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
  • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
  • C23C14/14—Metallic material, boron or silicon
  • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
• • 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
  • C23C14/24—Vacuum evaporation
  • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
• • 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
  • C23C14/50—Substrate holders
  • C23C14/505—Substrate holders for rotation 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
  • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
  • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
  • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
  • C23C28/321—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer with at least one metal alloy layer
• • 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
  • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
  • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
  • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
  • C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
• • 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
  • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
  • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
  • C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
  • C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer

Definitions

• Corrosion-protected component and method for its production and device for carrying out the method
• the invention relates to a corrosion-protected component, which consists of a base body and a corrosion-inhibiting surface layer, as well as a method for producing the same and a device for carrying out the method.
• Such components are often designed as connecting elements such as rivets, bolts or screws. They are primarily used in the automotive, aircraft and space industries as well as in mechanical and plant engineering. Numerous components are known which consist of a base body and a corrosion-inhibiting surface layer, this surface layer being metallic, ceramic or organic in nature. Chemical and electrochemical, especially galvanic deposition processes are used to apply the surface layer to the base body. Examples include copper plating, nickel plating, chrome plating and cadmium plating. Layers of zinc and its alloys are applied by hot dip coating.
• the corrosion-inhibiting surface layer is organic in nature, then it is usually applied by spraying or dipping with subsequent curing or crosslinking.
• metallic-ceramic mixed layers for. B. from a ceramic carrier layer with finely distributed lamellar metallic components used therein (DELTA-Tone, DACROMET) [US 4,391, 855, US 5,131, 948].
• the IVD process is a PVD process for applying a corrosion-inhibiting surface layer to the base body by means of the evaporation process, in which the rotating mesh or grid-like baskets are moved. It uses a glow discharge to activate the condensation process through ion bombardment and to achieve a denser layer structure.
• the Mc-Donnell-Douglas process as well as the IVD process produce corrosion-inhibiting coatings, the corrosion protection effect of which, however, is inadequate without post-treatment. Therefore, an elaborate after-treatment by mechanical
• the invention is therefore based on the object of providing a component consisting of a base body and a corrosion-inhibiting surface layer, and of specifying a method for its production and a device for carrying out the method, which are free from the deficiencies of the prior art.
• the manufacturing costs are to be significantly reduced and the surface layer should have a sufficient corrosion protection effect without the structure of the applied layer having to be subsequently compacted by mechanical means.
• the essence of the invention lies in the application of a layer of aluminum or an aluminum alloy or compound of sufficient thickness and with such a layer structure to the base body as can only be achieved by the direct action of a very dense plasma of comparatively low ion energy during the layer formation.
• This dense layer structure already present immediately after the deposition makes additional mechanical compression of the layer unnecessary. If the base bodies are distributed statistically and their position is often changed relative to the steam sources and if the special plasma becomes effective during the condensation process and without electrically shielding grids or networks between the plasma source and the base bodies during the layer formation, it is also possible for complex shapes Basic bodies achieve a uniform coating of high quality.
• Such a layer is characterized by a dense, fine-grained, largely pore-free structure.
• the component according to the invention additionally comprises a layer of chromate or phosphate and / or a layer of an organic material.
• the surface layer made of aluminum or an aluminum alloy or compound in a manner known per se.
• the component contains a surface layer made of an aluminum alloy, an aluminum-magnesium alloy with a magnesium content of 1 to 10 percent by weight, preferably 3 to 5 percent, or an aluminum-zinc alloy with a zinc content is particularly suitable for this purpose from 1 to 10 percent by weight, preferably from 2 to 5 percent.
• the surface layer can also be deposited under the action of a reactive gas and then contain aluminum compounds such as aluminum oxide, nitrate or carbide.
• the method for producing the components according to the invention is carried out in a vacuum coating system.
• This contains a drum or basket that can be rotated around a horizontal axis.
• Steam and plasma sources are located inside the rotating basket.
• a multiplicity of base bodies are essentially fixed on the inner wall of the rotating basket and passed one or more times through a vapor cloud generated by metal evaporators. Thereafter, mixing with a change in the position and orientation of the base body relative to the steam sources is carried out and the base body thus fixed in a changed position and direction is guided through the steam cloud one or more times.
• the alternation of mixing and fixing of the base bodies and their coating is continued until the base bodies are provided on all sides and without defects with a surface layer of the stated average thickness.
• the process can be designed as a continuous coating process for the treatment of bulk goods. It is crucial for the production process that the evaporators are arranged inside the rotating basket and thus cause the layer formation directly, ie without interposed nets, grids or sieve structures, and that the coating is carried out with plasma activation.
• the layer formation process takes place in the plasma of a hollow cathode arc discharge.
• ion energies of a few to a few tens of electron volts and a charge carrier density in the range of over 10 10 / cm 3 are typically over 10 1 l / cm 3 , characteristic. It is also important for the effectiveness of the plasma that the plasma sources are arranged inside the rotating basket and that there are no potential-determining sieves or networks between the hollow cathode plasma sources and the base bodies to be coated.
• the surface layer applied under these conditions has a dense, fine-grained, pore-free structure, which provides corrosion protection for the component.
• the base bodies of the components consist of a ferromagnetic steel material
• magnetic fixation of the base bodies can also be expedient.
• an arrangement of permanent magnets or an electromagnet with a plurality of poles, the field lines of which penetrate the wall of the rotating basket and cause the magnetic fixing of the base body is located in the upper region of the rotating basket, but outside and stationary.
• the basic bodies are mixed with changes in direction and position when the basic bodies moved with the rotating basket leave the area penetrated by the magnetic field and are subject to the action of gravity.
• the mixing takes place with a change in direction and position of the base body with the aid of a mechanically acting scraper, which separates the base body from the wall of the rotating basket after it has passed through the steam zone.
• a motor-driven, rotating brush is also particularly advantageous in order to bring about a large number of changes in direction and position for the base body.
• the rotational speed of the rotating basket is changed frequently, preferably periodically, in such a way that the rotational speed is temporarily higher than the rotational speed at which the base bodies are fixed by centrifugal force and temporarily lower than this characteristic rotational speed, whereby they are mixed under the action of gravity and changed in their position and position before they are fixed again by centrifugal force.
• the mixing of the base bodies is carried out by a device which contains a rotating roller with inner, likewise rotating magnetic poles. A direct mechanical contact between the wall of the rotating basket and the stripping device can thus be avoided and a particularly gentle mechanical treatment of the base body can be achieved.
• boat evaporators heated by direct current passage, in which the evaporation material for the surface layer is supplied in wire form.
• Such boats are most often made of titanium boride. Arrangements of many similar boat evaporators arranged in parallel next to one another are suitable for carrying out the method in coating systems with a larger longitudinal extension of the rotating basket.
• Another design of the production method uses one or preferably a plurality of electron beam evaporators to generate the aluminum vapor or the vapor of the aluminum alloy. So-called transversal evaporators are used in coating systems of lower output. In high-power coating systems, electron beam evaporators are used according to the invention, which have a preferably ceramic evaporator crucible that extends parallel to the axis of the rotating basket and a separate generation, focusing and deflection unit for the electron beam in the form of a so-called axial electron gun.
• Another expedient embodiment of the method according to the invention further includes exposing the base bodies to the action of a dense plasma before the surface layer is applied in order to activate its surface.
• a dense plasma pretreatment causes desorption of foreign atoms, the removal of oxidic contaminations and an energetic activation of the surface and thus ensures good adhesive strength and uniform growth of the surface corrosion-inhibiting surface layer on the base bodies.
• a preferred embodiment of the method includes the pretreatment and activation of the surface of the base body using the dense plasma of one or more hollow cathode arc discharges, ie the same plasma sources that are also used for the plasma-activated deposition of the surface layer.
• a component according to the invention and a method for its production, together with the device required for carrying it out, are explained in more detail below.
• the component has the function of a hollow rivet with a length of 6 mm and a shaft diameter of 4 mm, as it is used in large quantities as a connecting element in mechanical engineering and vehicle construction for the permanent mechanical connection of machine, system and body parts.
• the material for the base body is the unalloyed carbon steel C 35 (material no. 1.0501).
• this base body is coated on all sides with an aluminum alloy layer that is on average 25 ⁇ m thick. Inside the recess of the rivet shaft, the layer thickness is approximately 15 ⁇ m.
• This surface layer consists of the aluminum-magnesium alloy AIMg3 with a magnesium content of about 3 percent by weight.
• the micrograph of the surface layer shows a dense fine-grained structure without pores with a typical grain size of 1 ⁇ m when examined by light and electron microscopy. There is no stalky layer growth and therefore no grain boundaries that run through the entire layer. In the salt spray test, no recognizable red rust forms after 200 hours. A test on numerous of these components shows that they meet the requirements of the MIL-C-83488 C standard, which is widely used in aircraft construction.
• the coating process for applying the AlMg3 surface layer to the base body includes a PVD process that is carried out in a vacuum coating system.
• the main chamber of the coating system has a volume of approximately 1 cubic meter and houses a water-cooled rotating basket with a diameter of 800 mm and a length of 700 mm.
• the rotating basket is horizontally supported on one side and driven by a motor; it typically rotates at 72 revolutions per minute.
• the coat surface of the rotating basket is closed.
• the boat evaporators are heated at 800 A each at 15 V.
• the wire feed sets an evaporation rate of 5 grams per minute and evaporator.
• the wire has the composition and quality AlMg3 F22.
• the hollow cathode arc discharges burn with an argon inlet of 80 sccm at 300A at an operating voltage of 30 ... 35 V between each hollow cathode and two electrodes arranged symmetrically between the boat evaporators and connected as anode.
• the coating system works quasi-continuously without vacuum interruption. For this purpose, it is equipped with a separately evacuable vacuum lock for inserting and removing 25 kg of the basic body. The transfer of the base body from the input lock into the rotary basket or from the rotary basket into the output lock takes place through a valve and tubular guide devices under the effect of gravity.
• the basic bodies are filled in batches of 25 kg into the input lock of the coating system. After degassing, they are transferred to the rotating basket and pretreated there for 10 minutes in the dense hollow cathode plasma.
• the rotating basket is at a negative potential of 500 V.
• the subsequent process for plasma-activated evaporation takes 20 minutes.
• the base bodies are fixed on the inner wall of the rotating basket by centrifugal force and lie in approximately three layers, statistically evenly one above the other.
• the basic body is periodically wiped off before the centrifugal force is fixed again using rotating metal brushes.
• the rotary basket is braked and inclined to transfer the coated base body to the delivery lock.
• a swiveling screen prevents the falling components from colliding with the evaporators and plasma sources. At intervals of 35 minutes, a batch of about 25 kg of the coated components is ejected from the system. The parts are checked and packed. The high productivity of the coating system and the avoidability of expensive post-treatments of the surface layer are the basis for low manufacturing costs for the components according to the invention.

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• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Engineering & Computer Science (AREA)
• Materials Engineering (AREA)
• Mechanical Engineering (AREA)
• Metallurgy (AREA)
• Organic Chemistry (AREA)
• Inorganic Chemistry (AREA)
• Physical Vapour Deposition (AREA)
• Other Surface Treatments For Metallic Materials (AREA)

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• 2002
  • 2002-08-30 DE DE10240160A patent/DE10240160A1/de not_active Ceased
• 2003
  • 2003-08-28 EP EP03794953A patent/EP1532286A1/de not_active Withdrawn
  • 2003-08-28 JP JP2004535187A patent/JP2005537393A/ja active Pending
  • 2003-08-28 AU AU2003258677A patent/AU2003258677A1/en not_active Abandoned
  • 2003-08-28 WO PCT/EP2003/009504 patent/WO2004024976A1/de active Application Filing
• 2005
  • 2005-02-25 US US11/064,964 patent/US20050196548A1/en not_active Abandoned

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