EP1738000B1 - Herstellung einer strukturierten hartchromschicht und herstellung einer beschichtung - Google Patents

Herstellung einer strukturierten hartchromschicht und herstellung einer beschichtung Download PDF

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Publication number
EP1738000B1
EP1738000B1 EP05700700.7A EP05700700A EP1738000B1 EP 1738000 B1 EP1738000 B1 EP 1738000B1 EP 05700700 A EP05700700 A EP 05700700A EP 1738000 B1 EP1738000 B1 EP 1738000B1
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EP
European Patent Office
Prior art keywords
layer
structured
chromium layer
workpiece
structured hard
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Not-in-force
Application number
EP05700700.7A
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German (de)
English (en)
French (fr)
Other versions
EP1738000A2 (de
Inventor
Rudolf Linde
Stefan Dürdoth
Wolfgang Stuckert
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Federal Mogul Burscheid GmbH
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Federal Mogul Burscheid GmbH
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
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Publication of EP1738000A2 publication Critical patent/EP1738000A2/de
Application granted granted Critical
Publication of EP1738000B1 publication Critical patent/EP1738000B1/de
Not-in-force legal-status Critical Current
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/04—Electroplating: Baths therefor from solutions of chromium
    • C25D3/10—Electroplating: Baths therefor from solutions of chromium characterised by the organic bath constituents used
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/10—Electroplating with more than one layer of the same or of different metals
    • C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/627—Electroplating characterised by the visual appearance of the layers, e.g. colour, brightness or mat appearance

Definitions

  • the invention relates to a method for producing a structured hard chrome layer on a workpiece, a method for producing a coating with a structured hard chrome layer, structured hard chrome layers and coatings obtainable thereby, and an electrolyte for carrying out the method.
  • Electrochemically produced hard chrome coatings are not only used for decorative finishing of surfaces. Rather, hard chrome layers are also applied as functional coatings on conductive and non-conductive workpieces, for example, to exercise a protective function or to influence the surface properties low. Typical applications are therefore protective coatings of hard chrome to reduce corrosion, wear or friction, and structured hard chrome layers on printing rollers to facilitate the wetting with printing inks or on stamping, embossing and thermoforming tools to optimize manufacturing processes in the industry.
  • EP 0 196 053 A2 and DE 34 02 554 A1 describe in each case processes for the electrodeposition of hard chromium on metallic surfaces from an aqueous, chromic acid, sulfuric acid or sulfate and a sulfonic acid-containing electrolyte, wherein working with cathodic current efficiencies ⁇ 20%. Due to the composition of the electrolyte, the risk of disruptive etching of the surface to be coated should be excluded. However, no structures are created in the hard chrome layer.
  • GB 2 153 387 A1 describes a method for depositing hard chrome on workpieces of metal alloys from an aqueous electrolyte wherein the electrolyte contains chromic acid and sulfuric acid and an organic compound is added in the form of a saturated aliphatic sulfonic acid having a maximum of two carbon atoms and a maximum of six sulfonic acid groups their salts or halogen derivatives and the process is carried out with a concentration of more than 0.5 g / l of the organic substance, at a bath temperature of 20 ° - 70 ° C and a current density of 15 - 100 A / dm second
  • An electrochemical process for producing structured hard chrome layers is known, for example, from US Pat DE 44 32 512 A1 known.
  • the structure of the hard chrome layer is made possible by the addition of salts, such as salts of the elements selenium or tellurium, to the electrolyte.
  • the layers produced have a spherical structure with spherical shapes of a size between less than 1 micron and several microns. This results in a often non-uniform spherical structure of the hard chrome layer, which is not suitable for all applications.
  • the object of the invention is therefore to provide a method for producing a structured hard chrome layer, with which the disadvantages of the prior art are overcome.
  • structured hard chrome layers are produced, which are of cup-shaped and / or labyrinth-like and / or columnar design. This is achieved by a specific influencing of the cathode film forming during the electrochemical deposition, which will be explained below.
  • the electrolytes used in galvanic processes contain salts which dissociate into anions and cations in the aqueous medium.
  • a hydration shell forms around the dissociated ions.
  • hydrated metal ions of the electrolyte migrate to the workpiece to be coated, which is connected as a cathode.
  • cathode film In the boundary region between the electrolyte and cathode directly on the surface of the cathode is the so-called cathode film.
  • a hydrated metal ion enters this phase boundary, it picks up electrons from the cathode and thereby aligns in the diffusion zone.
  • Helmholtz double layer Under this diffusion zone and directly on the cathode surface is formed an electrochemical double layer, the "Helmholtz double layer". This consists of an electrically charged zone at the electrolyte-cathode interface and is about a few atomic or molecular layers thick. Their formation involves ions, electrons or directed dipole molecules. Since the "Helmholtz double layer" is positively charged on one side and negatively charged on the other side, it behaves on the cathode like a plate capacitor with a very small plate spacing.
  • the metal ion In order for the metal ion to get onto the workpiece surface and be incorporated into a growth site on the surface of the workpiece, it must overcome the cathode film.
  • This process can be influenced by a suitable choice of deposition conditions, such as chemical composition of the electrolyte, temperature, hydrodynamics and electric current.
  • the deposition conditions for the electrolyte are selected so that the transmissivity of the cathode film for the metal ion is as uniform as possible.
  • chromium When the element chromium is to be deposited from an aqueous electrolyte on a workpiece, it is in strongly acidic solution as a negatively charged hydrodichromate complex.
  • chromium has the oxidation state 6, although small amounts of chromium (III) compounds may be included.
  • an electrolyte with a chromium (VI) compound in an amount corresponding to 50 to 300 g / l, preferably 50 to 150 g / l, chromic anhydride, 0.5 to 10 g / l sulfuric acid and 5 g / 1 to 15 g / l of aliphatic sulfonic acid having 1 to 6 carbon atoms to form a cathode film having a very dense barrier layer.
  • the barrier layer will strike, resulting in the formation of a layer of chromium of uneven thickness on the workpiece, operating at a cathodic current efficiency of 12% or less.
  • the cathodic current efficiency of 12% or less ensures the formation of the structured hard chrome layer in the method according to the invention, since structuring of the hard chrome layer is not obtained with a higher current efficiency.
  • the structured hard chrome layers produced by the method according to the invention are more uniform than the structured hard chrome layers of the prior art because of the cup-shaped and / or labyrinth-like and / or columnar structure.
  • Structured hard chrome layers obtainable by the process according to the invention are best suited for coating piston rings, in particular those of internal combustion engines.
  • layers produced according to the invention also have outstanding tribological properties, such as good sliding properties and wear and scuffing resistance, in particular in the case of insufficient lubrication.
  • the hard chrome layers obtained according to the invention can be used for many decorative and functional applications.
  • the surface topography of the hard chrome layers produced according to the invention makes it possible, for example, for a high absorption capacity for light and heat radiation when using solar collectors. Furthermore, the special structure of the hard chrome layers according to the invention allows a better absorption capacity for liquids. Also, gas cushions can be well constructed on the textured surface.
  • component (a) ie the Cr (VI) compound, CrO 3 is preferably used, since it is particularly suitable for the electrodeposition.
  • component (c) i.
  • aliphatic sulfonic acid methanesulfonic acid, ethanesulfonic acid, methanedisulfonic acid, or ethanedisulfonic acid are preferably used, which has proven to be particularly favorable for the formation of the advantageous decorative and functional properties of the hard chromium layer produced.
  • the electrolyte may in one embodiment be substantially free of fluorides.
  • the latter often complicate the formation of the structured hard chrome layer. Therefore, only as many fluorides in the electrolyte are tolerable that do not affect the deposition of the structured hard chrome layer. It has proven to be favorable if not more than 0.1 g / l fluorides are present in the electrolyte.
  • conventional catalysts for the separation of chromium such as SO 4 2- and / or Cl - , may be present in the electrolyte in conventional amounts.
  • structured hard chrome layers are deposited on workpieces by the method described above.
  • the term "workpiece” means metallic or non-metallic objects which are to be provided with a structured hard chrome layer.
  • a non-metallic article it is coated with a thin metal film prior to application of the patterned hard chromium layer to render it electrically conductive.
  • the structured hard chrome layer on the workpiece In order to deposit the structured hard chrome layer on the workpiece, the latter is connected as a cathode and immersed in the electrolyte. Then a DC current is applied to the workpiece, e.g. a pulsating direct current with a frequency up to 1000 Hz, applied. During the deposition of the chromium, the temperature is maintained at 45 ° C to 95 ° C, preferably 55 ° C. The longer the deposition is carried out, the greater the layer thickness of the hard chrome layer.
  • a DC current e.g. a pulsating direct current with a frequency up to 1000 Hz
  • the method according to the invention can be used with a current density of 20 A / dm 2 to 200 A / dm 2 .
  • This range of current density leads to the deposition of particularly favorable structured hard chrome layers. The higher the current density is chosen, the denser the protruding areas of the surface of the hard chrome layer according to the invention.
  • a second layer is deposited before and / or after the deposition of the structured hard chromium layer.
  • several layers can be applied to the workpiece, for example a metal layer of a conventional electrolyte on the structured hard chromium layer according to the invention.
  • the two layers may be made of different materials, and when a conventional metal layer is applied to the patterned hard chrome layer, improved anchoring of the conventional metal layer is enabled.
  • a conventional hard chromium layer or a structured hard chromium layer according to the invention can be deposited in each case with inclusions, wherein the inclusions can consist of aluminum oxide, diamond and / or boron nitride of the hexagonal type. In the electrolyte used for these materials are suspended. The deposits lead to a further improvement of the tribological properties.
  • a hard chromium layer according to the invention is applied electrolytically to a conventional hard chrome layer of uniform layer thickness.
  • the invention also relates to a method for producing a coating, wherein chromium is deposited on a workpiece to form a structured hard chrome layer, and to the structured hard chrome layer is applied a composition containing epoxy resin, a solid lubricant, a hard material or mixtures thereof.
  • the structured hard chrome layer may be a structured hard chrome layer produced according to the invention.
  • the epoxy resin serves as a binder to hold the solid lubricant and / or the hard material in the recesses of the patterned hard chrome layer.
  • As a solid lubricant in particular MoS 2 boron nitride, preferably the hexagonal type of boron nitride, or Teflon, or a mixture of two or more of these substances is suitable.
  • hard materials are microscale diamond, alumina, Si 3 N 4 , B 4 C, SiC or a mixture of two or more of these substances.
  • This coating construction not only improves the general wear properties, but also provides excellent runflat properties when MoS 2 is used of the workpiece in case of insufficient lubrication.
  • boron nitride is included in the composition, there is an excellent self-lubrication of the coating so that it can be dispensed depending on the application on the use of other lubricants. If a mixture of two or more of said solid lubricants is used in the composition which is applied to the structured hard chrome layer, the favorable tribological properties mentioned above add up.
  • the invention further comprises a structured hard chrome layer as obtainable by one of the above methods.
  • the invention relates to a coating obtainable by the above process for producing a coating.
  • the electrolyte which may preferably contain the Cr (VI) compound in an amount corresponding to 50 to 150 g / l of chromic anhydride, serves in particular for the electrodeposition of the structured hard chrome layers described in greater detail above on workpieces.
  • FIGS. 1 to 10 show photographs of the hard chrome layers of Examples 1 to 4.
  • the product to be coated is immersed in the electrolyte after a standard pretreatment. At 55 ° C., chromium is deposited on the product part for 30 minutes at a current density of 40 A / dm 2 .
  • the resulting article has a conventional glossy and uniform chrome layer, as in Fig. 1 shown.
  • an electrolyte according to the invention which contains: chromic anhydride CrO 3 200 g / l sulfuric acid H 2 SO 4 3 g / l methane CH 3 SO 3 H (70% pure) 9 ml / l.
  • chromic anhydride CrO 3 200 g / l sulfuric acid H 2 SO 4 3 g / l methane CH 3 SO 3 H 70% pure
  • structured hard chrome layers according to the invention are deposited on workpieces.
  • the current densities are varied as follows: Fig. 2 : 30 A / dm 2 ; Fig. 3 : 40 A / dm 2 ; Fig.
  • Conventional hard chrome layers with deposits of aluminum oxide and structured hard chrome layers according to the invention are alternately deposited on a product part.
  • an electrolyte is used which chromic anhydride CrO 3 100 g / l sulfuric acid H 2 SO 4 3.5 g / l methane CH 3 SO 3 H (70% pure) 6 ml / l contains.
  • the structured hard chrome layers are deposited at a temperature of 60 ° C., a cathodic current efficiency of 10% and a current density of 80 A / dm 2 for 30 minutes. In total, six layers are applied alternately with and without deposits.
  • Fig. 7 and 8th show a typical cross-section of these graded structured chromium layers in different magnifications.
  • the corrosion protection is ensured by the conventional hard chrome layers, while the favorable tribological properties result from the structured hard chrome layers according to the invention.
  • diamond or hexagonal boron nitride can also be incorporated.
  • the resulting graded structured hard chrome layers can be further treated as described in Example 4 to aid the self-lubricating properties of the surface.
  • a patterned hard chrome layer according to the invention produced on a workpiece according to Example 2 the structural valleys or depressions of the surface are filled with a mixture of epoxy resin and boron nitride of the hexagonal type.
  • the photographs of Fig. 9 and 10 illustrate the filling of the recesses of the hard chrome layer.
  • the resulting coating has excellent self-lubricating properties.
  • the additional use of other lubricants can be dispensed with.
  • a workpiece covered with a patterned hard chrome layer prepared according to Example 2 is treated with a mixture of epoxy resin and MoS 2 so that the recesses of the chromium layer are filled with the mixture.
  • the epoxy resin serves as a binder to fix the MoS 2 in the depressions and in part also on the elevations. This results in good wear properties, as well as excellent emergency running properties when a lack of lubrication of the workpiece occurs.
  • an improved corrosion behavior is given.
  • the wells of a patterned hard chrome layer produced on a product part according to Example 2 are filled with a mixture of epoxy resin and microscale diamond, ie diamond granules with a size in the micron range.
  • a mixture of epoxy resin and microscale diamond, ie diamond granules with a size in the micron range are filled with a mixture of epoxy resin and microscale diamond, ie diamond granules with a size in the micron range.
  • a workpiece produced according to Example 5 is additionally treated with a mixture of Example 6.
  • the resulting coating has greatly improved tribological properties, as compared to Examples 5 and 6, e.g. excellent self-lubrication, as well as compared to the untreated structured hard chrome layer more favorable corrosion behavior.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Electroplating Methods And Accessories (AREA)
EP05700700.7A 2004-04-21 2005-01-05 Herstellung einer strukturierten hartchromschicht und herstellung einer beschichtung Not-in-force EP1738000B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102004019370A DE102004019370B3 (de) 2004-04-21 2004-04-21 Herstellung einer strukturierten Hartchromschicht und Herstellung einer Beschichtung
PCT/EP2005/000037 WO2005108648A2 (de) 2004-04-21 2005-01-05 Herstellung einer strukturierten hartchromschicht und herstellung einer beschichtung

Publications (2)

Publication Number Publication Date
EP1738000A2 EP1738000A2 (de) 2007-01-03
EP1738000B1 true EP1738000B1 (de) 2018-04-18

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EP05700700.7A Not-in-force EP1738000B1 (de) 2004-04-21 2005-01-05 Herstellung einer strukturierten hartchromschicht und herstellung einer beschichtung

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Country Link
US (1) US8110087B2 (pt)
EP (1) EP1738000B1 (pt)
JP (1) JP4542134B2 (pt)
BR (1) BRPI0506445B1 (pt)
DE (1) DE102004019370B3 (pt)
PT (1) PT1738000T (pt)
WO (1) WO2005108648A2 (pt)

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DE102007038188B4 (de) * 2007-08-13 2018-11-15 Federal-Mogul Burscheid Gmbh Verschleißfest beschichteter Kolbenring und Verfahren zu dessen Herstellung
DE102008017270B3 (de) * 2008-04-04 2009-06-04 Federal-Mogul Burscheid Gmbh Strukturierte Chrom-Feststoffpartikel-Schicht und Verfahren zu deren Herstellung sowie beschichtetes Maschinenelement
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DE102011084051B4 (de) * 2011-10-05 2020-03-12 Federal-Mogul Burscheid Gmbh Beschichteter Kolbenring mit radial zunehmender Schichtdicke und Verfahren zu dessen Herstellung
DE102011084052B4 (de) 2011-10-05 2024-05-29 Federal-Mogul Burscheid Gmbh Beschichteter Kolbenring mit scharfer Ölabstreifkante
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Also Published As

Publication number Publication date
WO2005108648A3 (de) 2006-03-30
JP4542134B2 (ja) 2010-09-08
PT1738000T (pt) 2018-07-03
BRPI0506445B1 (pt) 2015-04-14
JP2007533852A (ja) 2007-11-22
DE102004019370B3 (de) 2005-09-01
EP1738000A2 (de) 2007-01-03
BRPI0506445A (pt) 2006-12-26
US8110087B2 (en) 2012-02-07
US20080060945A1 (en) 2008-03-13
WO2005108648A2 (de) 2005-11-17

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