EP1740737A1 - Procede de revetement d'un corps de base, dispositif destine a la mise en oeuvre de ce procede et corps de base revetu - Google Patents

Procede de revetement d'un corps de base, dispositif destine a la mise en oeuvre de ce procede et corps de base revetu

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Publication number
EP1740737A1
EP1740737A1 EP05729356A EP05729356A EP1740737A1 EP 1740737 A1 EP1740737 A1 EP 1740737A1 EP 05729356 A EP05729356 A EP 05729356A EP 05729356 A EP05729356 A EP 05729356A EP 1740737 A1 EP1740737 A1 EP 1740737A1
Authority
EP
European Patent Office
Prior art keywords
base body
layer
heating
temperature
pulsed
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP05729356A
Other languages
German (de)
English (en)
Inventor
Erich Bergmann
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
BESTCOATING Sarl
Original Assignee
BESTCOATING Sarl
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by BESTCOATING Sarl filed Critical BESTCOATING Sarl
Publication of EP1740737A1 publication Critical patent/EP1740737A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/54—Controlling or regulating the coating process
    • C23C14/541—Heating or cooling of the substrates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/46—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for heating the substrate
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
    • H01J37/32321—Discharge generated by other radiation
    • H01J37/3233—Discharge generated by other radiation using charged particles

Definitions

  • the invention relates to a method for depositing a layer on a base body, in which the structure of the layer corresponds to a substantially higher production temperature than the temperature that the material of the base body is allowed to reach, and in particular to a method in which parts of the growing layer tempered at high temperatures for limited periods of time.
  • the invention also relates to a device for the deposition of layers from a plasma, for the plasma-assisted deposition of a layer on a base body, in which the structure of the layer corresponds to a substantially higher production temperature than the temperature that the material of the base body may reach, and in particular a method in which parts of the growing layer are left on at high temperatures for limited periods of time, which makes it possible to start parts of the growing layer on certain periods of time.
  • the invention also relates to a coated base body with a layer material, the structure of which is also determined by tempering the growing layer during certain periods of time, which is produced according to the method of the invention.
  • Pulsed heaters are unknown in the prior art.
  • deposition of layers from the vapor phase in particular in the deposition of
  • Layers with physical vapor deposition correspond to the structure of the layer always a low temperature phase of the deposited layer material.
  • the layers are more often amorphous.
  • Multi-phase materials which can also be referred to as microcomposites or nanocomposites, have highly interesting properties for numerous wear protection applications, in particular their toughness is considerably improved compared to single-phase materials. Indeed, the use of nanocomposites would be of great advantage in most wear problems. So far, however, it has been limited to layer systems whose components have a very low melting point, such as Al-Sn, or whose components cannot be mixed for crystallographic reasons, such as TiCrN.
  • the temperatures necessary for the formation of multi-phase structures and high-temperature modifications can only be achieved in exceptional cases by heating the base body.
  • the base bodies are made of materials that lose their technical properties if they become too hot: aluminum alloys, steels, glasses, etc.
  • pulsed heating in which the power used over time is so low that excessive heating of the base body is avoided.
  • a special version of the pulsed heating is possible with plasma coating processes.
  • An embodiment of the heater for plasma coating processes according to the invention works with the pulsed bombardment of the coating base body with low-energy electrons from the plasma. It differs from the state of the art of heating with low-energy electrons (R. Schmid, H. Kaufmann DE 3614398 A1) in the pulse mode and from the state of the art of coating with bipolar pulsed base body bias (F. Fietzke, K. Goedicke, S. Schiller WO 00/39355) by a different range of the engagement ratio and by a different range of the frequency.
  • the method according to the invention is characterized in that the growing layer is heated in a pulsed manner.
  • the device according to the invention is characterized in that it has heating means which enable pulsed heating of the growing layer.
  • the coated base body according to the invention is characterized in that the structure of the layer material corresponds to a deposition temperature which is substantially above the temperature at which the material of the base body changes its technical properties.
  • a pulsed heater in the sense of the invention is a heater that is only in operation during the deposition and that also works very much during the deposition is switched off more often than switched on.
  • a pulsed heater in the sense of the invention is a heater with a sequence of periods of being switched on, in which a surface-specific power P (W / m 2 ) is applied to the surface of the base body to be coated, and periods of being switched off t aU s > in which no heat is applied to the base body.
  • the invention relates to an additional heater and does not exclude or exclude the presence of other process-related heat sources such as the radiation from a melt or a continuous ion bombardment during the deposition.
  • the area-specific power applied on average over time is so low that excessive heating of the base body is avoided.
  • the meaning of this criterion characterizing the invention is application-specific, but is clear to the person skilled in the art. Examples of excessive heating are reaching the tempering temperature for steel materials, reaching the temperatures at which a stainless steel loses its corrosion resistance, at which deformation occurs in the case of glasses and polymers, etc.
  • the term thermal budget is used used.
  • the heater according to the invention can be defined as a heater that takes up less than 10% of the thermal budget of the coating process.
  • a composite material is a substance in which at least two different substances or two different phases of the same substance are present that are spatially separated. Originally, the term was limited to materials in which the two materials were present and recognizable as macroscopic components: laminates, polymers with fillers or metals with insoluble additives. In the past 20 years, the term has been extended to finer mixtures and - depending on the size of the particles of the individual substances or phases, one speaks of macro-composites, micro-composites and nanocomposites.
  • a typical example of a micro-composite is gray cast iron, which is made of low-carbon ferrite and graphite. It can be generated by very slow cooling or tempering at high temperatures.
  • amorphous and nanocrystalline materials are determined by the extent of the local order on the atomic scale. This limit is not easy to determine and is often determined by the analysis method used - for example, X-ray amorphous.
  • the materials we refer to the materials as amorphous, in which the spatial expansion of the local crystalline order of the atoms does not reach the size of five unit cells.
  • a nanocomposite material is therefore a material in which a spatial separation of different substances or phases from the expansion of at least five unit cells of one of the two substances or one of the two phases can be observed.
  • Examples of this are: materials that consist of a single or multi-phase crystalline or amorphous matrix and fragments - in English clusters - of hard materials or lubricants, the size of which does not reach 1 micrometer, materials in which two or more phases of the same are spatially separated Substance occur and so on. Numerous further examples are known to the person skilled in the art from the literature.
  • a special form of composite materials are laminates, in the case of coating multi-layer sequences in which layers with different chemical compositions and / or different phase compositions and / or different structures alternate.
  • the multi-layer sequences according to the invention include multi-layer sequences in which layers with structures that correspond to different production temperatures follow one another.
  • phase diagrams commonly used in materials science. These have been created for all binary as well as most ternary and quaternary substance systems and are generally accessible. There are also interpolation and calculation models that it allow to calculate phase diagrams that have not yet been created. For a given chemical composition, one generally observes different equilibrium structures that are stable in different temperature ranges, separated by limit temperatures. If the temperature falls below or falls below the limit temperature, a phase transition is observed, the kinetics of which depend on the mobility of the atoms forming the material. The time required to reach the new equilibrium structure is phase transition-specific and shortens when the difference between the actual temperature and the limit temperature increases.
  • Coating temperature that is, in the case of the methods according to the prior art, the temperature of the base body.
  • the atoms are applied to the surface in an arbitrary order and arrangement. Diffusion on the surface and in the growth phase of the layer then results in the finest crystalline structures with sufficient energy of the applied atoms, which generally correspond to the simplest lattice structures of the material. If the energy is insufficient, amorphous layers form. The formation of single-phase, finely crystalline layers becomes possible if the mobility of the applied atoms after the condensation is sufficient to cover a distance that corresponds to a fraction of the lattice constant, i.e. less than 0.3 nanometer (nm).
  • the mobility of an atom depends on the energy brought from the plasma, the average energy of the atoms that have already condensed, and the time it has before it is covered by the subsequent atoms. It is generally assumed that the mean energy of the condensed atom at this time is determined in a known manner by the body temperature. The events up to this point are called nucleation and are in the literature below this Keyword described.
  • the person skilled in the art changes the energy brought from the plasma with the basic body pretension (see F. Fietzke, K. Goedicke, S. Schiller WO 00/39355) and the gas pressure, the average energy of the already condensed atoms by the basic body temperature (see case (see E Bergmann, Gl van der Kolk, B. Buil, T.
  • the temperature of the growing layer corresponds to the temperature of the base body.
  • the laminate In order to produce a nanocomposite from a deposited single-phase laminate, the laminate must therefore be brought to a high temperature for a certain period of time.
  • the advantages of thermal aftertreatment are known and have numerous applications.
  • the entire coated body is always heated.
  • most of the technical moldings to be coated are made of materials that lose their mechanical properties at high temperatures, which were previously given to you by precise heat treatment.
  • the heating and cooling of large masses is associated with considerable costs and time.
  • the invention solves this problem by pulsed heating of the surface.
  • the skilled artisan can the parameters for its use of the inventive method by using the principles illustrated in e t. T a us, P readily determine.
  • T e the structure of which should correspond to a temperature T e
  • the depth of penetration is negligible. Then it makes sense to another characteristic of the process time t e i n + t to choose from, for example, the duration of the complete rotation of the body receiving device 14 or the time the main body in the coating process needs to get from one layer material source 3 to the other layer material source 4.
  • a special but not exclusive embodiment of the method according to the invention is the use of low-energy electrons, such as those which strike the anodes in low-energy plasmas, for heating the growing layer and as described in (R. Schmid, H. Kaufmann DE 3614398 A1) ,
  • This pulsed low-energy electron heating of growing layers according to the invention can in principle be set up in all low-energy plasma discharges, that is to say both corona discharges and also glow discharges or arcing discharges.
  • the base bodies are briefly switched to a potential V + while t e m is positive with respect to the plasma potential.
  • the workpieces take over the electrical function of the anode and are bombarded with an electron current, the value of which corresponds to the plasma discharge current I.
  • This power pulse causes a temperature pulse, which decays as it spreads into the growing layer.
  • the pulse width and height are chosen such that the edge zone of the layer that has grown between 2 pulses reaches the temperature T e required for the solid-state reaction.
  • FIG. 1 schematically shows a desired basic body intake preload and round body intake current profile for the application of the method according to the invention
  • FIG. 2 shows an example of a system in which the method can be carried out
  • FIG. 3 schematically shows a target base body pre-stressing and base body intake current profile for the application of the method according to the invention for the production of intermediate layers
  • FIG. 4 shows the structure of a multi-layer sequence coating according to the invention.
  • the use of carbide end mills is not possible because, compared to high-speed steel end mills, they either have a too blunt cutting edge or break the teeth when they enter the material due to excessive elastic deformation.
  • High-speed steels can only be tempered at temperatures below 540 ° C and lose their resistance to plastic deformation if they are heated above this temperature.
  • the coating method of the prior art was expanded to include a pulsed heater according to the invention as follows.
  • the prior art for carbide tool coating is vapor deposition with the aid of cathodic arc evaporation, in which the tools are heated to the coating temperature of 650 ° C.
  • the tools were heated to 450 ° C with the radiant heater and subjected to the same coating process, only this time an additional pulsed heater was used during the coating process.
  • This consisted of moving the workpiece surfaces from the negative bias of - 110Volt to a positive bias of + 10V (opposite the chamber wall) every 9 seconds by reversing the polarity of the base body carrier bias power supply (see Figure 1).
  • This positive bias was accompanied by a current of approximately 200 amps.
  • the potential of the body support carrier bias power supply was reversed and set to - 110 volts. This process was repeated throughout the entire coating process (see Figure 1).
  • Example 1 the method described in Example 1 was modified in order to reduce the formation of comb cracks which occur in the hard metal tools coated according to the prior art at 650 ° C.
  • the carbide tools were only heated to 450 ° C and then coated with a pulsed heater.
  • the pulsed heating was switched on and off periodically, namely after every 36 minutes.
  • the exact course of the tool holder preload is shown in Figure 3.
  • a structural analysis of the cross section of the layer showed a sequence of 7 layers. It is shown schematically in Figure 4.
  • An approximately 0.45 ⁇ m thick nanocomposite base layer 44 had grown on the base body surface 42.
  • the basic bodies of the connecting rod bearings of modern internal combustion engines consist of hot strip on which a 0.1 - 1 mm thick layer of bronze is cast or sintered.
  • this base body is coated with a 10 to 15 ⁇ m thick aluminum / tin bronze, which is deposited using sputtering.
  • the systems used for this consist of, for example polygonal cylinders, on the side walls of which up to 8 magnetron vapor sources with aluminum / tin bronze target plates are attached.
  • the aluminum / tin bronze layers are micro- or nanocomposites in which the finest tin crystals are deposited in an aluminum / tin matrix. The size of the tin deposits and the microhardness of the layer depend on the workpiece temperature during coating.
  • Layers that are deposited below 30 ° C are nanocomposites and have hardnesses of up to 150 HV, while the layers deposited in the range of 80 ° C - 90 ° C are submicro-composite materials and have hardnesses in the range of 70 - 90 HV.
  • An electrical pre-tensioning of the base body mounts is not used with this coating. Reference measurements have shown that in the coating process according to the prior art, the workpieces assume a potential of - 12 volts relative to the chamber wall. - 12 volts is the plasma potential when operating this system.
  • cooled base body receptacles are used, while for the deposition of microcomposites, a non-stationary temperature can be accepted, which results from the use of a 300kg aluminum cooling block for the workpiece receptacles.
  • the poured bronzes must not be heated above 210 C.
  • the coating time in the prior art is 120 minutes. Reference measurements have shown that during this time the temperature rises almost linearly from 20C to 150C. Details of the prior art are described by E. Bergmann, H. Pfestorf, J. Braus in DE 3629451 A1.
  • the aluminum / tin bronze is not suitable for engines with higher loads because it cannot withstand the loads that occur at high injection pressures.
  • Nano and micro composites based on tungsten / tin bronze would be suitable in this area.
  • a comparison of the phase diagrams of the Al / Sn system and the W / Sn system shows that nanocomposites of tungsten and tin do not form below 630 ° C. Such a high coating temperature is not conducive to the basic body.
  • the method according to the invention with pulsed heating of the growing layer but allows coating with nano and even micro-composite layers.
  • the workpiece holder surface exposed to the coating is negligible compared to the workpiece surface to be coated.
  • the system can accommodate 2000 connecting rod half-shells (inner diameter 76 mm, height 27 mm).
  • the speed of the base body holder (single rotation) can be regulated in the range of 0.1 - 20 revolutions / minutes.
  • the aim of the process was the deposition of a tungsten / tin bronze with 40 vol% tin content with a temperature of the growing layer of 630 ° C.
  • the procedure according to the invention was as follows. Calculation of the constants of the layer material:
  • the parameters of the rotation of the workpiece holding device were therefore chosen as 3.5 revolutions / minute, so that for each steam source at each Revolution of 3 nm.
  • the on time of the pulsed heating was set at 0.15 sec and the off time at 2.01 seconds. With these parameters it was possible to deposit the tungsten / tin bronze as a nanocomposite.
  • Piston rings for modern internal combustion engines consist of a base body made of martensitic stainless steel and a chromium nitride layer of 10 - 70 ⁇ m applied by physical vapor deposition.
  • the friction of these piston rings against the cylinder wall is too great, which leads to severe losses in engine performance.
  • about 30% of the power generated by the combustion is lost again due to this friction of the piston ring against the cylinder wall and is therefore not available for the drive. From the perspective of materials science, a nanocomposite would be very finely distributed in the chromium nitride
  • Solid lubricant particles a good solution.
  • Micro-composite materials such as gray cast iron were once state of the art.
  • the base body made of martensitic stainless steel must not be heated above 350 ° C during the coating, otherwise it will be
  • Working piston rings in the limit friction area is a solid lubricant
  • Chromium / molybdenum disulfide composite targets in layers deposited in nitrogen / argon plasma are an amorphous mixture of
  • Composition CrMoSN A stationary base body temperature of 280 ° C was established during the deposition. From the thermodynamic
  • the processes for the deposition of titanium nitride from TiCl 4 and nitrogen using the plasma-assisted CVD (PACVD) process are known.
  • a bipolar pulsed power supply is used, which surrounds the workpieces to be coated with a plasma seam. The process takes place at about 400 Pa in a vacuum oven. If these layers are deposited on hardened steel as usual, you have to choose a coating temperature below 550 ° C, usually 530 ° C.
  • the layers deposited in this way have a chlorine content of 2-5% from the reaction product. This chlorine content corresponds to the thermodynamic equilibrium of the chemical reaction which leads to the deposition of the layer. He limits the application of the coating with this process to components that are not exposed to moisture.
  • Brass parts for example sanitary facility components, are state of the art. Up to 2 m long rectangular cathode evaporators with metallic zircon cathodes are used for this.
  • the coating is usually carried out with 90 amperes / evaporator in a nitrogen atmosphere at a pressure of 1.2 Pa. Most systems have 4 evaporators.
  • the galvanic chrome underlayer is required because the corrosion protection that the vapor-deposited zirconium nitride layer offers to the base body is insufficient.
  • the structure of the layer is stalky and the crystals forming it are preferably aligned with the (111) plane parallel to the layer surface. Due to the low vapor pressure, the zinc contained in the brass, the temperature of the base body during the coating must not exceed 200 ° C.
  • the systems also contain cooling screens in order to intensify the cooling of the body by radiation.
  • the coating runs at a steady temperature of 180 ° C. During the procedure there is a negative bias of - 70 volts on the base body holder. The layer thickness is about 1 ⁇ m and the coating takes 90 minutes. This coating could be significantly improved by a pulsed heater according to the invention.
  • Fig. 1 shows schematically a typical course of the basic body prestressing as a function of time.
  • the workpiece surfaces are brought from a negative bias of - 110Volt to a positive bias of + 10V (opposite the chamber wall) by reversing the polarity of the workpiece holder carrier bias power supply (see Figure 2).
  • This positive bias is accompanied by a current of approximately 200 amps.
  • the bias of the workpiece holder carrier bias power supply is reversed again and set to - 110 volts. This process is repeated throughout the entire coating process.
  • An independent measurement with a Langmuir probe showed that under the conditions of the coating the plasma potential was - 5V compared to the earthed chamber wall.
  • the workpiece temperature was also measured during the coating process. It was 460 ° C with a usual measurement inaccuracy of +/- 10 ° C.
  • the described pulsed heating of the growing layer only caused an insignificant, hardly measurable heating of the workpieces.
  • FIG. 2 schematically shows an apparatus for carrying out the method according to the invention.
  • Certain designs were selected for the assemblies that correspond to the state of the art, such as vacuum chamber, evaporator and workpiece holder. It is clear to the person skilled in the art that the assembly examples can be replaced by others.
  • a plurality of evaporators 3, 4 are attached to a vacuum chamber 1, the shape of which is not essential and which is designed as a cylinder in this example and which is connected with a nozzle 2 to a vacuum pumping station (not shown). Depending on the application, this can be one or more evaporators of the same or different types. Details of the construction and operation of systems with different evaporators are described in US 4,877,505 issued to E. Bergmann.
  • cathodic arc evaporators there are two magnetic field-assisted cathode sputtering sources 3 and two cathodic arc evaporators 4.
  • the drawing shows only one evaporator of each type. Details of the structure of sputtering sources 3 are given in US Pat. No. 6,620,269 to S. Schiller et al. and the publications cited therein. Details of the construction of cathodic arc evaporators are described, for example, in US 4,622,452 issued to Clark Bergmann.
  • the device naturally also contains cooling and heating devices according to the prior art, as well as devices for measuring and regulating the gas pressure and device for regulating various gas flows into the system. The structure of such devices is known and is therefore not shown.
  • the cathode sputtering sources 3 are electrically insulated from the vacuum chamber 1, for example by an intermediate flange 5 made of a suitable insulation material such as glass fiber-filled Teflon or polyethylene ether ketone.
  • the cathode sputtering sources are provided on the vacuum side with a target plate 6 made of the material to be sputtered. In this Example, their surface area was 300 cm 2 .
  • the target plate was made of molybdenum disulfide. This is electrically connected to the negative pole 8 of a direct current source 7.
  • the direct current source 7 it is also possible to use a unipolar pulsed source, a radio frequency source or a microwave source, probably also a pulsed bipolar current source, as are known in the prior art and are described, for example, in US Pat. No. 6,620,269 as prior art. It is crucial when using sources other than direct current that their frequency is significantly higher than the frequency of the repetition of the heating pulses t e in + t off .
  • the positive pole 9 of the direct current source 7 is connected to the vacuum chamber 1 in the example.
  • Other electrical arrangements for the cathode sputtering source such as the use of an independent anode or the use of another cathode sputtering source as the anode, are also known and are fundamentally compatible with the method.
  • the direct current sources delivered a current of 3 amperes.
  • the arc evaporators 4 are electrically insulated from the vacuum chamber 1, for example by an intermediate flange 5 made of a suitable insulation material such as glass fiber-filled Teflon or polyethylene ether ketone.
  • the arc evaporators are provided on the vacuum side with a target plate 10 made of the material to be evaporated, chromium in the present example.
  • the surfaces of the two target plates were each 240 cm 2 .
  • the surface is electrically connected to the negative pole 11 of a direct current source 12. This is typically a direct current source of the kind used for electric welding and which is commercially available.
  • the positive pole 13 of the direct current source is connected to the vacuum chamber 1 in the example.
  • Devices are also known from the literature in which the positive pole 13 is connected to an anode. Such devices can also be used in the device according to the invention.
  • the two evaporators 3 and 4 can be operated simultaneously and in succession. Of course other evaporators such as laser evaporators or electron beam evaporators can also be used in the device according to the invention.
  • the base body 15 is attached to it with clamping angles 21 and screws 22 or clamped in sleeves 23 in the case of shaft-shaped base bodies.
  • the connection between the base body and the base body receptacle is not only electrically conductive as in the prior art. It was found that the flawless and reliable implementation of the method according to the invention requires special basic body receiving devices which are part of the device according to the invention.
  • the basic body receiving device according to the invention has a low electrical resistance between the axis of rotation 16 and the workpieces to be coated. So not only wires or positioning clamps are used as the clamping body 21 as in the prior art.
  • the base bodies are either screwed to the base body receptacle with screws of a large diameter, such as at least M6, preferably at least M10, or copper parts are used for the fastening.
  • the sleeves are equipped with clamping devices, for example contact springs made of copper or copper alloys, as are unknown in the prior art.
  • Such low-resistance clamping devices are part of the device according to the invention.
  • the conductivity of the table top 24 is also important. In the case of table tops made of stainless steel, as are usually used, it has proven useful to use strips 25 of a material with high electrical conductivity, such as copper, in the table top.
  • bands braided from copper wire can also be used to conduct the current from the axis of rotation 16 to the workpiece carrier axes 26. Tests have shown that the effectiveness of these measures can be checked as follows: The device is similar with the base bodies to be coated Load dummy bodies. With these dummy bodies, a coating process is initiated in which the evaporators are operated at the power provided in the coating process while the
  • Base body receiving device is connected to the coating chamber via an ammeter.
  • the current read from this ammeter is compared to the sum of all evaporator currents. It has been shown that a basic body receiving device is suitable for carrying out the method according to the invention if the current read on the ammeter is at least 80% of the total of all evaporator currents. A basic body receiving device that fulfills this condition is part of the device according to the invention. If the current read is less than 80% of the sum of all evaporator currents, the person skilled in the art should take several or more of the measures described above for reducing the electrical resistance between the axis of rotation 16 and the base bodies 15. During the coating process, the base body receptacle rotates about a central axis 16.
  • This rotary movement 17 can be brought about, for example, by a motor attached to the axis outside the vacuum chamber.
  • Asynchronous motors with adjustable speed are usually used.
  • the engine is not shown in the picture.
  • Eccentric drives and support on bearing rollers are also possible, known to the person skilled in the art and compatible with the device according to the invention.
  • a central axis 16 is used, which also serves as a carrier.
  • This is provided with an insulated vacuum rotary feedthrough 18 which electrically insulates the axis and the base body receptacle from the vacuum chamber wall.
  • An electrical line 19 is attached to the axis 16 outside the chamber. This is connected to the axle with a slip ring 20.
  • This slip ring is a high-current construction with which up to 500 amperes of current can be transmitted. Instructions for the design of such slip rings can be found in the textbooks for electrical engineering. State-of-the-art slip rings are used for systems of this type Size designed for less than 50 amps. Such a slip ring caught fire the first time it was used.
  • the base body receptacle of the device according to the invention must have a high electrical conductivity right down to the base bodies.
  • the electrical resistance of the bushing between the slip ring and the table was less than 1 m ⁇ .
  • Rotary axes 16 with higher resistance showed a strong warming.
  • the axis of rotation of the example of the system according to the invention was made of non-magnetic stainless steel.
  • the low resistance of the example of the system according to the invention was achieved by a special high diameter.
  • a slimmer axis of rotation 16 made of a material with higher electrical conductivity such as copper or silver would also be a suitable solution.
  • Another solution could be that the device is equipped with a high current feedthrough and the slip ring on the axis of rotation 16 is replaced by a transfer brush or transfer lamella on the underside of the base body.
  • a uniform coating of all base bodies according to the invention can only be achieved if the electrical resistance between slip ring 20 and all base bodies is not less than 50 m ⁇ . If the electrical resistance between the slip ring 20 and all base bodies is not greater than 50 m ⁇ , there are differences in the layer structure between the different base bodies. If the electrical resistance between the slip ring 20 and all base bodies is less than 50 m ⁇ , deviations from the coating achieved by the method according to the invention occur only in individual cases.
  • the arrangement consists of a power supply 26, which is able to deliver both the high base body biases and the high current pulses. It is connected to the switching device 27 via two cables 28, 41, at the ends of which sliding contacts 29 and 35 are attached.
  • the switching device 27 essentially consists of a cylindrical body 30 made of a suitable insulation material, in which 4 silver-plated copper rods 31, 32, 33, 34 are installed. The ends of the rods are also provided with sliding contacts 36.
  • the cylindrical body 30 carries on one end face an axis 37 to which a stepping motor (not shown) is coupled. This stepper motor is switched on in periods of alternating t out and t e m and causes a% rotation of the cylindrical body each time.
  • the negative pole of the basic body bias supply 26 is connected to the slide ring 20 via the cable 19, while the positive pole of the basic body bias supply 26 is connected to the vacuum chamber wall by the cable 40.
  • the positive pole of the basic body bias supply 26 is connected to the slide ring 20 via the cable 19, while the negative pole of the basic body bias supply 26 is connected to the vacuum chamber wall by the cable 40.
  • Base body bias supply 26 with switchover device 27 could also be used 2 base body bias supplies with switchers. It has furthermore been shown that the construction of the switching device 27 can be considerably simplified if the base body bias supply is switched off during the rotational movement of the axis 37. This has no effect on the course of the process if the rotation is fast enough and the rotation time is added to the period. This embodiment is of course only one example of how a pulsed substrate heating according to the invention can be implemented.
  • FIG. 3 shows the time profile of the base body pre-stress and the base body current in a method according to the invention in which the pulsed heating is periodically suspended.
  • the workpiece surfaces are brought from a negative bias of - 110Volt to a positive bias of + 10V (opposite the chamber wall) by reversing the polarity of the workpiece holder carrier bias power supply. (see drawing 2).
  • This positive bias is accompanied by a current of approximately 200 amps.
  • the bias of the workpiece holder carrier bias power supply is reversed again and set to - 110 volts. This process is repeated continuously for 36 minutes. Thereafter, the base body holder bias is left at - 110 volts for 36 minutes. The pulsed heating is then switched on again for 36 minutes. This process is repeated twice - not shown in the drawing.
  • Example 4 shows the result of the coating method according to the invention described in Example 2.
  • An approximately 0.45 ⁇ m nanocrystalline two-phase isotropic AlTiN layer 44 of a nanocomposite material is located on the tool surface 42.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

L'invention concerne un procédé de dépôt d'une couche sur un corps de base, au cours duquel la fabrication de la couche nécessite une température de fabrication nettement supérieure à la température maximale supportée sans dégâts par le matériau du corps de base. Ces températures élevées de la couche en cours de croissance peuvent être atteintes par bombardement pulsé d'électrons basse énergie lors de procédés de revêtement plasma. L'invention concerne également un dispositif de dépôt de couches à partir d'un plasma, permettant de faire revenir des parties de la couche en cours de croissance lors d'intervalles de temps définis.
EP05729356A 2004-04-15 2005-04-15 Procede de revetement d'un corps de base, dispositif destine a la mise en oeuvre de ce procede et corps de base revetu Withdrawn EP1740737A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CH6572004 2004-04-15
PCT/CH2005/000211 WO2005100631A1 (fr) 2004-04-15 2005-04-15 Procede de revetement d'un corps de base, dispositif destine a la mise en oeuvre de ce procede et corps de base revetu

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EP1740737A1 true EP1740737A1 (fr) 2007-01-10

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EP05729356A Withdrawn EP1740737A1 (fr) 2004-04-15 2005-04-15 Procede de revetement d'un corps de base, dispositif destine a la mise en oeuvre de ce procede et corps de base revetu

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EP (1) EP1740737A1 (fr)
WO (1) WO2005100631A1 (fr)

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DE102007035502A1 (de) 2007-07-28 2009-02-05 Federal-Mogul Burscheid Gmbh Kolbenring
CN111962043B (zh) * 2020-08-19 2022-05-10 山东交通职业学院 一种轴承表面自润滑薄膜的制备装置及方法
CN112111747B (zh) * 2020-08-24 2024-03-01 青岛理工大学 一种硬质合金刀具清洗、涂层生产线及方法

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JPS58153775A (ja) * 1982-03-08 1983-09-12 Nippon Telegr & Teleph Corp <Ntt> 薄膜の製造方法
JPS62222073A (ja) * 1986-03-24 1987-09-30 Mitsubishi Electric Corp 薄膜形成装置
DE4102380C1 (en) * 1991-01-28 1992-03-26 Battelle-Institut Ev, 6000 Frankfurt, De High temp. superconductor film mfr. - by heating substrate with laser beam
US5759634A (en) * 1994-03-11 1998-06-02 Jet Process Corporation Jet vapor deposition of nanocluster embedded thin films
US6071595A (en) * 1994-10-26 2000-06-06 The United States Of America As Represented By The National Aeronautics And Space Administration Substrate with low secondary emissions
DE19513614C1 (de) * 1995-04-10 1996-10-02 Fraunhofer Ges Forschung Verfahren zur Abscheidung von Kohlenstoffschichten, Kohlenstoffschichten auf Substraten und deren Verwendung
GB2323855B (en) * 1997-04-01 2002-06-05 Ion Coat Ltd Method and apparatus for depositing a coating on a conductive substrate

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