EP1682697A2 - Revetement de substrats - Google Patents

Revetement de substrats

Info

Publication number
EP1682697A2
EP1682697A2 EP04798168A EP04798168A EP1682697A2 EP 1682697 A2 EP1682697 A2 EP 1682697A2 EP 04798168 A EP04798168 A EP 04798168A EP 04798168 A EP04798168 A EP 04798168A EP 1682697 A2 EP1682697 A2 EP 1682697A2
Authority
EP
European Patent Office
Prior art keywords
layer
substrate
aluminum
coated
heat treatment
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP04798168A
Other languages
German (de)
English (en)
Inventor
Jörg HELLER
Christoph Strobel
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.)
Aluminal Oberflachentechnik GmbH
Original Assignee
Aluminal Oberflachentechnik 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.)
Filing date
Publication date
Priority claimed from EP03026218A external-priority patent/EP1533401A1/fr
Application filed by Aluminal Oberflachentechnik GmbH filed Critical Aluminal Oberflachentechnik GmbH
Priority to EP04798168A priority Critical patent/EP1682697A2/fr
Publication of EP1682697A2 publication Critical patent/EP1682697A2/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • C25D5/50—After-treatment of electroplated surfaces by heat-treatment

Definitions

  • the present invention relates to a coated workpiece, which has an improved temperature resistance, and the provision of a method for its production.
  • Alloys that have a low density in combination with high strength and mechanical strength only have a certain temperature resistance.
  • the maximum temperature at which the workpiece is not adversely affected is approximately 500 ° C. If the temperature exceeds this value, the workpiece made of titanium or the titanium alloy is oxidized. The workpiece becomes unusable.
  • This oxidative degradation takes place not only in titanium or titanium alloys, but also in all other workpieces made of z.
  • B a chrome steel, a chrome-nickel alloy or a nickel-based alloy. Only the temperature at which the oxidation begins to differ is different.
  • the aluminum layer applied to the titanium workpiece is heated to a temperature which enables an intermetallic phase to be obtained from the originally existing aluminum layer with the workpiece made of titanium or a titanium alloy underneath.
  • This alloy layer shows an increased temperature resistance of approx. 650 - 700 ° C. Since the surface layer formed in this way is very hard and brittle, it is not possible to mechanically deform such a workpiece in a subsequent treatment step. The temperature-stable surface layer would immediately be damaged.
  • WO 02/058923 proposes to apply an aluminum layer to a titanium sheet by roll cladding.
  • roll cladding a thin aluminum foil is applied to a titanium sheet or a titanium foil at a high temperature of approx. 500 ° C. Due to the high processing temperatures, the aluminum layer adheres to the titanium sheet. Subsequently, molded parts can be produced from the titanium sheet treated in this way, which are thermally treated in a subsequent processing step.
  • this thermal treatment forms a corrosion protection layer, which consists of a titanium / aluminum alloy. By exposing this surface layer to oxygen, it is converted into a titanium-aluminum mixed oxide layer.
  • a disadvantage of the method described in WO 02/058923 is that if the titanium sheet is to be provided with an aluminum layer on both sides, this aluminum layer must also be applied to the titanium sheet on both sides. This requires a very high level of operational expenditure, since either a second station in the roll plating system must be available, with which a second aluminum layer can be applied, or it is necessary for the titanium sheet to pass through the roll plating system twice.
  • Another disadvantage of the described method is that only sheets or foils can be provided with an aluminum layer in order to subsequently produce molded components from these sheets. It is not possible to provide a three-dimensional workpiece with an aluminum layer by roll cladding.
  • a layer is applied to a titanium substrate, which has the composition MCrAL or MCr, where M is a metal selected from the group consisting of iron, nickel, cobalt and mixtures thereof.
  • M is a metal selected from the group consisting of iron, nickel, cobalt and mixtures thereof.
  • These alloys are applied to the titanium substrate by very complex processes, such as. B. plasma spraying, chemical vapor deposition or physical vapor deposition. Above all, it can be seen that these processes result in an only thin metal layer in the case of angled workpieces in hard-to-reach places. It is precisely at these points that the surface layer is particularly thin, which should guarantee the temperature stability of the workpiece.
  • the present invention thus has as its object to overcome the disadvantages of the prior art.
  • the technical object of the present invention is in particular the provision of a coated workpiece, which has superior high-temperature resistance, and the provision of a method for producing the coated workpieces.
  • geometrically complex and large workpieces are to be provided with a protective layer which is distributed homogeneously on the workpiece. The method used for this should be easier to carry out and less expensive.
  • the technical object of the present invention is achieved by a method for producing coated workpieces comprising the steps:
  • the substrate of step a) is electrically conductive. It is further preferred that the substrate of step a) is a metallic substrate and / or a metallized substrate.
  • the metallic substrate and / or metallized substrate can contain one or more metals, which are preferably transition metals.
  • the substrate is selected from the group of substrates containing the metals magnesium, zinc, tin, titanium, iron, nickel, chromium, vanadium, tungsten, molybdenum, manganese, cobalt and mixtures thereof and / or alloys thereof.
  • Preferred substrates include substrates. tend titanium, titanium alloys, chrome-nickel steel, chrome-nickel alloys, and / or nickel-based alloys.
  • the electrodeposition of the layer (s) (step a) can be carried out using any galvanic method known to the person skilled in the art.
  • the layer which is applied in step a) can be applied from a non-aqueous electrolyte or from an aqueous electrolyte.
  • the layer of step a) is preferably selected from aluminum, magnesium, tin and mixtures thereof and / or alloys thereof.
  • the layer preferably contains an aluminum / magnesium alloy and / or an aluminum / tin alloy.
  • the layer (intermediate layer) first applied to the substrate preferably contains metals selected from the group consisting of iron, iron and nickel, tin and nickel, nickel, cobalt, copper, chromium , Molybdenum, vanadium or alloys of the above metals.
  • One or more intermediate layers can be applied to the substrate.
  • the outer layer selected from aluminum, magnesium, tin and mixtures thereof and / or alloys thereof is then applied to the intermediate layer.
  • the outer layer preferably contains an aluminum / magnesium alloy and / or an aluminum / tin alloy
  • the layer or the outer layers of a layer structure contains an aluminum / magnesium alloy, it is preferred that the layer 1-80% by weight magnesium, more preferably 2-50% by weight magnesium, more preferably contains 3 to 40% by weight of magnesium and most preferably 4 to 30% by weight of magnesium. If the layer or the outer layers of a layer structure contains an aluminum / tin alloy, it is preferred that the layer 1-80% by weight of tin, more preferably 2-50% by weight of tin, even further preferably contains 3 to 30% by weight of tin and most preferably 4 to 25% by weight of tin.
  • Each layer applied in step a) preferably has a layer thickness of 0.1 ⁇ m - 100 ⁇ m.
  • the layer thickness is 0.5 ⁇ m to 70 ⁇ m, more preferably 1 ⁇ m - 50 ⁇ m, preferably 2 ⁇ m - 40 ⁇ m, more preferably 3 ⁇ m - 30 ⁇ m, more preferably 4 ⁇ m - 28 ⁇ m and most preferred 5 ⁇ m - 25 ⁇ m.
  • the layer or one of the layers of step a) is electrodeposited from an aqueous electrolyte
  • solutions of the aforementioned metals can be used as possible electrolytes.
  • the metals can be present as halides, sulfates, sulfonates or fluoroborates.
  • the electrolytes can contain other additives, such as. B. complexing substances.
  • the layer or one of the layers of step a) is electrodeposited from non-aqueous electrolytes, it is possible to use all non-aqueous electrolytes which are known to the person skilled in the art.
  • Possible electrolytes contain compounds of the above-mentioned metals.
  • the metals are preferably in the form of halides which can be complexed with ether, in particular diethyl ether. However, it is also possible for the metals to be present as acetyl acetonates (acac).
  • step a) it is possible in step a) for a layer if it is a
  • Layer containing aluminum / magnesium, aluminum or a layer containing aluminum / tin is to use any electrolyte that is known to the person skilled in the art.
  • the electrolyte preferably contains organoaluminum compounds of the general formulas (I) and (II):
  • n 0 or 1
  • M is sodium or potassium and R 1 , R 2 , R 3 , R 4 may be the same or different, wherein R 1 , R 2 , R 3 , R 4 is a C 1 -C 4 alkyl group are and a halogen-free, aprotic solvent is used as a solvent for the electrolyte.
  • a mixture of the complexes K [AIEt], Na [AIEt] and AIEt 3 can be used as the electrolyte.
  • the molar ratio of the complexes to AIEt 3 is preferably 1: 0.5 to 1: 3 and more preferably 1: 2.
  • the electrodeposition of the layer can be carried out using a soluble anode containing the metals intended for the deposition.
  • This anode can either contain the metals intended for deposition as a metal alloy, or several soluble anodes of the respective pure metals can be used. If a layer containing an aluminum / magnesium alloy is to be deposited, it is possible to use a soluble aluminum and a likewise soluble magnesium anode or an anode made of an aluminum / magnesium alloy.
  • Aluminum / tin alloy is to be deposited, a soluble aluminum and a likewise soluble tin anode or an anode made of an aluminum / tin alloy.
  • the electrolytic coating of a non-aqueous electrolyte is preferably carried out at a temperature of 80-105 ° C. A temperature of the electroplating bath of 91-100 ° C. is preferred.
  • an electrically conductive layer is applied to the substrate before the layer is applied galvanically in step a).
  • the layer which conducts the electrical current can be applied to the substrate by any method which is known to the person skilled in the art.
  • the layer that conducts the electrical current is preferably applied to the substrate by metallization.
  • step b) of the method according to the invention the temperature and / or the duration of the heat treatment is chosen such that, at least in the boundary region between the substrate and the applied layer of step a), an alloy containing metal of the surface layer of the substrate and metal and / or Metal alloys of the applied layer is formed.
  • the temperature and / or the duration of the heat treatment are to be selected so that they are matched to the properties of the substrate and the specific layer applied.
  • this temperature is preferably ⁇ 650 ° C.
  • the heat treatment generally forms an intermetallic phase on the surface of the coated workpiece, in which the layer applied in step a) is converted either partially or continuously into the intermetallic phase.
  • the liqui dusline is the melting temperature of the material mixture formed depending on the specific composition.
  • the proportion of aluminum in the surface layer is first 100%.
  • a titanium-aluminum alloy with a specific melting point will form during the heat treatment. If the temperature is now selected during the heat treatment so that the melting point of the alloy that is formed is reached or is just below, then this heat treatment is to be understood as heat treatment below / along the liquidus line of the resulting material mixture.
  • the heat treatment of the coated substrate is carried out in such a way that a liquid phase is formed on the surface of the coated substrate. This is achieved by treating at a temperature that is higher than the melting temperature of the resulting surface layer.
  • the heat treatment can be carried out under a protective gas atmosphere. It is preferred here that a protective gas is used which does not react with the coated material.
  • the protective gas is preferably a rare gas, e.g. Argon. However, it is not necessary for the heat treatment to take place in a protective gas atmosphere. Alternatively, the heat treatment can also be carried out in air.
  • the temperature of the heat treatment of step b) is preferably between 400 ° C and 1000 ° C, more preferably between 450 ° C and 900 ° C and most preferably between 500 ° C and 800 ° C.
  • the duration of the heat treatment of step b) can be between one second and 10 hours. Preferably it is between 1 minute and 5 hours and most preferably between 2 minutes and 3 hours.
  • the heat treatment of step b) is then carried out when the workpiece is installed at its destination. So it is possible that, for. B. a motor element or turbine element is heated during its first use in such a way that the diffusion of the surface layer of the substrate with the applied layer takes place.
  • the layer can be subjected to a further treatment.
  • All treatment methods that are known to the person skilled in the art can be used here.
  • the treatment can be an anodic oxidation, which is preferably the anodizing of the layer. Such a treatment is appropriate if a layer containing aluminum was applied in step a).
  • the coated workpiece used in the method of the present invention is preferably a rack product, a bulk product, an endless product or a molded part.
  • the coated workpiece is preferably a wire, a sheet metal, a screw, a nut, a concrete anchor, a machine component, an engine, an engine part or a turbine blade.
  • Workpieces have excellent long-term resistance to thermal stress. With repeated heating and cooling cycles, they show that, due to the temperature load, there is no corrosion of the workpiece over a long period of time. In particular, the coated workpieces show improved resistance to oxidation or other corrosive high-temperature influences at which the uncoated workpiece, that is to say the substrate, is already beginning to corrode.
  • a coated titanium substrate according to the present invention when z. B. with aluminum or an aluminum um / magnesium alloy was coated, a temperature stability in the range of 750 - 1000 ° C.
  • the coated substrates of the present invention are significantly more temperature-resistant than those of the prior art.
  • An explanation for this could be without, however, being bound to a theory that a highly pure layer is obtained by the galvanic application, while in the coating processes of the prior art, such as, for. B. chemical vacuum deposition, physical vacuum deposition, or plasma spraying, impurities are present in the applied layer, which have an adverse effect on the temperature stability. Since high-purity layers are obtained by the galvanic process, germs that are caused by contamination are not present in the layer. High-purity diffusion layers are thus formed which, owing to the high purity, have improved stability and, above all, improved temperature stability.
  • the layer thickness is less than on more accessible areas.
  • no homogeneous layer forms on the substrate, which inevitably causes deteriorated corrosion resistance at those points where the layer thickness is less.
  • galvanic deposition of the layer on the substrate a homogeneous and sufficiently thick layer itself is hard to reach places, such as', for example, corners and edges, is applied.
  • the diffusion layer obtained by heat treatment also has a sufficient layer thickness at these locations which are difficult to access geometrically and thus has adequate and improved corrosion stability.
  • the workpieces obtained by the present invention differ from the workpieces of the prior art. Furthermore, as already explained, they also form at these critical points due to the fact that pure layers are applied, after the heat treatment high-purity diffusion layers.
  • Another advantage of the method of the present invention is that it is less expensive compared to the methods of the prior art.
  • the galvanic application of a layer is less expensive than e.g. B. plasma spraying.
  • Another advantage is that both by plasma spraying such. B. by chemical vacuum deposition or physical vacuum deposition, the substrate is subjected to greater thermal stress. This leads to thermal distortion of the workpiece, in particular in the case of geometrically complex substrates. If the method of the present invention is used, the thermal stress on the workpiece in step a) is significantly lower. This makes it possible to produce coated workpieces with lower manufacturing tolerances, which has significant advantages in subsequent operation as e.g. Turbine blade causes. Furthermore, lower manufacturing tolerances result in an increased level of safety for coated workpieces subject to high thermal loads.
  • the workpieces produced by the method of the present invention, such as. B. ensure turbine blades, when installed in a gas turbine, higher safety reserves compared to the turbine blades of the prior art.
  • a sheet of size 5 x 25 x 1 mm made of titanium is provided with a layer of aluminum with a layer thickness of 12 ⁇ m by galvanic deposition from a non-aqueous electrolyte. 2. Heat treatment of the sheet
  • the titanium sheet provided with a layer of aluminum is heated in an oven to the temperature shown in Table 1. The temperature is maintained for the period specified in Table 1.
  • the coated titanium sheet is then removed from the furnace and it cools down in an air atmosphere. During the alloying process, the furnace is either exposed to ambient air or the protective gas argon.
  • the coated titanium sheets with the numbers A, B and C are heated in an oven to the temperature shown in Table 2. After the holding time given in Table 1, the material sample is taken out of the furnace, cooled and the corrosion of the coated titanium sheet is assessed visually. This shows that the applied layer has excellent corrosion resistance, even at very high temperatures, such as. B. 900 ° C. A non- coated titanium sheet would be permanently damaged by oxidation at a temperature above approx. 650 ° C. Even with a holding time of 384 hours at 700 ° C, there is no noticeable corrosion of the coated titanium sheet.
  • a titanium sheet which is produced according to the method of the present invention has an improved corrosion resistance.
  • the workpieces coated in this way are significantly more corrosion-resistant than those of the prior art.
  • the corrosion resistance is significantly improved at elevated temperatures.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Laminated Bodies (AREA)
  • Insulated Metal Substrates For Printed Circuits (AREA)

Abstract

La présente invention concerne un procédé de production de pièces revêtues. Ce procédé comporte les étapes suivantes: a) précipitation par électrolyse d'au moins une couche contenant au moins un métal et/ou un alliage métallique sur un substrat, et b) un traitement thermique du substrat revêtu à une température comprise entre 300 DEG C et 1000 DEG C, de telle manière qu'au moins la couche superficielle du substrat et la ou les couches appliquées à l'étape a) se diffusent partiellement et/ou entièrement l'une dans l'autre. L'invention concerne également les pièces revêtues par ce procédé.
EP04798168A 2003-11-07 2004-11-05 Revetement de substrats Withdrawn EP1682697A2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP04798168A EP1682697A2 (fr) 2003-11-07 2004-11-05 Revetement de substrats

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
EP03025645 2003-11-07
EP03026218A EP1533401A1 (fr) 2003-11-14 2003-11-14 Electroplacage de substrats suivi d'une étape de diffusion
PCT/EP2004/052828 WO2005045102A2 (fr) 2003-11-07 2004-11-05 Revetement de substrats
EP04798168A EP1682697A2 (fr) 2003-11-07 2004-11-05 Revetement de substrats

Publications (1)

Publication Number Publication Date
EP1682697A2 true EP1682697A2 (fr) 2006-07-26

Family

ID=34575670

Family Applications (1)

Application Number Title Priority Date Filing Date
EP04798168A Withdrawn EP1682697A2 (fr) 2003-11-07 2004-11-05 Revetement de substrats

Country Status (3)

Country Link
US (1) US20070261965A1 (fr)
EP (1) EP1682697A2 (fr)
WO (1) WO2005045102A2 (fr)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1524336A1 (fr) * 2003-10-18 2005-04-20 Aluminal Oberflächtentechnik GmbH & Co. KG Pièces à usiner recouvertes d'un alliage aluminium-magnesium
KR101338824B1 (ko) 2005-12-01 2013-12-06 스미토모 고무 고교 가부시키가이샤 금속 코드, 고무 코드 복합체 및 이들을 이용한 공기 타이어
US20090025846A1 (en) 2005-12-13 2009-01-29 Sumitomo Rubber Industries, Ltd. Metal Cord, Rubber-Cord Complex and Pneumatic Tire Using the Same
US9926793B2 (en) 2013-03-15 2018-03-27 United Technologies Corporation Blades and manufacture methods
FR3013781A1 (fr) * 2013-11-25 2015-05-29 Airbus Operations Sas Element de fixation de pieces d'un assemblage
US10041361B2 (en) 2014-10-15 2018-08-07 General Electric Company Turbine blade coating composition
WO2016068838A1 (fr) * 2014-10-27 2016-05-06 Hewlett-Packard Development Company, L.P. Substrat en alliage de magnésium

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US2044742A (en) * 1934-11-27 1936-06-16 Armstrong Composite ferrous bodies
US3028319A (en) * 1960-02-01 1962-04-03 Ethyl Corp Manufacture of magnesium organo compounds
US3560274A (en) * 1969-10-10 1971-02-02 Ibm Wear-resistant titanium and titanium alloys and method for producing same
US4148204A (en) * 1971-05-07 1979-04-10 Siemens Aktiengesellschaft Process of mechanically shaping metal articles
US3755090A (en) * 1972-03-27 1973-08-28 British Steel Corp A method of providing a surface of a steel substrate with an aluminum coating
FR2244017B1 (fr) * 1973-09-14 1977-09-23 Stephanois Rech
US4236940A (en) * 1979-06-12 1980-12-02 United Technologies Corporation Wear resistant titanium alloy coating
EP0184985A3 (fr) * 1984-12-12 1987-12-23 Eltech Systems Corporation Couche pour substrats métalliques, procédé de fabrication et utilisation de la couche
US4655884A (en) * 1985-08-19 1987-04-07 General Electric Company Nickel plating of refractory metals
GB2188942B (en) * 1986-04-11 1990-04-04 Rolls Royce Plc Protective coating
DE3622032A1 (de) * 1986-07-01 1988-01-21 Menrad Ferdinand Gmbh Co Kg Verfahren zum beschichten von titan und aehnlichen werkstoffen
EP0289432A1 (fr) * 1987-03-30 1988-11-02 PECHINEY RECHERCHE (Groupement d'Intérêt Economique régi par l'ordonnance du 23 Septembre 1967) Procédé pour former à la surface d'un substrat en alliage d'aluminium une zone riche en aluminiure d'au moins un des éléments nickel, fer, cobalt
US5196075A (en) * 1988-02-17 1993-03-23 Itw-Ateco Gmbh Method for modifying and thereby improving the corrosion resistance and hardness of workpieces of ferritic steel
JP3045612B2 (ja) * 1992-06-22 2000-05-29 東洋鋼鈑株式会社 高耐食性ニッケルめっき鋼帯およびその製造法
EP1105245B1 (fr) * 1998-01-29 2008-04-02 Clad Metals LLC Methode d'assemblage de metaux dissemblables
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Title
See references of WO2005045102A2 *

Also Published As

Publication number Publication date
US20070261965A1 (en) 2007-11-15
WO2005045102A2 (fr) 2005-05-19
WO2005045102A3 (fr) 2006-02-16

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