thickness, as well as a uniform and reproducible treatment, it is advantageous to design the apparatus in such a way that the workpieces can be rotated around a central axis and arrange the sources on the chamber wall in such a way that
• all work from the outside to the inside. In this case, a very large work piece can be arranged for processing in such a way that it rotates on its own axis. In the same space, however, also a large number of small work pieces, even of different sizes, can be arranged on a support and passed through the fountains, while rotating around
this central axis in order to achieve homogeneous results. Bliss
• provision is particularly compact and easy to develop, which is essential for an economic process. The plasma source or the low voltage arc discharge is preferably disposed on the process chamber wall,
transversely to the transport direction. The low voltage arc discharge device can, for example, and preferably, be disposed in a box type junction, here in the
• shape of a discharge chamber, which is connected to the process chamber through a long narrow opening of such
Thus, the low voltage arc is arranged directly opposite the workpiece (s) or the zone that will be processed. The low voltage arc discharge is generated by an electrically heated or thermionic emitting cathode and an anode arranged at a certain distance. A corresponding discharge voltage is
applied to this anode, causing an arc current to be
A.jiSaSt * £ - ***. I **? * Jí - ?. aáA * t. i. ,. . J..1..Í. ..._, ... - * ,, * ..%, ... * ..... *., .. * .- .. * *. * -u i *. x. i * extracted. This discharge characterizes a gas inlet port through which the arc discharge is supplied with the working gas. This arrangement is preferably operated with a noble gas such as argon, but as mentioned above, reactive gases can also be added. The size of the discharge path should be at least 80% of the width of the treatment zone and be placed relative to the treatment zone in such a way that the desired treatment distribution or homogeneity can be obtained. To achieve the corresponding cathodic deposition attack on the work piece, the latter or the workpiece holder is operated with a negative voltage in relation to the arc discharge arrangement. Depending on the process, such as in reactive processes during coating, the arrangement can also be operated if said voltage or even with a positive voltage, that is, with electron bombardment. In addition to a DC voltage, a medium-frequency or high-frequency AC voltage can also be used, and the overlap of DC over AC is also recommended. The DC voltage can also be transmitted by pulses, and it is possible to superimpose only a part of it on the AC supply. With this supply, it is possible to control certain reactive processes. Also, in particular, it can avoid or prevent parasitic arcs if dielectric zones exist or are formed in the equipment and surfaces of the workpiece. The desired distribution with respect to the processing zone can be set through the length of the discharge and its location. Another parameter to control the distribution is the distribution of plasma density along the arc discharge. This distribution can be, for example, influenced by the aid of additional magnetic fields, which are arranged in the area of the discharge chamber. For fixing and correcting the process parameters, permanent magnets are placed along the discharge chamber. However, better results are obtained if the trajectory of
discharge is operated with additional anodes, operated in
• Separate, which are arranged along the discharge path according to the distribution requirements. With such a provision, even the distribution curve can be influenced to some degree. Therefore, the arrangement is preferred
without corrections and with more than one anode along the discharge path. However, it is also possible to combine this preferred arrangement with additional correction magnets. The
• Additional anodes can be easily operated in combination with a single cathode. However, it is advantageous to have a cathode of
emission opposite to each anode in order to obtain an optimal decoupling of these circuits, which in turn improves the control capacity. The thermionic emission cathode is preferably arranged in a small, separate cathode chamber, which communicates
with the discharge chamber through a small entrance. This cathode chamber is preferably equipped with an inlet port for a noble gas. If desired, reactive gases can also be admitted through this gas inlet. Preferably, the reactive gases are not admitted to the cathode chamber but, for example, in the discharge chamber itself. Through the opening in the cathode chamber, the electrons are expelled towards the anode or anodes, so that the gas that is at least partially ionized also emerges from this opening. The process chamber is preferably designed in such a way that the central axis
around which the workpieces are rotated, is
• arranged vertically. The cathode or cathode chamber is preferably arranged above the anode. In the cathode chamber, the outlet opening preferably is disposed downward. These provisions simplify the entire management of the system and
help avoid problems that can be caused by the formation of particles. In addition to the low voltage arc discharge arrangement,
• the process chamber is equipped with at least one additional source, preferably in the form of an arc evaporator. 20 These sources act radially in the same direction from the outside towards the central axis or the processing zone. It is advantageous if the low voltage arc discharge is disposed before the coating source with respect to the transport direction An arc evaporator, such as the discharge arrangement
of arc, usually has a linear degree that is transverse to the direction of transport, so that the entire processing zone can be coated with the desired homogeneity. In the proposed coating arrangement, several round arc evaporators are preferably used, which are distributed along the chamber wall in such a manner as to obtain the desired homogeneity. The advantage is that the high energy consumption of the evaporator can be divided and that the thickness distribution of the coating can be controlled better or to a certain degree in order to be adjusted through the power supply. In this way, exceptionally high coating speeds can be obtained, which results in high economy. For example, a process for tools, particularly given trainers, could be configured as follows:
Process Example The system configuration corresponds to illustrations 2 and 3. The tools are not rotated around their own axis, but are only passed in front of the sources by rotating the workpiece holder around its axis central. A coating area with a width b of 1000 mm and a diameter d of 700 mm is formed, within which the workpieces are arranged. The process chamber has a diameter of 1200 mm and a height of 1300 mm. Chemical attack parameters: Low voltage arc current 'LVA = 200 A Arc discharge voltage: ULVA = 50 V
• Argon pressure PAR = 2.0 x 10"3 mbar Current of chemical attack ub = 12A Time of chemical attack t = 30 min Depth of chemical attack 200 nm
Coating: 10 Current for each IARC arc evaporator = 200 A • (8 evaporators with titanium lenses with a diameter of 150 mm) Arc discharge voltage UARC = 20 V Nitrogen pressure PN2 = 1.0 x 10"2 mbars Pressure of deviation UB, as = 100 V 15 Coating time t = 45 min Coating thickness of TiN 6 μm
• The process cycle time for a batch, including heating and cooling, is 150 minutes. 20 The voltage generation equipment for the negative acceleration voltage on the work piece is usually operated with voltages of up to 300 volts DC, but to protect the work pieces, the voltage is preferably kept within the range of 100 to 200 volts, to which 25 good attack speeds without defects are still reliable. The arch arrangement
a ^^^^^ MttMBaakfla * ^ Low-voltage MÉHlaiMih must be operated at least 10 cm away from the work piece, but the distance should preferably be > 15 cm, or preferably within the range of 15 to 25 cm at which
• achieve high speeds with good distribution. The coating system according to this invention is particularly suitable for processing tools such as drills, milling cutters and forming dies. The supports and the transport device are designed specifically for this type of tool. The coating arrangement of the present 10 is generally capable of achieving good results even if the pieces
• Work that will be coated is only spun around the central axis of the equipment. In particularly critical cases or if a very large number of small parts are to be loaded into the system, rotation around the central axis can easily be supplemented in this design concept by adding additional rotation axes, which in turn turn around of the central axis. • The invention is subsequently illustrated and schematically explained through the following figures. 20 Figure 1. A coating arrangement with low voltage discharge according to conventional technology. (State of the art). Figure 2. Cross section of a typical coating system according to the invention, with a peripheral discharge chamber 25 for low voltage discharge
.... ** -. ftn ttm? ihaki - ^ Figure 3. Horizontal section of the system illustrated in Figure 2. Figure 4a. Cross section of a part of the arrangement with the discharge chamber for the discharge of low flp voltage arc and multiple anodes disposed within the
camera. Figure 4b. Same as Figure 4a, but illustrated with cathode-anode discharge paths with the cathodes arranged in the separate cathode chambers. Figure 4c. Same as Figures 4a and 4b, also with trajectories of
separate cathode-anode discharge, but with the
• Cathodes arranged in a common cathode chamber. Figure 5. Service life comparison curves for tools coated with conventional technology and technology according to the present invention. Figure 1 illustrates a known workpiece cladding arrangement. A vacuum chamber serves as a process chamber 1 for adapting a low voltage arc discharge 18, the
• which runs in the center of the vacuum chamber 1 along this last central axis 16 and to which are attached with tabs sources of
Cathodic deposition of magnetron 14 at the periphery from the outside towards the chamber wall of the process chamber 1. On the upper part of the process chamber 1, there is a cathode chamber 2 supporting a thermionic hot cathode 3, the which can be supplied through the gas inlet 5 with the working gas,
typically a noble gas such as argon. Active gases can also be added for reactive processes. The cathode chamber 12 communicates with the process chamber 1 through a small hole in the obturator 4. The cathode chamber is usually isolated from the processing chamber through insulators 6.
shutter 4 is furthermore isolated from the cathode chamber through the insulator 6 so that the shutter 4 can be operated at a floating potential or auxiliary potential, as required. The anode 7 is arranged in the direction of the central axis 16 on the opposite side of the cathode chamber 2. The anode 7 can have the
form a crucible and keep the material that will be evaporated by the
• low voltage arc discharge. During the chemical attack process, this evaporation option is not used; only the ions are extracted from the low voltage arc discharge and accelerated towards the work pieces in such a way that you
The last 15 are attacked by cathodic deposition. To operate the low voltage arc discharge 18, the cathode 3 is heated with a heater supply unit, so that the cathode 3
• emits electrons. Between the cathode 3 and the anode 7 there is an additional power supply 8 for operating the arc discharge. Usually
produces a positive DC voltage on the anode 7 in order to support the low voltage arc 18. Between the arc discharge 18 and the chamber wall of the processing chamber 1, workpiece supports are supported which hold the work pieces 11, which can be rotated about their vertical central axis
17 in order to obtain an adequate uniformity of process. The
workpiece supports 10 are supported on an additional workpiece support arrangement 12, which is equipped with a rotary actuator through which these
• Workpiece supports 10 are rotated about the central axis 5. In this type of equipment, it is also necessary to focus the low-voltage arc discharge 18 through additional coils 13, for example in the form of coils of Helmholz It is evident that the work pieces 11 can be processed with the low voltage arc discharge 18, so that an ion bombardment occurs
when a negative voltage is applied to the substrate, and the bombardment
• Electronic is possible by applying a positive substrate voltage. In this way, the workpieces can be pretreated with the help of a low voltage arc discharge either through electron bombardment induced by heating, or through
ion bombardment with attack by cathodic deposition. Subsequently, the workpiece 11 can be coated, either through evaporation of the material from the crucible 7 by the low voltage arc, or through cathodic deposition with a cathodic magnetron deposition source 14, which is
supplied by the power supply 15. It is readily apparent that the mechanical assembly for the movement of substrate and the arrangement of the low voltage arc discharge are rather complex in this representation. On the one hand, the degree of freedom is severely restricted, since
work pieces can only be arranged between the discharge
low-voltage arc located in the center and the external chamber wall. A system of this type is not economical to operate for large work pieces or large quantities per batch.
• An example of a preferred coating arrangement according to the invention is illustrated as a cross section in Figure 2. The process chamber 1 contains a support part holder 11, which is arranged in such a way that the parts can be rotated around the central axis 16 of the process chamber. The camera is usually pumped by the
vacuum pumps 19 that maintain working pressures
• required for the steps of the process. In the proposed arrangement, a large workpiece 11, which extends beyond the central axis 16, can be, for example, arranged in the process chamber 1 such that this large workpiece 11 can
to be processed through the sources arranged on the wall of the process chamber. The area available to load the workpieces essentially fills process chamber 1 completely. In said arrangement, it is possible to place either a single large workpiece 11 or a large number of workpieces more
small ones, which essentially fill the volume of the camera. The workpiece holder that rotates the workpieces 11 about the central axis 16, expands the coating width b transversely to the direction of rotation. In the system according to the invention, it is particularly advantageous
that results in uniform and reproducible coating
either through the widths b of the large liner or through a large scale of depth extending from the central axis 16 towards the periphery of the width of the liner, that is, within the entire diameter D. Based on the concentric arrangement 5 known in accordance with conventional technology, where these conditions are critical, it was not expected that an eccentric arrangement according to the present invention could produce better results. A variety of workpiece geometries with thin edges and cutting edges can be handled in this large area without stress-related problems.
• thermal or unwanted occurrence of arcs. On the external wall of the process chamber, the chemical attack and the coating sources are placed in such a way that they act from the outside towards the work pieces. For the cathodic deposition chemical attack process 15 of important preparation, the chamber wall features a slot-like opening, the length of which corresponds at least to the processing width b. Behind this opening 26 there is a box-shaped discharge chamber 21, where the low-voltage arc discharge 18 is generated 18. This low-voltage arc discharge 18 runs essentially parallel to the processing width b and has an effective length, which must be at least 80% of the processing width b. Preferably, the discharge length must be equal to the processing width b or extend beyond it.
m ^ '_; : ^ - k .. i J »JMi» as.
The arc discharge shaft 18 has a distance d from the nearest processing zone, ie the next workpiece section. This distance d must be at least 10
• cm, preferably 15 to 25 cm. This results in a good process uniformity and a high rate of cathodic deposition can be maintained. At the bottom of the discharge chamber 21, the cathode chamber 2 is joined by flanges, on which it communicates with the discharge chamber 21 through the orifice 4. The cathode chamber 2 contains a hot cathode 3, the
which is supplied through the heating power supply unit 9. This supply can be operated with AC or DC. The cathode chamber 2 characterizes a gas inlet port 5 for supplying the working gas, normally a noble gas such as argon, or a noble gas, active gas mixture for certain processes
reagents. It is also possible to admit working gases through the process chamber 1 through the auxiliary gas inlet 22. The active gases are preferably admitted directly to the process chamber 1 through the gas inlet 22. In the upper part of the discharge chamber 21 there is a
electrode 7, which is designed as an anode. The DC supply 8 is connected between the cathode 3 and the anode 7, in such a way that the positive pole is on the anode 7 and a low voltage arc discharge can be extracted. The application of a negative voltage to the workpiece holder or to the workpieces 11
With the help of the voltage generator 20 between the low voltage arc discharge arrangement and the work piece 11, the argon ions are accelerated towards the work pieces, so that the surface is attacked by cathodic deposition. This can be achieved with accelerating voltages of up to 300 volts DC, but preferably with a voltage in the range of 100 volts to 200 volts to ensure moderate processing of the workpieces 11. The uniformity of the process can be set through the appropriate positioning of the cathode chamber 2, and arranging the anode 7 in relation to the processing width b of the work pieces that will be processed in accordance with the process specifications. Another factor is the shape of anode 7. The latter may have, for example, either a flat, dish or rectangular shape, or it may be designed as a tubular, cooled anode. Figure 3 shows a horizontal cross-section of the system based on Figure 2. Again the box-type discharge chamber 21 is shown on the external wall of the process chamber 1, which communicates with the treatment area through of the slot opening 26. Of course, several of these discharge chambers can be arranged on a system, as required, for example to further promote the processing effect. Also illustrated are the evaporation sources 23, which are flanged to the chamber wall. For example, magnetron sputtering sources can be used as evaporation sources 23, but to achieve high processing speeds at low costs, arc evaporation sources, so-called, are preferably used. The advantage of this arrangement is that the sources of arc evaporation 23 can be freely arranged from the outside in such a way that through the distributed arrangement of multiple sources, the homogeneity of the desired coating can be set and can be maintained high. coating speed. It has been shown that it is more advantageous not to use rectangular, individual evaporation sources, but if several smaller, round sources are arranged on the periphery of the system in accordance with the requirements of the
process. Figure 4a illustrates another advantageous variant of the arrangement according to the invention, wherein the cathode chamber 2 is located on top of the discharge chamber 21. The advantage is that the operation of the discharge path at
less is disturbed by particles that always occur in said coating system. It also shows the possibility of subdividing the discharge path using several circuits of
• anode-cathode and making the intensity along the discharge 1, adjustable. The main discharge is generated with the supply of
energy 8 between the main anode 7 and the cathode chamber 2. Additional auxiliary discharges can be generated with auxiliary anodes 24 and auxiliary power supply 25. In this way, it is possible to adjust the energy density of the discharge along the the entire discharge path between the anode 7 and the cathode 2
locally and with respect to the intensity of the homogeneity requirements of the work piece. Figure 4b shows an alternative arrangement. The anode-cathode trajectories can be kept completely apart, or even uncoupled using separate anodes 7, 24, 5, 3, 3 'separated cathodes, and separate 2, 2' cathode chambers. Another version is illustrated in Figure 4c, wherein 2 separate anodes 7, 24 are used, but a common cathode chamber 2 with 2 with two hot cathodes 3 and 3 '. Figure 5 illustrates the test results of rolling mills
finished HSS that were processed according to the invention
• (curve b) and conventional technology (curve a). In both cases, the mills were provided with a TiN coating of 3.5 μm. For the laminator according to conventional technology (curve a), a high-voltage chemical attack was first performed on the
Conventionally, while for the laminator represented by curve b, the process according to the invention was used. The test conditions were the following: •
HSS finishing mill: Diameter 16 mm 20 Number of teeth: 4
Test material: 42 CrMo4 (DIN 1.7224) Hardness: HRC 38.5
Feeding 15 mm x 2 5 mm Cutting speed 40 m / min. Feed per tooth 0.088 mm Feed 280 mm / min. • Term of life: Spindle torque 80 (arbitrary unit).
The result shows clear improvements in the life of the tool treated according to the invention. An improvement is easily achieved by a factor of 1.5 or more. It is important not only the expansion of the life of the tool, but also the
progression of flattening of the torque curve, which is indicative of the deterioration of the quality of the tool towards the end of the life of the tool. In the example according to Figure 5, this can clearly be recognized at a total rolling depth of 15 m. The curve a, which represents the
conventional technology shows sharp degradation in the quality of the tool at a total rolling depth of 15 m. This shows that the cutting quality that can be obtained with conventional technology has a greater variation throughout the life of the tool, which means that it is not very
consistent. The systems developed according to the invention, as illustrated in Figures 2 to 4, achieve even higher yields with the aforementioned high quality than system 1 conforming to conventional technology. Productions can be easily
duplicates or even increased by a factor of 3 to 5, which
dramatically increases the economy.
SUMMARY To deposit hard coatings on high performance tools that must be attacked by cathodic deposition prior to coating, the invention proposes to attack by cathode deposition tools with a low voltage arc discharge and subsequently coat them from the direction in which they have been applied. been attacked.
CLAIMS OF PATENT
1. - A coating arrangement for treating work pieces (11) with a vacuum process chamber (1) and a plasma source (18) disposed on the chamber, and with a coating source (23) disposed inside said chamber, and the chamber being equipped with a support and / or transport device, which defines a treatment area (b) for placing or passing the work pieces (11) in front of the sources, said sources being arranged at a certain distance towards the workpiece and acting from the same direction, characterized by a plasma source (18) designed as a hot cathode low voltage discharge arrangement, the linear degree (1) of which in a direction transverse to the direction The transport of the workpiece essentially corresponds to the width (b) of the processing zone, and contains a device for generating an electric field (20) between the arc discharge (18) and the workpiece (11).
• The arrangement according to claim 1, wherein the support and transport device for the workpieces (11) is arranged rotatably around the central axis (16) of the process chamber (1) and with the sources (18, 23) arranged on the chamber wall in such a way that they all act radially from the outside in the direction of the central axis (16). 3. The arrangement according to claim 1 or 2, in
• where the plasma source of a discharge chamber (21) is arranged on the external wall of the chamber (1), wherein in or on the discharge chamber (21) a thermionic emission cathode (3), and less 80% of the width of the processing area already
along the processing width (b), an anode (7) for generating a low voltage arc discharge (18) is placed and in said arrangement a noble gas port (5) in the discharge chamber (21). ) with a voltage generator (20) is arranged between the anode-cathode circuit and the workpiece (11) in such a way
that the negative pole is on the workpiece (11) so that the plasma source arrangement (2, 7, 18, 21) functions as a cathode deposition device. 4. The arrangement according to one of the preceding claims, wherein at least one additional anode (24)
extending along the plasma path at a distance from the plasma path, it is disposed between the emitting cathode (3) and the anode (7) to adjust the plasma density distribution throughout the discharge of the plasma. arch (18).
. The arrangement according to one of the preceding claims, wherein the anode (7) and the additional anode (24) are connected to separate, adjustable power supplies (25) and characterize an opposite cathode (3) preferably for each anode (7, 25) which together with the corresponding anode (7, 25) and the separate energy supply (8, 25) forms its own circuit
adjustable power. 6. The arrangement according to one of the preceding claims, wherein the emitting cathode (3) is arranged in a cathode chamber (2) separated from the discharge chamber (21) and the cathode chamber (2). ) communicating with the discharge chamber
(21) through the opening (4), through which the electrons emerge, with the noble gas inlet port (5) preferably disposed on this cathode chamber (2). 7. The arrangement according to one of the preceding claims, 2 to 6, wherein the process chamber (1) with its axis
The central one (16) is arranged vertically, and the cathode (3) or the cathode chamber (2) is disposed above the anode (7, 24), and the opening (4) of the cathode chamber (2) is preferably points down. 8 - The arrangement according to one of the claims
above, wherein at least one coating source
(23), which preferably consists of at least one arc evaporator (23), is disposed on the wall of the process chamber near the plasma source (18), which is located upstream in the transport direction . 9. The arrangement according to one of the preceding claims, wherein the voltage generator (20) is designed for voltages up to 300 V DC, preferably for 100 V to 200 V. 10.- The arrangement in accordance with one of the claims
above, wherein the low arc discharge arrangement
• voltage (18) is located at least 10 cm, but preferably 15 to 25 cm away from the workpiece (11). 11. The arrangement according to one of the preceding claims, wherein the support and transport device is
designed as a tool holder, particularly for drills, laminators and forming dies. 12. The arrangement according to one of the claims
• precedents, wherein at least one magnetic field generator is arranged in or on the discharge chamber (21)
to adjust the density distribution of the plasma. 13. The arrangement according to one of the preceding claims, wherein the discharge chamber (21) has an opening along the entire width (b) of the processing area, and the opening facing the latter, so that the
processing zone is exposed to the arc discharge.
14. - A process for at least partially coating work pieces (11) in a vacuum process chamber (1) with a plasma source (18) disposed on the process chamber and ^ a coating source (23) and with a support device and / or
transport arranged in the chamber (1), said device determining a treatment area (b) to place or pass the workpieces (11) in front of the sources (18, 23), where the sources act from the same side and are disposed at a certain distance from the workpiece (11), in said process, the source of
Plasma (18) generates a hot cathode low voltage arc (18) in a direction transverse to the transport direction of the workpiece essentially at least through 80% of the width (b) of the zone of treatment, in said process, a voltage is applied between the arc discharge and the work piece to extract
charge carriers of the plasma, so that they can be accelerated towards the substrate. 15. The process according to claim 14, wherein the work pieces preferably rotate continuously around the central axis (16) of a processing chamber and pass
in front of the sources (18, 23), and in said process, the plasma treatment occurs through the bombardment of load carrier in a first step and the coating of the workpiece (11) in a second step. 16. The process according to claim 14 or 15, in
where charge carriers consist of ions that are extracted
of the arc discharge (18) directly with the help of a negative workpiece voltage, in such a way that they can attack the workpiece (11) by cathodic deposition. 17. The process according to one of claims 14 to 16, wherein the homogeneity of the chemical attack distribution through the coating zone (b) can be set to predetermined values by selecting the arc length, the distance (d) between the arc and the work piece, the position of the arc in relation to the work piece, as well as adjusting the density distribution
plasma along the arch. •
Figure 5 Spindle torque [a.u] End of tool life 15 High voltage chemical attack + 3.5 μm TiN (arc coating) High voltage arc coating + 3.5 μm TiN (coating
• of arc), (Invention) 20 Depth of total rolling [m]
**** - *.! * MÜadMtftMIiSlh ^ Ariii
Claims (17)
1. - A tool with a tool body and a resistant layer system, said resistant layer system comprising at least one layer of MeX, wherein: I comprise titanium or aluminum, X is at least one of nitrogen and carbon, and wherein said layer has a Q ?, defined as the ratio of the diffraction intensities 1 (200) to 1 (111), assigned respectively to the planes (200) and (111) in the X-ray diffraction of a material , using the method of? -20, thus measuring the intensity values with the following equipment and with the following parameters: Siemens D500 diffractometer Power: Operating voltage: 30 kV Operating current: 25 mA Opening diaphragms: Diaphragm position I : 1st Diaphragm position II: 0.1 ° Detector diaphragm: Soller groove Time constant: 4 s Angular speed 29: 0.05 ° / min. Radiation: Cu-Ka (0.15406 nm) where Q? has a value of: Q < 2 and said tool is one of. - a solid carbide terminal laminate; a solid carbide ball nose laminate; a tool for carving cemented carbide gears, so the value of 1 (111) is at least 20 times the value of the average noise intensity.
2. The tool according to claim 1, wherein it is valid for Q | -. Q? < _ 1, preferably, Q? £ 0.5, so preferably: Q? < .0.2, especially preferred: Q, < 0.1.
3. The tool according to one of claims 1 or 2, wherein said MeX material is one of titanium-aluminum nitride, titanium-aluminum carbonitride, titanium-aluminum boronitride, thus preferably one of titanium-aluminum nitride. titanium-aluminum and titanium-aluminum carbonitride.
4. The tool according to one of claims 1 to 3, wherein Me further comprises at least one additional element outside the group consisting of boron, zirconium, hafnium, yttrium, silicon, tungsten, chromium, preferably of this at least one of trio and silicon and boron.
5. The tool according to claim 4, wherein said additional element is contained in Me with a content of 0.05 to% < i < 60 to%, taking the content of Ti as 100%.
6. - The tool according to one of claims 1 to 5, further comprising an additional layer of titanium nitride between at least said layer and said tool body, and wherein the additional layer has a thickness d, for the • 5 which is valid 0.05 μm < d < _ 5.0 μm.
7. The tool according to claim 6, wherein the layer system is formed through at least one layer and the additional layer. 10 8.- The tool according to one of the • claims 1 to 7, wherein the voltage within at least one layer, s, is 2 GPa < s ^ 8 GPa, preferably thus 4 GPa < s < 6 Gpa. 9. The tool according to one of claims 1 to 8, wherein the x content of titanium in Me is: • 70 to% > x > 40 to%, preferably 65 to% > x > 55 to%. 10. The tool according to one of claims 1 to 9, wherein the content of y of aluminum in Me is from: 30 to% < and < 60 to%, most preferably 35 to% < and < 45 a% 25 11.- A method to produce a tool that comprises a tool body and a wear-resistant layer system, which comprises at least one layer of hard material comprising the steps of: fl-depositing reactive PVD of at least one layer of MeX on said body, wherein I understand titanium and aluminum, X is at least one of nitrogen and carbon; selecting the predetermined parameter values for said deposition of PVD in addition to at least one of the two parameters consisting of partial pressure of a reactive gas in said vacuum chamber and deviation voltage of the body of • tool with respect to a predetermined reference potential; adjust at least one of the partial pressure and the deviation voltage so that said layer obtains the Q? desired, which can assume a value greater than or less than unity, and to obtain a value of at least one of 1 (200) and 1 (111) of at least 20 times greater than the value of the intensity of the average noise, • exploiting thus, that said Q |, as a function of the partial pressure and the deviation voltage, is reduced with the reduction of the partial pressure 20 as well as with the increase of the deviation voltage, Q, being defined as the ratio of the diffraction intensities 1 (200) to 1 (111), assigned respectively to the planes (200) and (111) in the X-ray diffraction of a material using the method of? -20, the intensity values being measured with The following equipment and with 25 the following parameters: ? ".%» * & ,, - ..?. Jjen, i t - ,. .-. > - .. .. . *. to"***!**. . .-.,. ,, * t., ^ X- *? * Ír. ^ ¡** HltM ** ßiMi ** Siemens D500 diffractometer Power: Operating voltage: 30 kV Operating current: 25 mA Opening diaphragms: Diaphragm position I: 1st Diaphragm position II: 0.1 ° Detector diaphragm: Soller slot Time constant: 4 s Angular speed 2 ?: 0.05 ° / min. Radiation: Cu-Ka (0.15406 nm). 12. The method according to one of claims 10 • u 11, which further comprises the step of performing the deposition of reactive PVD through reactive cathodic arc evaporation. 13. The method according to claim 12, further comprising the step of magnetically controlling said arc evaporation. 14. The method according to claim 11 to 13, further comprising the step of depositing on the body of • tool, a layer of MeX, where I understand titanium and aluminum and X is at least one of nitrogen and carbon and 20 introduces PVD by depositing through reactive gas. 15. The method according to one of claims 11 to 14, wherein the tool body is one of the materials: a solid carbide terminal laminate; a solid carbide ball nose laminate; 25 - a tool for carving cemented carbide gears, thus selecting the value of Q | to be: adjusting at least one of the reactive pressure and the voltage of • Deviation for said deposition of reactive PVD. 16. The method according to claim 15, thus selecting the value of Qt to be Q? > 1 preferably to be Q? > 5 or even to make it Q? < _0.2. 17. The method according to claim 16, thus selecting the value of Q | to make it 10 Q, > 0.1. • • • * ~ m **. ? * m & * ^ -. a. »-. . *. . < * - *. * * .. * .--. . ¿M ... --A .-. .. .. *. mt? .x ?. . ? -Oi,
Publications (1)
Publication Number | Publication Date |
---|---|
MXPA00002589A true MXPA00002589A (en) | 2002-07-25 |
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