WO1999054060A2 - Surfaces industrielles, notamment en metal ou en metallo-ceramique, chargees d'un compose fluoro-organique - Google Patents

Surfaces industrielles, notamment en metal ou en metallo-ceramique, chargees d'un compose fluoro-organique Download PDF

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Publication number
WO1999054060A2
WO1999054060A2 PCT/DE1999/001133 DE9901133W WO9954060A2 WO 1999054060 A2 WO1999054060 A2 WO 1999054060A2 DE 9901133 W DE9901133 W DE 9901133W WO 9954060 A2 WO9954060 A2 WO 9954060A2
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Prior art keywords
chain
formula
branched
straight
loading
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Application number
PCT/DE1999/001133
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German (de)
English (en)
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WO1999054060A3 (fr
Inventor
Igor Groza
Natalia Bultykhanova
Original Assignee
Extreme Energy And Power Company Limited
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.)
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Publication date
Priority claimed from DE19848614A external-priority patent/DE19848614A1/de
Priority claimed from DE19848591A external-priority patent/DE19848591A1/de
Priority claimed from DE19848613A external-priority patent/DE19848613A1/de
Application filed by Extreme Energy And Power Company Limited filed Critical Extreme Energy And Power Company Limited
Priority to AU44967/99A priority Critical patent/AU4496799A/en
Publication of WO1999054060A2 publication Critical patent/WO1999054060A2/fr
Publication of WO1999054060A3 publication Critical patent/WO1999054060A3/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • B05D1/18—Processes for applying liquids or other fluent materials performed by dipping
    • B05D1/185—Processes for applying liquids or other fluent materials performed by dipping applying monomolecular layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
    • C03C17/32—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material with synthetic or natural resins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/002—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from unsaturated compounds
    • C08G65/005—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from unsaturated compounds containing halogens
    • C08G65/007—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from unsaturated compounds containing halogens containing fluorine
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
    • C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
    • C10M105/32—Esters
    • C10M105/34—Esters of monocarboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
    • C10M105/56—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing nitrogen
    • C10M105/58—Amines, e.g. polyalkylene polyamines, quaternary amines
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
    • C10M105/56—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing nitrogen
    • C10M105/58—Amines, e.g. polyalkylene polyamines, quaternary amines
    • C10M105/64—Amines, e.g. polyalkylene polyamines, quaternary amines having amino groups bound to a carbon atom of a six-membered aromatic ring
    • C10M105/66—Amines, e.g. polyalkylene polyamines, quaternary amines having amino groups bound to a carbon atom of a six-membered aromatic ring containing hydroxy groups
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
    • C10M105/72—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing sulfur, selenium or tellurium
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M107/00—Lubricating compositions characterised by the base-material being a macromolecular compound
    • C10M107/38—Lubricating compositions characterised by the base-material being a macromolecular compound containing halogen
    • 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
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
    • 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
    • C23C16/02—Pretreatment of the material to be coated
    • C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
    • 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
    • C23C30/00—Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2211/00—Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions
    • C10M2211/04—Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions containing carbon, hydrogen, halogen, and oxygen
    • C10M2211/042—Alcohols; Ethers; Aldehydes; Ketones
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2211/00—Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions
    • C10M2211/04—Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions containing carbon, hydrogen, halogen, and oxygen
    • C10M2211/044—Acids; Salts or esters thereof
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2211/00—Organic non-macromolecular compounds containing halogen as ingredients in lubricant compositions
    • C10M2211/06—Perfluorinated compounds
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
    • C10M2213/04—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions obtained from monomers containing carbon, hydrogen, halogen and oxygen
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2213/00—Organic macromolecular compounds containing halogen as ingredients in lubricant compositions
    • C10M2213/06—Perfluoro polymers
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/04—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M2215/04—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2215/042—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms containing hydroxy groups; Alkoxylated derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/08—Amides
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/08—Amides
    • C10M2215/082—Amides containing hydroxyl groups; Alkoxylated derivatives
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/26—Amines
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/28—Amides; Imides
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
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    • C10N2040/00—Specified use or application for which the lubricating composition is intended
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    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/30—Refrigerators lubricants or compressors lubricants
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    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/32—Wires, ropes or cables lubricants
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    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/34—Lubricating-sealants
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    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/36—Release agents or mold release agents
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    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/38—Conveyors or chain belts
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    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/40—Generators or electric motors in oil or gas winning field
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    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/42—Flashing oils or marking oils
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/44—Super vacuum or supercritical use
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    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/50—Medical uses
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    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/015—Dispersions of solid lubricants
    • C10N2050/02—Dispersions of solid lubricants dissolved or suspended in a carrier which subsequently evaporates to leave a lubricant coating
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    • C10N2070/00—Specific manufacturing methods for lubricant compositions

Definitions

  • the invention relates to the loading of in particular metallic or metal-ceramic technical surfaces with an organofluorine compound.
  • the invention is used in particular for loading technical surfaces in the form of movement contact surfaces of machine components, work or
  • Functional surfaces of mechanical deformation tools or metal-containing surfaces of optical disks or a surface coating or a surface covering thereof are also preferred area of application of the invention.
  • Another preferred area of application of the invention is surface treatment before or during a coating process, in particular a plasma coating process.
  • “Movement contact surface” in the sense of the invention is to be understood as a sliding or rolling surface of the machine component on which, in cooperation with another machine component that is in contact with the surface, it results in a sliding and / or rolling movement of the two which is subject to friction and wear Machine components come relative to each other.
  • Gears and gear drives to name just a few examples, and for example in motor vehicle engine construction in the piston-cylinder unit, the valve arrangement, the camshaft arrangement and the crankshaft bearing of the internal combustion engine.
  • Lubricant related in the engine area, for example, engine oil, which provides a hydrodynamic lubricating film.
  • Various additives are added to the oil, especially motor oil, in order to be able to perform other necessary or desired functions in addition to the wear protection function.
  • the viscosity improvers are to be mentioned here, which are intended to ensure that the engine oil viscosity does not decrease too much with increasing engine temperature, and which for this purpose consist of mostly ball-shaped molecular structures.
  • Temperatures in an atmospheric oxygen environment are often not sufficiently stable and are therefore not suitable in internal combustion engines without an engine oil to ensure an adequate lubrication function.
  • Lubricants which form a lubricating film between the components moving relative to one another have already made efforts in the prior art to harden the surface of the respective components by applying a coating on at least one surface of the components sliding on one another.
  • Iron alloys used in internal combustion engines were able to reduce the areas exposed to wear by appropriate
  • Aluminum alloys can be protected against premature wear by applying a wear layer such as Nikasil (R) .
  • a wear layer such as Nikasil (R) .
  • LO layer is a layer of oxides, nitrides and / or carbides of a stoichiometric or substoichiometric metal component, which are either present on the tread, in particular the cylinder liner of the engine, or are applied by a corresponding method. In any case, it is a relatively loosely applied layer that exhibits relatively poor properties with regard to adhesion to the metal surface.
  • the socket must be inserted into the mold when the block is being cast and enormous casting pressures must be applied in order to ensure a firm connection between the engine block, which is usually made of aluminum, and the socket from others
  • the invention can also be advantageously used for loading the working or functional surfaces of a mechanical shaping tool with an organofluorine compound.
  • Shape tool in the sense of the invention is a cutting tool for one of the cutting types of machining from fine machining such as honing, lapping, fine turning, fine drilling, press polishing and fine grinding to other machining types such as turning, milling, drilling, planing, filing, sawing To understand cutting, punching and chiseling.
  • shapeing tool is also to be understood as a tool for non-cutting processing such as bending, forging, rolling, embossing, drawing, deep drawing, pressing, pressing and other non-cutting deformations. These include punches, rollers, hammers, extrusion and drawing nozzles, matrices and patrices and the like. The same also applies to casting molds and similar casting tools for plastics processing.
  • Tools with working tips, cutting edges and other work surfaces made of a carbon-containing, ceramic, metal-containing or metallic material such as HSS, powder-metallurgical and other tool steels, hard metals and tungsten carbides, cutting ceramics, CBN and PCD, natural diamond and cermet are particularly suitable for the inventive loading with the fluoroorganic compound - materials.
  • work surface is to be understood as the functional surface of the tool with which the tool can process in contact with the workpiece carries out.
  • the fluorine compounds in particular are known, in particular PTFE, which are used in the machining or shaping process, for example, as additives which are added in solid or dissolved form to the lubricant or coolant used in mechanical processing, in order to reduce tool wear on the one hand and to increase the service life of the tool, but also to improve the surface quality of the machined workpiece.
  • the effect of the polymer is only limited to the initial stage of lubricant use. If and after the lubricant is saturated with the cutting process wear products, the polymer loses its effect.
  • the fluoropolymer of the known material systems is thermally unstable and, when used at elevated temperatures, of approximately 500 ° C. and higher, causes the polymer to decompose; the decomposition products are chemically aggressive and unstable, which can significantly interfere with the machining process. Suggestions are also known
  • the invention When applied to the loading of the working and functional surfaces of mechanical deformation tools, the invention achieves an increase in the service life of mechanical deformation tools and tool systems by loading them with a special organofluorine compound.
  • the invention provides an improved functionality of the work surfaces of the tool and a suitable surface topography of the tools used in adaptation to the respective machining process to achieve less friction with the workpiece to be machined and thus reduced tool wear.
  • optical disk in the sense of the invention means semitransparent (tinted) or fully transparent panes, but also reflective or mirrored panes, regardless of their shape and size.
  • the disk can be flat or curved or curved, it can also be designed on one surface different from its other surface.
  • the disc can be plate-shaped or lenticular.
  • a currently preferred field of application of the invention is in the field of automotive engineering. In this field of application, the invention is also directed, in particular, to windshields and headlight panes.
  • the optical disc can be made of a metal-containing
  • Base material to be produced for example a base material with color pigments made of a metal compound.
  • the optical disk is preferably provided with a metal-containing surface coating.
  • the base material of the optical disk can be made of glass or a
  • the surface coating can be designed, for example, as a functional or decorative layer.
  • DLC layers are known, but they are still too expensive to manufacture for the windshield area and cannot be used for the optics because the light transmission is too poor and the light losses would therefore be too high for the conventional optical area. These layers are also unacceptable for plastic glasses, since they are not sufficiently flexible and can therefore flake off at any time during use.
  • the invention When applied to the loading of optical disks, the invention specifically achieves to improve their resistance to environmental influences.
  • the surface coating is in particular made of a metal or a metal alloy, a metal oxide, a metal nitride, a metal carbide.
  • a further field of application of the invention is that of CVD or PVD or PCVD coating processes (chemical, physical or physical / chemical deposition from the ionized gas phase) or other coating processes, in particular plasma coating processes.
  • CVD or PVD coating processes are state of the art well known.
  • a cleaned substrate to be coated is exposed to an atmosphere composed of a chemical compound of the layer-forming compound or of the layer-forming element, for example a semiconductor element, or a chemical or physical decomposition treatment , whereby the connection or the element is deposited on the substrate.
  • This creates a high-purity layer for example made of semiconductor material, such as
  • the invention remedies this by providing a surface treatment agent and a method for improving interface adhesion.
  • the object is thus achieved by the invention, in particular to improve the wear and resistance properties of technical surfaces.
  • the invention lies in particular in the use of a special organofluorine compound of the formula R f -V for producing a surface loading matrix of the technical surface which is composed of the organofluorine compound R f and is bound to the surface via residues of group V.
  • the technical surface is in particular a metallic or metal-ceramic surface, which can, however, also be coated with a coating containing carbon or silicon or nickel silicon.
  • R f stands for an aliphatic hydrocarbon radical which can be partially or completely fluorinated and can be straight-chain, branched-chain or cyclic, where the
  • Hydrocarbon residue can be interrupted by one or more oxygen, nitrogen or sulfur atoms.
  • V stands for the previously specified polar or dipolar group and R v denotes a straight-chain or branched-chain alkylene radical, which can be partially or completely fluorinated or chlorofluorinated, with 1 to 12, preferably up to 8, carbon atoms.
  • an alkylene radical is to be understood in particular as a methylene or polymethylene group.
  • V is preferably a member from the group consisting of -COOH, -S0 3 H, -COOR, -S0 3 R, -COR, ⁇ B, -OP (OH) 2 , -OPO (OH) 2 , and - S0 2 R, in particular -COOH, -S0 3 H, -COR, and -S0 2 R, where R is a straight-chain or branched-chain alkyl radical which is partially or completely fluorinated and has up to 12, preferably up to 8, carbon atoms, or stands for -RN-, where V stands for the previously indicated polar or dipolar group and R v is a straight-chain or branched-chain
  • Alkylene radical which can be partially or completely fluorinated or chlorofluorinated, with up to 12, preferably up to 8 carbon atoms.
  • R f which is partially or completely fluorinated, is preferably one with a molecular weight of 1000 to 10,000, preferably 1400 to 10000.
  • molecular chains of favorable length are formed, which on the one hand are not too short and, on the other hand, are not too long in order to be able to form the spiral-like molecular structures to be explained further below.
  • the radical R f is more preferably partially or fully fluorinated alkanes or partially or fully fluorinated alkyl ethers or thioethers with a preferred molecular weight of 1,400 to 10,000.
  • R f represents a straight-chain or branched-chain aliphatic hydrocarbon radical having the following schematic formula (1): RO x (C a H b F 2a . B O) m (C a H b F 2a _ b ) n (1)
  • X 0.1; 20 ⁇ n + m ⁇ 500; n> 1 and m ⁇ 0, and
  • R fl R f2 -V Compounds of the general formula R fl R f2 -V can be used as particularly preferred compounds of the formula R f -V in the surface loading matrix according to the invention, where V has the meaning given above and the groups R fl and R f2 have the following meanings:
  • R f2 stands for a perfluoroalkyl ether group of the following formulas (I) to (IV): (-CFCF 2 0-) n (CF 2 0) m (CFO) lc CF 2 - (I),
  • n, m and k denote the number of the unit indicated in each case in a perfluoroalkyl ether group (I) or (II), but, for example, m or k units are not follow each other directly.
  • Temperature can be treated with a mixture of fluorine and oxygen.
  • An alternative way of producing these compounds consists in the reaction of perfluoroethylene with formaldehyde under elevated pressure at 20-60 * C in the presence of hydrogen fluoride to form the corresponding oxetane and subsequent polymerization in the presence of COF 2 * KF in an aprotic Solvent with ring opening of the oxetane.
  • the organofluorine compound of the formula R f -V can be used as such, ie undiluted, or, preferably, in the form of a liquid substance system from a suspension in which the organofluorine compound R f -V is used in a proportion of 0.5 to 40 % By weight is contained in a suspension liquid, in particular water.
  • a solution containing 0.001 to 10% by weight, preferably 0.5 to 2% by weight of the organofluorine compound R f -V in a solvent is used.
  • the organofluorine compound adheres firmly to the surface loaded with it, even after the excess liquid has been knocked off or washed off and dried.
  • the surface to be loaded is completely freed of residual fat due to its fat-dissolving properties, so that the attachment of the molecules R f -V to the surface is made possible accordingly easily.
  • Application can be by rubbing, brushing, spraying, dipping or otherwise wetting the surface, and the solvent evaporates after the excess solution has drained or washed off the surface.
  • the compounds of the general formula Rf-V can be obtained in the form of a solution in a solvent, in accordance with the invention a halogenated hydrocarbon solvent, or in the form of an aqueous solution with an emulsifier or surfactant in an amount of from 0.01 to 5% by weight on the total weight of the aqueous solution.
  • the emulsifier or surfactant used can preferably be one or more compounds in an amount of from 0.01 to 3% by weight, which is sufficient to dissolve the compound of the formula R f -V in water, the emulsifier or the surfactant itself has fluorinated hydrocarbon radicals, for example fluorinated or perfluorinated alkyl radicals.
  • surfactants or emulsifiers can be used in the form of cationic, anionic, nonionic or ampholytic surfactants or similar surface-active substances.
  • the following compounds are mentioned by way of example: (a) C 8 F 17 CONHCH 2 CH 2 CH 2 N (CH 3 ) 2 + Cl " (cationic surfactant);
  • Fluorine-containing cationic, nonionic or ampholitic surfactants of the "Zonil” type from DuPont, or ethoxylated perfluoroalcohols with a number of perfluoroethoxy units of 5 to 25, or surfactants of the type such as, for example, the perfluorinated, can also be used as emulsifiers
  • Acid amide derivatives with a quaternary amino group and sulfate or sulfonate anions such as C 6 F 13 CONHCH 2 CH 2 CH 2 N (CH 3 ) 2 + " 0 3 SOC 2 H 5 , or a nonionic ⁇ -surfactant such as CF 3 _CFH_CF 2 _CH 2 0 (C 2 H 4 0) 7 _ 15 H, or a nonionic hydrocarbon surfactant such as C 4 H 9 0 (CH 2 CH 2 0) 25 H can be used.
  • dislocation points represent defects in the crystal structure of the metal which are present at the points where the smallest ordered crystallite units of the metal meet or corresponding irregularities in the crystal structure are present.
  • Such dislocation points have the effect that the electron gas, which is fundamentally freely movable between the metal atoms, hits interfaces which can only be overcome with additional energy supply.
  • the inventor has surprisingly found that the friction between sliding pair components can be reduced in that at least one of the components of the sliding or rolling pair is provided on its movement contact surface with the special surface loading matrix according to the invention.
  • This special surface loading matrix is formed by molecules attached to the dislocation sites of the hydrocarbon radical R f present in the fluoroorganic compound R E -V, which is partially or fully fluorinated or chlorofluorinated and can be straight-chain or branched-chain, the chain also being formed by one or more Oxygen, nitrogen or sulfur atoms can be interrupted, and the polar or dipolar group V, which enables the attachment of the molecule R f at the dislocation sites on the metal surface.
  • the inventor assumes that due to the charge differences on the surface formed by the dislocation sites between individual areas of the surface, the compounds of the formula R f -V are transferred the hydrophilic group, ie a group with dipolar or polar properties, is attached and thus "freezes" the dislocation state at the attachment point, so to speak.
  • dipole property is understood to mean that, due to the different electronegativities of the atoms present in group V, bonds are polarized and charge differences between the individual atoms, ie small positive or negative potentials, are produced on the atoms involved in the bond. Of course, such interactions can also be caused by atoms in group V with free electron pairs.
  • V is due to the fact that, in addition to the metallic substrate surfaces, it is also possible to load those surfaces which, owing to polar structures on the surface, allow the molecules of the formula R f -V to be attached.
  • Nitrogen- or boron-containing residues V in the compound R f -V are particularly preferred for increasing the surface hardness of a treated machine component, the boron-containing compounds being present as borates, for example as (R f O) 3 B.
  • the surface loading matrix is understood to mean that it is not a relatively dense continuous molecular layer of molecules of the formula R f -V that is formed on the surface, but that individual molecules are formed over the group
  • V are bound to the metallic surface in particular at a distance from one another, so that between the individual, "pile-like" pointing away from the surface non-polar Molecular residues R f individual areas of the surface free of R f molecules remain. Solid lubricant and wear particles which may arise may be embedded in these remaining free areas, so that a kind of "self-healing" of the surface loading matrix is made possible by these free areas.
  • the Me-VR f connection system is formed with the loading matrix according to the invention, in which Me is a plurality of metal atoms on the surface to which the aliphatic one is attached
  • Hydrocarbon residue R £ which is contained in the organofluorine compound according to the invention, is chemically and physically bound via the polar or dipolar group V with high binding energy.
  • OH groups which are attached to the metal atoms are reacted with H atoms contained in the polar or dipolar group V to form H 2 0 and are thereby released.
  • such an “intercalation material” should be a material with lubricant properties and preferably from the group of the lubricating oils, the solid lubricants based on carbon such as graphite, the solid lubricants based on metal sulfide such as molybdenum or antimony sulfides, the carbon cluster compounds, in particular the diamond cluster compounds or the fullerene - Cluster compounds, in particular C 30 to C 60 , the powder of metal oxides, metal nitrides, metal carbides of valve metals, in particular Ti, Ta, Zr, Hf, Co, Ni, Al, and boron nitride, in a grain size below 500 nm, preferably below 100 nm , and the compounds of the formula R f -R f , where R f stands for an aliphatic hydrocarbon radical which can be partially or completely fluorinated or chlorofluorinated and can be straight-chain or branched-chain, the hydrocarbon radical being represented by one or
  • Oxygen, nitrogen or sulfur atoms can be interrupted.
  • This storage material can also be the same or related compounds as the compounds of the formula R f -V, as long as these can be attached or incorporated due to the structure of the individual compound through interactions with the coil-like structure.
  • R f -R f is the one given above Has meaning.
  • a particularly preferred intercalation compound in the sense of the invention is a diamond-carbon cluster compound in the form of a dry powder with the following properties:
  • the clusters Due to the higher Gibbs energy, the clusters form a conglomerate with a size of 20-60 nm, and with the following further conglomeration up to 10 3 nm.
  • the size of the base cluster (actual diamond crystal) is approximately 10 to 100 angstroms.
  • the electrochemical potential of the particles is equal to - (0.3-0.4) mV for an oxidized surface and +0.15 mV for a modified surface.
  • the cluster's crystal-internal bonds are similar to those of diamonds, so extremely stable; however, clusters at the borders are chemically very active and "aggressive". Such cluster connections are known in the prior art and can be produced using known detonation methods.
  • the loading matrix according to the invention is also outstandingly suitable for storing oil, in particular motor oil.
  • the loading matrix according to the invention even because of its attachment to the dislocation and their charge states show a strong polarization, which interacts with the molecules of the intercalation material.
  • Embedded oil molecules are also polarized as a result and represent oil structures whose energy tends towards a minimal state, which is why they are divided into the finest oil droplets that are largely physically independent of the rest of the oil liquid.
  • these oil balls are bound to the loading matrix. Under the action of the electric field, the smaller the oil balls are, the more they are bound to the loading matrix.
  • the intercalation material used according to the invention is applied to the surface previously loaded with the compound R f -V in the sense of the invention simply by applying the intercalation compound as such or in suspension or solution and removing the residues visible on the surface with the naked eye, for example by wiping or Wash off applied, and the storage material is stored in the previously formed "spiral" or "ball” structures of the residues R f .
  • the surface loading of the movement contact surface according to the invention thus serves as a loading matrix for receiving the storage material.
  • the density of the generated R f matrix can be increased by increasing the density of the dislocations per unit area.
  • the surface of the machine component to be loaded can be loaded before a "microscopically roughening" surface treatment is loaded undergo, such as by mechanical processing of the surface such as grinding, rolling, microblasting, hammering, etc., possibly with subsequent smoothing.
  • the dislocation density can also be increased by physical or chemical processing of the surface.
  • the density of the generated R f matrix can be increased by increasing the density of the dislocation points: a. mechanically by shot peening, fine blasting, sandblasting or other fine removal processes; As a result, the finest mechanical material defects are generated on the surface, as a result of which the attachment points of the R f matrix occur on the surface in higher density
  • Polishing can be done. When honing, however, this should preferably be done in such a way that there is no so-called honing structure.
  • the surface can be cleaned with a solvent that may be present in the presence of impurities, and then the surface can be cleaned at a temperature above the evaporation temperature of the one used
  • Dry solvent temperature Drying before loading can be particularly important in order to remove liquid bubbles or the like which would otherwise cover the dislocation points and thereby impair or prevent the attachment of the compounds R f -V.
  • This cleaning pretreatment is particularly advantageous if the surface loading matrix made of the fluoroorganic compound R f -V is used further as a loading matrix for the storage material.
  • a solution is preferably left in which the organofluorine compound R f -V in a concentration of 0.001 to 10 wt .-% is included and which is used to generate the loading matrix for the storage material, act on the movement contact surface over a period of up to 60 minutes, preferably from 10 to 30 minutes.
  • the action can be particularly favored here if the surface is heated to a temperature above the evaporation temperature of the solvent of this solution before the solution used according to the invention is applied and the solution is applied to this heated surface. As a result, the H 2 0 fractions formed during loading are evaporated.
  • the incorporation material is introduced into the loading matrix in the form of a solution containing a solvent that is or is compatible with the solvent used to apply the loading matrix to the surface, it is often not necessary to load the loading matrix prior to insertion of the storage material to dry. Rather, in these cases, the solution containing the storage material can be applied to the movement contact surface immediately after the solution generating the loading matrix has been applied. However, it may also be advantageous here to provide a drying process before the storage material is applied in order to evaporate and thus remove remaining liquid inclusions, in particular water formed.
  • Load matrix used to dry solvent until this and the water formed are completely evaporated. Thereafter, the surface loaded with the loading matrix can be rinsed in particular with an alcoholic solvent, after which the storage material is undiluted or in
  • Solution is entered in the loading matrix.
  • the storage material or the solution containing it can be spread or sprayed onto the loading matrix.
  • the final surface load can be dried at an elevated temperature and then preserved if necessary.
  • the method for surface loading according to the invention can in principle be carried out on any machine component which has at least one movement contact surface designed as a sliding surface or rolling surface, which are suitable for the inventive attachment of the molecular chains R f -V in the sense explained above.
  • An important field of application is that of reciprocating piston machines.
  • this includes piston valves, piston spools and in particular reciprocating pumps and reciprocating motors.
  • a preferred use of the method in this field of application is for reciprocating internal combustion engines of a motor vehicle, particularly if the machine components of these engines are at least largely made of a light metal, in particular an aluminum alloy or a magnesium alloy.
  • the invention makes it possible to provide cast engine blocks made of light metal on their cylinder running surfaces formed in the casting process with the surface loading matrix according to the invention without having to first honing these cylinder running surfaces.
  • the manufacturing effort can be reduced considerably. If honing is nevertheless carried out, this should advantageously be done in such a way that no honing structure remains. By eliminating the honing structure, the subsequent loss of motor oil is reduced considerably.
  • the loading matrix can thereby be used, for example, to treat the cylinder surfaces of an engine block applied that the cylinder bores are filled with the solution or suspension of the organofluorine compound according to the invention, so that the running surfaces are at least approximately wetted over the entire surface. This is a special case of "diving" mentioned elsewhere herein. After a predetermined exposure time, the residual solution can then be suctioned off, the loading matrix can be dried after rinsing, if necessary, and the storage material can be spread on the loading matrix, for example.
  • organofluorine compound used according to the invention is to heat the organofluorine compound in a pressure vessel, for example in water under high pressure, and then to spray or spray through a spray valve onto the surface to be loaded. Due to the relaxation when dispensing the hot liquid, it evaporates, so that the molecules of the compound R f -V are hurled directly against the surface to be loaded and spread on it.
  • the invention can also be advantageously used for machine components other than cylinder blocks.
  • machine components are engine and transmission machine components, such as pistons, connecting rods, piston pins, piston rings, cylinders, crankshafts, crank pins, main bearings, crank pins, valve stems, valve guides, camshafts, valve actuators, valves, bucket tappets, synchronizer rings and the like.
  • the components interacting with one another as sliding or rolling partners are preferably both loaded on their sliding or rolling surfaces according to the invention, although in many cases it has already been successful to reduce wear by treating only one of these component partners according to the invention.
  • Examples of such component partners in motor vehicles are, in particular, piston / connecting rod bearings, piston ring / cylinder race, valve / valve guide, camshaft / cam / valve, Camshaft / bucket tappet, gear / gear, synchronizer ring / synchronizer ring and the like.
  • Another important field of application for the invention is that of screw or worm spindles or gear wheels, in particular gear wheels, as well as that of slide or roller bearings, namely the treatment according to the invention of, for example, slide bearing bushes or on rolling elements and / or races of roller bearings.
  • Loading matrix can be successfully renewed by using the fluoroorganic compound.
  • organofluorine compound of the formula R f -V it is also possible to use the organofluorine compound of the formula R f -V in those described above
  • a lubricating liquid which, as such, can be a lubricating liquid customary for this lubricating and cooling purpose.
  • oils for metalworking that are used to dissipate heat and to cool tools and
  • a loading matrix according to the invention not only forms on the work surfaces of the tool, but also on the machined surface of the workpiece. That the loading of the workpiece surface takes place during the shaping processing itself is due to the above
  • Binding and formation mechanism of the molecular chains R f formed in accordance with the invention and their binding at dislocation points on the workpiece surface via the polar or dipolar group V are significantly opposed, because during processing such dislocation points can be newly created to which further molecular chains R f are bound.
  • a carbon cluster connection in the lubricant can also be used successfully. This is preferably done in an amount of 0.001 to 5% by weight, based on the weight of the lubricating liquid containing the fluoroorganic compound.
  • the diamond cluster connections described above are particularly preferred as such a lubricant additive.
  • the fullerene cluster compounds can also be used successfully.
  • the treatment of the workpiece with the lubricant then leads to the formation of the loading matrix according to the invention, in which the carbon clusters are embedded as storage material.
  • carbon cluster compounds are preferably used together with the organofluorine compound R f -V in the lubricant, it is also successfully possible to use the carbon cluster compound, in particular the diamond cluster compound alone, without the organofluorine compound in the lubricant. This is preferably done in an amount of
  • Cluster material from 0.001 to 10% by weight, based on the weight of the lubricant.
  • lubricant in workpiece machining is not limited to the type of workpiece machining.
  • this proposal is preferably implemented in the case of fine or ultra-fine machining such as fine turning, grooving and lapping and the like as finishing (finishing).
  • This proposal according to the invention to use the fluoroorganic compound used according to the invention in a lubricating liquid during workpiece machining is preferably, but not exclusively, intended for workpieces made of, in particular, metal and metal-ceramics, plastics, CBN, silicon or other semiconductor materials, glass, but also, for example, wood.
  • Disks have special advantages adapted to this area of application.
  • the formation of the surface loading according to the invention of the optical disk, in particular coated with a metal-containing coating, with molecules R f -V in the sense of the invention results in a highly effective protective coating, which is particularly effective against scratching the coating and thus the disk, without the optical properties of the Affect the disc significantly.
  • the effectiveness of The protective covering according to the invention can, however, be significantly improved if, in one embodiment of the invention, a silicon compound or a boron compound is incorporated into the loading matrix according to the invention. This silicon or boron compound should preferably have a molecular weight of less than 2,000, more preferably from 100 to 500.
  • a particularly preferred field of application of the invention is that of the windshields, other window panes or headlight panes of vehicles, such as aircraft, watercraft or in particular motor vehicles.
  • the resulting advantages are in particular the following:
  • the hard layers which protect the “softer” plastic are themselves protected from scratching and environmental influences by the surface loading according to the invention.
  • silicate glasses are used as the optical disks loaded according to the invention, they are also better protected against wear of the applied functional layers.
  • the functional layers for example the anti-reflective layers of the lens, are protected against wear, scratching and injuries and become insensitive to severe weather and external influences.
  • the invention is preferably used in the production of the optical disk, it can also be used advantageously, e.g. be used for repair work.
  • the inventor has surprisingly also found coating processes that the adhesion between the layers of the pair of layers produced in a CVD or PVD process can be improved in that the surface of the substrate that is used in the CVD or PVD process, for example with a semiconductor material to be coated, treated with a solution of one or more compounds of the formula R f -V in a solvent, preferably a perfluorinated solvent such as Frigen, in a concentration of 0.001 to 10% by weight, optionally with the addition of an emulsifier or surfactant then coating is done in a PVD, CVD or PCVD chamber.
  • a solvent preferably a perfluorinated solvent such as Frigen
  • the inventor assumes that the molecules R f -V can be attached via the hydrophilic group, ie a group with dipolar or polar properties, due to the charge differences between individual areas of the substrate surface present on the surface and formed by the dislocation points freeze the state of dislocation at the point of attachment, so to speak, as already explained above using the example of movement contact surfaces.
  • Molecules R f -V take place via the group V on the surface, which, according to the inventor, is attributable to the polarization of the group V, apart from the metallic substrate surfaces it is also possible to load surfaces which allow the molecules of the formula R f -V to attach to the surface due to polar structures.
  • the invention is therefore also directed to a method for treating the surface of a substrate, which preferably comprises the following steps:
  • % of the organofluorine compound of the formula R f -V with an emulsifier in an amount of up to 5% by weight, based on the total weight of the aqueous solution; and optionally allowing the solution to act for a period of up to 60 minutes, preferably 2 to 30 minutes, and optionally drying the substrate at a temperature above the evaporation temperature of the solvent used for a period of time which is complete
  • Ultrasonic vibrations are applied or the solution can be brought into the boiling or cavitation state.
  • the substrate treated in this way can be introduced directly into a vapor deposition chamber and then provided with a coating which, due to the loading of the surface of the substrate with compounds of the formula R f -V, acts as an adhesion promoter shows improved adhesion as an untreated substrate.
  • the organofluorine compound R f -V before the start of the CVD, PVD or PCVD vapor deposition process under the working atmosphere and its pressure conditions which are provided for the vapor deposition process, can be introduced into the vacuum chamber in the form of the treatment agent in solution or undiluted, in particular be sprayed or injected and so form a load on the surface of the substrate. It is additionally or alternatively also possible to enter the organofluorine compound after the evaporation process under the evaporation atmosphere and its pressure conditions in the evaporation atmosphere and thereby to deposit it on the vaporized surface.
  • the inventor has also found that the organofluorine compound can be deposited alternately with the vapor deposition material used in the vapor deposition process on the previously vapor-deposited surface of the substrate.
  • the process of evaporation with the evaporation material is interrupted for a predetermined period of time and during this period the organofluorine compound according to the invention is deposited on the evaporation surface of the substrate, after which the evaporation process is continued with the evaporation material.
  • the evaporation of the evaporation material is interrupted.
  • substrates to be vapor-coated are those with a metallic, metallized or ceramic surface.
  • Suitable metals, metal alloys, which are in the vapor deposition process on a Let the substrate evaporate, especially titanium, chromium, tungsten, titanium aluminum, magnesium and the like.
  • other vapor deposition materials such as carbon fractions or boron nitride are also suitable.
  • Chemosorption of the molecules on the surface generate a kind of monomolecular loading matrix over the surface with a loading thickness of 40 to 100 angstroms.
  • the molecules of the compound of the formula R f -V adsorbed in this way form molecular chains which are perpendicular to the surface and which, owing to the steric factors (low availability of space and space), form a spiral-like structure with a kind of anchoring via group V. form on the loaded surface.
  • these spirals have a diameter of 24 to 26 angstroms, and the distance (base distance) between the spirals is approximately 26 to 35 angstroms.
  • the molecules of the formula R f -V are preferably attached and anchored primarily to the surface dislocations, which are characterized by increased electron density.
  • the compound of the formula R f -V is applied undiluted or as a liquid substance system in the form of a liquid solution or a suspension simply at atmospheric pressure at approx. 20 ° C. to the surface to be loaded, for example brushed on or sprayed on, and after approx. 5 to
  • the firmly bound mono loading matrix described above forms for 30 minutes.
  • the mono loading matrix formed in this way lowers the surface tension of a metal (eg iron) from 1800 to 5000 before the loading matrix is formed to 2 - 20 mN (milli-Newton) mN / m after loading with the fluoroorganic compound R f -V.
  • the lowering of the surface tension can also be used as a protective measure against cold welding of the sliding surfaces of two machine components interacting as sliding partners.
  • the formed loading matrix is mechanically and chemically stable and can withstand a pressure of 300 kg / mm 2 without breaking open or tearing off.
  • the temperature stability of the loading matrix is more than 450 ° C, and the compounds of the formula R f -V are non-flammable, non-toxic and easy to use.
  • the coefficients of friction of a metallic surface loaded with the compound of the formula R f -V are 0.05 to 0.1, which is approximately 10 to 15 times lower than that of an unloaded aluminum or iron alloy. As a result, wear can be reduced by up to 10 to 15 times, which makes the use of the surface loading matrix particularly attractive in precision mechanics.
  • a special feature of the surfaces loaded with the formed loading matrix which has surprisingly occurred in view of the small thickness of the loading matrix, is the increase in the microhardness of the loaded metal surfaces. Contrary to expectations, with a thin surface load that is only a few angstroms thick, the microhardness has increased by 10 to 30% to approximately 1.0 ⁇ m (micron) in the depth of the loaded metal surface.
  • indexes 55 and 10 represent the number of indexed units in a molecule
  • at a concentration of 0.05% in the solvent CF 2 C1-CFC1 2 (99.95% by weight) was used to generate a surface loading matrix with a Thickness of 50 angstroms as described above on an iron alloy Gx38CrMoV, gas nitrided with a layer thickness of the connection zone of 8-12 ⁇ m (homogeneous), layer thickness of
  • Diffusion zone 120 to 300 ⁇ m, surface hardness approx. 1100 HV1 and core hardness 520 to 670 HV10 (NHT 650 HV1 150 ⁇ m) applied.
  • the hardness of the material was increased by 10 HRc.
  • the coefficient of friction was measured at a pressure of 2311 kg force / cm and determined to be 0.09. The value remained constant at this value during a wear test over a test period of 100 hours, and the mean wear was 7.8 x 10 "5 grams / hour.
  • indices 46 and 14 represent the number of indexed units in a molecule
  • a concentration of 0.05% in the solvent perfluorocyclohexane (99.95% by weight) was used to produce a loading matrix according to the invention with a thickness of 60 angstroms as above described on a 16MnCrS 5 iron alloy, case hardened and tempered, applied to 58 + 4 HRC.
  • the hardness of the material was increased to 68 + 4 HRC.
  • the coefficient of friction was measured at a pressure of 2311 kg force / cm and found to be 0.09. The value remained constant during a wear test over a test period of 100 hours this value, and the mean wear was 8.1 x 10 "5 grams / hour.
  • Example 3 In the same way as described in Example 2, an iron alloy 17 CrNiMo6, case-hardened to 60 + 2 HRC, EHT 0.9-1.0 with core strength max. Load 1200 N / mm 2 (after hardening). This hardness is increased to approx. 67 + 2 HRC after the generation of the 55 angstrom thick loading matrix, the wear has been reduced 5 times, the friction coefficients were approx. 0.09.
  • the loads (pressure) during the test are the same as in previous examples.
  • An engine block made of an aluminum-silicon alloy (NG K AlSi9Cu3) (Si content ⁇ 13% - hypoeutectic) is washed with a solvent or an aqueous solution after drying (honing), dried and with a solution of CF 3 0- (CF 2 CF 2 0) 50 (CF 2 0) 10 CF 2 -COOH as an organofluorine compound R f -V in a concentration of 0.5% by weight in the solvent CF 2 Cl-CFCl 2 to form the loading matrix according to the invention wetted by spraying the track surface at room temperature for 2-10 minutes of the solution. The sprayed track is then dried with warm air at 50-70 ° C. for 20 minutes and then any of the above-described storage materials are rubbed onto the surface without any particular effort. A conventional engine oil is then sprayed on for corrosion protection purposes.
  • NG K AlSi9Cu3 Al content ⁇ 13% - hypoeutectic
  • Example 4 The same engine block as in Example 4 was treated with the solution shown in Table 1 under No. 7 after the engine block was cleaned with a water solution, rinsed with distilled water and dried by blowing with warm air (approx. 120 ° C. for 2 minutes) has been.
  • the treatment was carried out by spraying on the 0.5% solution No. 7 according to Table 1. After drying by blowing hot air at about 120 ° C. for 2 minutes, the following storage compound was placed on the loading matrix thus produced on the track area
  • the engine already showed the consumption values after 5 hours, which normally only occur after at least 10-30 hours; The running-in was therefore quicker and the friction power values stabilized faster.
  • the engine was then operated with a full test program during 400 hours of full load operation and then tested by repeated measurements; all values have remained stable, the friction has increased by about 4 to 5% depending on the speed, and the oil consumption has remained extremely low.
  • the engine was allowed to continue running until 1000 operating hours were reached, the oil changes were carried out as usual at fixed intervals so that the operating conditions were brought as close as possible to the normal condition.
  • the real situations were simulated that could occur during normal operation of the engine.
  • the engine has shown very little blow-by, very low fuel consumption and very favorable other usage-related values, so that it can be assumed that further successful use is also possible.
  • the career was examined and found to be smooth and injury-free.
  • Example 6 The same engine block as in Examples 4 and 5 was used, but with a gray cast iron bush made of GGGZ-25 with a hardness of 220 to 260 HB. This liner was treated as in Example 2. In addition to increasing wear resistance, another effect has been shown:
  • a gearbox was treated by treating the friction-loaded components with a 0.6% solution of the connection:
  • Example 8 The inner cage made of the material SAE 8617H and the
  • a gray cast iron camshaft was treated according to the treatment pattern from Example 2 by immersion in solution No. 6 from Table 1.
  • the frictional power losses compared to an untreated camshaft were reduced by approx. 20 to 35% after the treatment.
  • the same result was achieved when only the tappets were treated. It can therefore be assumed that it can in principle be sufficient to treat only one of the two interacting component partners in order to achieve the desired treatment result.
  • Example 10
  • a motor-cylinder tread made of an aluminum-silicon alloy (NG K AlSi9Cu3) was heated to a temperature of about 70 ° C with a loading matrix according to the invention from the compound R f -V in the form of
  • CF 3 0 (-CFCF 2 0-) 55 (CF 2 0) 10 CF 2 CO-NH 2 CF 3 smeared in undiluted form at approx. 70 - 120 ° C on the loaded track.
  • CF 3 0 (-CFCF 2 0-) 46 (CF 2 0) 14 CFO-CF 2 -CO-N (CH 3 ) 2 CF 3 CF 3 can be used.
  • An oily oil can be used as a preservative oil instead of motor oil
  • Polyoxide-ethylene can be used.
  • Example 5 The effects indicated in Example 5 also occurred here. After about 400 hours of operation, the ppm content of aluminum in the oil has changed only slightly. This indicates that the state of wear has largely stabilized.
  • an electrolyte is filled with the composition (i):
  • the electrolyte temperature (at start) was approx. 15 ° C; one worked with successive positive and negative current pulses with a duration of 200 ms and with a frequency of 50 Hz between the positive and negative pulses at a voltage of 500 V, and a pause of 200 ms between the successive pulses; the current density at the cylinder surface was 45 A / dm; the ratio of anode current to cathode current was 1.07: 2.0;
  • Process time was 30 minutes. A layer thickness of 20 ⁇ m has resulted. The surface was then rinsed with deionized water and dried. The oxidized surface was then treated with the solution of the active substance
  • the roughness of the raceway thus finished was approximately 0.3 ⁇ m.
  • the engine with the raceway treated in the above manner was tested for friction and consumption in the usual running test under normal conditions (running-in time 20 hours). An improvement in the friction performance compared to an engine block with a gray cast iron bushing of between 5 and 7% was found, depending on the speed. After a further 500 hours of operation, no failure criteria regarding oil consumption or compression reduction were found.
  • HSS tool saw, milling cutter
  • work surfaces dipped in a 0.5% by weight solution with the active substance:
  • the active substance was used in a concentration of 0.5% in the solvent CF 2 C1-CFC1 2 (99.5% by weight) to produce a loading matrix with a thickness of 40 angstroms on the anti-reflective layer.
  • indices 46 and 14 indicate the number of indexed units in a molecule.
  • the active substance was applied as a solution in a concentration of 0.5% in the solvent perfluorocyclohexane (99.5% by weight) to produce a loading matrix with a thickness of 60 angstroms. After generating the loading matrix of 60 angstroms, such a microhardness of the functional work surfaces made of CBN was measured, which surprisingly approx. Was 10% higher than before treatment.
  • the wear resistance was 3 to 7 times higher and the cutting forces during machining by hard turning on high-alloy steels have surprisingly decreased by 20 to 40%.
  • the tool life of the HSS, carbide and CBN tools used was increased by a factor of 2 to 7;
  • the roughness of the workpieces produced was 2 to 3 times less than the cutting process, in which no active substance was used;
  • the cutting forces of the machine tools are approx. 20 to 45% decreased, which has been shown by a corresponding decrease in the current consumption.
  • a substrate in the form of an optical lens is prepared by applying an anti-reflective coating on the glass surface is applied; immediately after coating, the active substance becomes:
  • indexes 55 and 10 denote the number of indexed units in a molecule, in a concentration of 0.01% in the solvent CF 2 C1-CFC1 2 (99.99% by weight) to produce a loading matrix according to the invention with a thickness of 40 angstroms applied to the anti-reflective coating.
  • the anti-reflective coatings showed no change in light transmission and, after a wear test, showed a 3 to 5 times longer service life of the coating.
  • the surface provided with the loading matrix has become significantly dust-repellent and easier to clean.
  • indices 46 and 14 represent the number of indexed units in a molecule, treated at a concentration of 0.01% in the solvent perfluorocyclohexane (99.99% by weight) to produce a loading matrix according to the invention with a thickness of 60 angstroms.
  • the microhardness of the functional coating was measured, which was surprisingly about 10% higher than in the state before the treatment. Also were Surprisingly improved properties of the finished windshield with regard to wear resistance and dirt repellency were found.
  • a semi-transparent glass plate with an anti-reflective layer was used. After the metal oxide layer had been produced, the glass plate was additionally dissolved in a solution of the active substance:
  • the surface of the plate has shown a strong dirt-repellent effect.
  • Connection R f -V can be seen from the attached table.
  • Example 18 a Cleaning the workpiece before coating as usual, in water solution, alkaline or acidic or in a solvent,
  • the workpiece is immersed in the solution for 5-10 minutes and then, possibly even without drying, conveyed into the vacuum chamber.
  • the treatment agent can also be in this solution during the evaporation process
  • Vacuum conditions are sprayed into the working atmosphere if additional support of the process by spraying is required or desired.
  • This active substance is diluted in a concentration of 0.3% by weight with the abovementioned solvent and is left to act on the workpiece for about 0.5 to 10 minutes.
  • the process can be supplemented by spraying the treatment agent during, before or after the coating, that is: after the substrate (workpiece) is plasma cleaned, the opening is made in the vacuum chamber
  • Sprayed treatment agent so that it encases the workpiece from all sides; this process can be repeated at a time interval of 1 to 10 minutes at least once in the evaporation process (step f.) after its interruption, so that the layers of evaporation material and the organofluorine compound according to the invention as a multilayer composite layer on the functional surface of the to be coated Part of the substrate are built.
  • the spraying process can additionally or alternatively also be carried out as the last step after the vapor deposition process.
  • Base substrate is significantly increased; the roughness of the TiN layer is reduced by approximately 20 to 40%; the material density of the layer is increased by approximately 20-40%, especially in the border area in which the layer is bound to the workpiece surface.
  • the adhesive strength of the TiCN layer produced on the base substrate is significantly increased; the roughness of the TiN layer is reduced by approximately 20 to 30%; the material density of the layer is increased by approximately 20-30%, especially in the border area in which the layer is bound to the workpiece surface.
  • the TiAlN layer produced has a significantly higher adhesion to the base substrate; the roughness of the TiN layer is reduced by approx. 30 to 40%; the material density of the layer is increased by approximately 30%, especially in the border area in which the layer is bound to the workpiece surface. These effects apply to both the arc and magnetron PVD process and the CVD process. Subsequent spraying of the layers produced reduces the coefficient of friction of the entire coating up to a coefficient of friction of 0.08 and increases the hardness by approx. 5%.

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Abstract

L'invention concerne des surfaces industrielles, notamment en métal ou en métallo-céramique, chargées d'un composé fluoro-organique. Un reste d'hydrocarbure, partiellement fluoré ou chloré, est fixé par addition de façon sélective à des imperfections de la surface par un groupe polaire ou bipolaire, ce qui améliore nettement les propriétés de la surface, notamment ses propriétés d'usure et de résistance. Ainsi, le frottement par glissement et roulement, par exemple, est considérablement réduit. Cette invention s'adapte à toutes les surfaces de glissement et de roulement des pièces de machines notamment d'un véhicule. Un domaine d'application préféré est la charge des surfaces de roulement d'un cylindre de moteur en métal léger, tel qu'en alliage d'aluminium. La charge de surfaces de travail et de surfaces opérationnelles d'outils de déformation mécanique, la charge de surfaces, contenant un métal, de disques optiques et l'utilisation du composé fluoro-organique dans des procédés de revêtement au plasma représentent d'autres domaines d'application.
PCT/DE1999/001133 1998-04-15 1999-04-15 Surfaces industrielles, notamment en metal ou en metallo-ceramique, chargees d'un compose fluoro-organique WO1999054060A2 (fr)

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Application Number Priority Date Filing Date Title
AU44967/99A AU4496799A (en) 1998-04-15 1999-04-15 Loading especially metallic or metal-ceramic technical surfaces with a fluoro-organic compound

Applications Claiming Priority (14)

Application Number Priority Date Filing Date Title
DE19816710.5 1998-04-15
DE19816710 1998-04-15
DE19816868.3 1998-04-16
DE19816868 1998-04-16
DE19830166.9 1998-07-06
DE19830166 1998-07-06
DE19848614A DE19848614A1 (de) 1998-04-15 1998-10-21 Beladen der Arbeitsoberflächen mechanischer Verformungs-Werkzeuge mit einer fluororganischen Verbindung
DE19848591.3 1998-10-21
DE19848591A DE19848591A1 (de) 1998-04-15 1998-10-21 Beladen einer optischen Scheibe mit einer fluororganischen Verbindung
DE19848613.8 1998-10-21
DE19848611A DE19848611A1 (de) 1998-04-15 1998-10-21 Oberflächenbehandlungsmittel und Verfahren zum Behandeln von Substratoberflächen sowie Verwendung des Behandlungsmittels in Beschichtungsverfahren
DE19848613A DE19848613A1 (de) 1998-04-15 1998-10-21 Beladen von metallischen oder metallkeramischen Gleit- und Wälzoberflächen mit einer fluororganischen Verbindung
DE19848614.6 1998-10-21
DE19848611.1 1998-10-21

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WO1994021386A2 (fr) * 1993-03-25 1994-09-29 Research Corporation Technologies, Inc. Polymeres utiles pour la formation de couches ultra-minces anisotropes collees auto-assemblees et leur utilisation
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EP0003071A1 (fr) * 1978-01-05 1979-07-25 International Business Machines Corporation Procédé de préparation de films de polymères
EP0501298A2 (fr) * 1991-02-27 1992-09-02 Matsushita Electric Industrial Co., Ltd. Dispositif autolubrifiant
WO1994021386A2 (fr) * 1993-03-25 1994-09-29 Research Corporation Technologies, Inc. Polymeres utiles pour la formation de couches ultra-minces anisotropes collees auto-assemblees et leur utilisation
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US20220025490A1 (en) * 2018-09-19 2022-01-27 Sumitomo Electric Industries, Ltd. Method of producing cubic boron nitride sintered material, cubic boron nitride sintered material, and cutting tool including cubic boron nitride sintered material
US12054813B2 (en) * 2018-09-19 2024-08-06 Sumitomo Electric Industries, Ltd. Method of producing cubic boron nitride sintered material, cubic boron nitride sintered material, and cutting tool including cubic boron nitride sintered material

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