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
  • C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
  • C23C14/564—Means for minimising impurities in the coating chamber such as dust, moisture, residual gases
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B24—GRINDING; POLISHING
  • B24C—ABRASIVE OR RELATED BLASTING WITH PARTICULATE MATERIAL
  • B24C1/00—Methods for use of abrasive blasting for producing particular effects; Use of auxiliary equipment in connection with such methods
  • B24C1/003—Methods for use of abrasive blasting for producing particular effects; Use of auxiliary equipment in connection with such methods using material which dissolves or changes phase after the treatment, e.g. ice, CO2
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B24—GRINDING; POLISHING
  • B24C—ABRASIVE OR RELATED BLASTING WITH PARTICULATE MATERIAL
  • B24C1/00—Methods for use of abrasive blasting for producing particular effects; Use of auxiliary equipment in connection with such methods
  • B24C1/04—Methods for use of abrasive blasting for producing particular effects; Use of auxiliary equipment in connection with such methods for treating only selected parts of a surface, e.g. for carving stone or glass
• • 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
  • C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
  • C23C16/4407—Cleaning of reactor or reactor parts by using wet or mechanical methods

Definitions

• the invention relates to a cleaning method in connection with coating installations, in particular in connection with vacuum coating installations.
• coating surfaces are coated inevitably in the coating chamber whose coating is not desirable.
• Such surfaces may be, for example, parts of the chamber, as well as parts of the substrates to be coated as well as support and other secondary surfaces.
• the undesired coated surfaces are referred to as secondary surfaces, while the desired coated surfaces are referred to as target surfaces.
• the secondary areas are at different potentials such as bias current, insulating or ground. This leads to different adhesion strengths of the coating on secondary surfaces.
• WO 08/040819 describes an improvement of the above-mentioned dry ice jet cleaning method in that a functional layer is provided on the surface to be cleaned, on which the impurity adheres less than it would adhere to the surface to be cleaned.
• the proposed functional layer is a plasma polymer layer.
• impurities in the context generally called both organic and non-organic materials to be stripped.
• the functional layer has a lower thermal conductivity there than the object to be cleaned, and the contamination adheres less firmly to the functional layer than it does to the object surface underlying the functional layer.
• several disadvantages associated with PVD or CVD coating systems are anchored:
• the contamination should very well adhere to the surface, as otherwise spalling could lead to the substrates to be coated themselves being undesirably contaminated.
• the plasma polymer layer is non-conductive.
• the components of the coating chamber should generally have a conductive surface in order not to negatively influence the electrical and / or magnetic conditions for the coating process.
• the basic idea of the present invention is to pretreat the secondary surfaces prior to the coating process in such a way that the adhesion of the coating material to the secondary surfaces is greatly reduced in the subsequent coating process compared to adhesion without pretreatment. In this way, the cleaning is greatly simplified.
• Such a pretreatment according to the invention can consist, for example, of applying a suitable "non-stick layer” to the secondary surfaces
• the non-stick layer is characterized by low adhesion to the secondary surfaces or by a low adhesion of the contamination to the non-stick layer Since the "non-stick layer" after the actual coating between the minor surface and the material applied in the coating process, the adhesion of the coating material is effectively prevented.
• the non-stick layer should be temperature-resistant, electrically conductive and vacuum-technically harmless. Vacuum safety, in particular, is a prerequisite for PVD processes.
• the application of the release layer should have no negative impact on the properties of the actual layer on the target surfaces.
• the method of dry irradiation can be applied.
• the cleaning process itself is sufficiently known to the person skilled in the art, for example, from WO08 / 040819 or WO02 / 072312 and need not be further elaborated here.
• FIG. 1 outlines the process of the pretreatment according to the invention
• FIG. 2 outlines an example of the use of a masking template
• FIG. 3 outlines the facilitated cleaning process after the coating process
• FIG. 4 outlines the cross section through an anti-adhesive layer and coating
• the non-stick layer is vacuum-compatible. However, this means that in the non-stick layer no binders or similar excipients occur.
• a suspension of powder in readily volatile solvent in a suitable mixing ratio is used in the application of the non-stick layer to the secondary surfaces.
• the volatile solvent must not form a chemical bond with the powder or treated surface used.
• the use of a volatile solvent as the carrier medium of the suspension ensures that the solvent has already completely evaporated immediately after the spraying process and only a slightly adhering powder layer remains on the surface.
• the solvent e.g. Isopropanol very well suited.
• Graphite powder is sufficiently temperature resistant, electrically conductive, especially in vacuum vacuum-compatible, and non-stick properties can be met and therefore used in the PVD process.
• the order is carried out, for example, by spraying by means of a spray gun.
• a spray gun This can be done without gas assistance or with gas support.
• gas assistance in the latter case, inter alia, air nitrogen or C0 2 is suitable.
• the influencing variables relevant for the spraying process eg injection pressure, nozzle size of the gun, mixing ratio of the suspension, spraying distance and duration
• other application methods are also possible (painting, dipping, etc.).
• the release layer ensures that the coating material applied to the treated minor surfaces during the PVD process can be substantially completely removed after the PVD process as described above by the application of the dry ice blasting process. This can be done by means of pellet blasting or C02 snow. Another possibility is to use the dry ice-water mixed jet process, as described in DE102006002653. Further post-treatment is not required, the secondary surfaces can be immediately provided with a new non-stick layer for subsequent use.
• confinement rings In connection with arc evaporation, often so-called confinement rings are used. These surround the coating material-containing target of the evaporation source and ensure that the arc remains restricted to the area of the target surface. Due to their proximity to the target material, they are subject to a strong application of material in the PVD coating process and their cleaning previously required extremely aggressive methods such as sandblasting or even post-machining. By applying the graphite powder according to the invention, the necessary electrical conductivity is maintained. The coating material applied during the PVD process comes to rest on the graphite layer. The graphite layer including coating can be easily removed from the confinement ring. The same applies to substrate holders which support the substrates to be coated during the coating process. Due to their spatial close to the substrates to be coated and these are heavily coated.
• Substrahalers are pretreated according to the invention with an anti-adhesive layer, so they can be cleaned easily and quickly and without wear after the PVD process.
• the system additionally comprises anodes for providing a plasma discharge, for example sputter sources, low-voltage arc discharges and etching devices, then these too can advantageously be pretreated prior to a coating step by applying an anti-adhesion layer.
• the non-stick layer itself is applied in a coating system as a relatively loose layer.
• the substrate carriers are brought into the coating system in the unequipped state.
• a layer can be, for example, a PVD layer which is coated without bias voltage.
• such a layer may be a graphite layer.
• a copper-arc coating is proposed as the non-stick layer, in contrast to the plasma polymer layer, copper is very readily electrically conductive and has a greater thermal conductivity than, for example, the inorganic non-metallic layers applied by means of PVD. More generally, as an anti-adhesion layer, metallic, i. good thermally conductive layers are used which are very different in thermal material properties of the PVD layer properties.
• the layer thickness of the copper arc coating is preferably in the range of 0.1-0.4 mm, the layer thickness of the contamination being in the range of 1-100 pm.
• this surface with a so-called nano-seal.
• This effect known as the so-called lotus blossom effect, is known to mean that impurities adhere more poorly to the structured surface and thus are easier to remove.
• the adhesive strength can be substantially adjusted. In particular, stresses on the surface are avoided by the structuring, so that a chipping from the surface during the coating process is less to be feared.
• the electrically or non-conductive deposits on the anode can cause the function of the anode to be no longer guaranteed even after a coating process, so that the cleaning of the anode after each batch is absolutely necessary in such processes is.
• the procedure is as follows.
• the starting point is an anode, free from deposits and residues, i. the "virgin" anode before the first coating process or after a cleaning treatment.
• a first step in the example, the immediate vicinity of the surface of the anode to be coated with an anti-adhesion layer, which in this case represents a secondary surface according to the definition defined in this description, is covered and / or masked.
• an anti-adhesion layer which in this case represents a secondary surface according to the definition defined in this description.
• a sheet metal template with adapted cut-out and suitable geometry comes into question. The template turns out that only the desired areas are provided with non-stick coating.
• the non-stick layer is applied by the tip method with a spray gun.
• a suspension containing the non-stick layer material is sprayed onto the masked anode.
• the anode is a vertically mounted metal surface. Care must therefore be taken that the spray distance and the thickness of the coating are selected so as to prevent excess solvent from dripping down on the surface. It is very advantageous if the volatile solvent in the aerosol already largely evaporated between spray nozzle and surface to be treated. This results in optimum coverage by graphite powder.
• the mixing ratio of solvent and graphite powder also plays a role here.
• the nozzle size is for example between 0.3mmm and 2mm and is preferably 0.8mm.
• compressed air is used at a pressure between 0.2bar and 1 .0 bar, preferably between 0.5bar and OJbar.
• the compressed air should be de-oiled and as free of particles as possible so as not to introduce any dirt into the suspension and thus into the non-stick layer. It is particularly important to ensure that the pneumatics of the gun does not introduce dirt.
• the suspension is homogenized. This can be done by shaking, shaking, by sonication or other methods known to those skilled in the art.
• a spray distance between 50mm and 250mm, ideally between 100mm and 200mm.
• a large spraying distance is advantageous in that the solvent is already given the opportunity during the flight time to evaporate. Too large a distance, however, leads to a too wide spatial dispersion.
• the layer thickness of the non-stick layer to be applied is in the example between 0.05 mm and 2.0 mm.
• the criterion "optically surface covering" has proven to be suitable and advantageous because of its simplicity.At least if the secondary surfaces are not themselves graphite surfaces, this can be done well due to the optical properties of the graphite powder several and advantageously evenly guided spray passes.
• the following should preferably be considered: Since the powder layer adheres to the surface essentially by adhesive forces, contact with the coated secondary surfaces should be avoided as far as possible after spraying. Therefore, it is advantageous - where possible - to treat the components in the finished installed state or to use appropriate devices and / or tools ("handling aids"), so that a violation of the non-stick layer is avoided.
• the sheet template used for masking is removed. It should be pointed out again that it does not always require such masking, but this was used in the example.
• the pre-treatment is completed and the actual PVD coating can be carried out in the usual way. That the coating chamber is charged with workpieces, the chamber is closed and pumped off, the coating, for example arc evaporation, is carried out and the coating chamber is then ventilated and opened. In this case, the pretreatment of the anode according to the invention has no adverse effect on the coating.
• the secondary surfaces can be cleaned according to the invention by means of the dry ice blasting.
• the C02 snow cleans gently, dry, residue-free and vacuum-compatible.
• the anode Before the next coating process, the anode is again pretreated according to steps 1 to 3. Ideally, this procedure is performed after each coating process. However, it is also possible to dispense with cleaning by means of dry ice blasting after a coating process and to renew the release layer only after several coating cycles.
• the anode is protected by the procedure according to the invention.
• the pretreatment according to the invention can be advantageously used in other coating methods, in particular in other vacuum coating methods such as, for example. If necessary, then the material of the release layer could be adjusted.
• the invention can also be used to advantage for substrates to be coated, for example if only a part of the substrate surface is to be coated.
• the non-coating surface portions of the substrates had to be shielded by the brackets.
• the non-coating parts of the substrate surface can be covered with an anti-adhesion layer by means of the procedure according to the invention, which can be cleaned after the coating in a simple manner by means of a dry-ice jet process.
• similar non-stick layer treatments e.g., carousels, substrate holders, substrates, etc.
• the use of an automatic spraying device is advantageous

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• Chemical & Material Sciences (AREA)
• Engineering & Computer Science (AREA)
• Mechanical Engineering (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Materials Engineering (AREA)
• Metallurgy (AREA)
• Organic Chemistry (AREA)
• General Chemical & Material Sciences (AREA)
• Application Of Or Painting With Fluid Materials (AREA)
• Physical Vapour Deposition (AREA)

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• 2010
  • 2010-01-25 DE DE102010005762A patent/DE102010005762A1/de not_active Withdrawn
  • 2010-12-22 WO PCT/EP2010/007971 patent/WO2011088884A1/de active Application Filing
  • 2010-12-22 MX MX2012008661A patent/MX2012008661A/es unknown
  • 2010-12-22 SG SG10201500561SA patent/SG10201500561SA/en unknown
  • 2010-12-22 CA CA2788448A patent/CA2788448A1/en not_active Abandoned
  • 2010-12-22 CN CN201080062436.3A patent/CN102812154B/zh not_active Expired - Fee Related
  • 2010-12-22 BR BR112012018524A patent/BR112012018524A2/pt not_active IP Right Cessation
  • 2010-12-22 RU RU2012136472/02A patent/RU2554838C2/ru not_active IP Right Cessation
  • 2010-12-22 SG SG2012055216A patent/SG182730A1/en unknown
  • 2010-12-22 KR KR1020127021306A patent/KR20120120944A/ko not_active Application Discontinuation
  • 2010-12-22 JP JP2012549264A patent/JP2013518177A/ja active Pending
  • 2010-12-22 US US13/574,817 patent/US20120298139A1/en not_active Abandoned
  • 2010-12-22 EP EP10800894A patent/EP2529040A1/de not_active Withdrawn

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