EP1970473B1 - Procédé d'électropolissage pour titane - Google Patents

Procédé d'électropolissage pour titane Download PDF

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Publication number
EP1970473B1
EP1970473B1 EP08003975A EP08003975A EP1970473B1 EP 1970473 B1 EP1970473 B1 EP 1970473B1 EP 08003975 A EP08003975 A EP 08003975A EP 08003975 A EP08003975 A EP 08003975A EP 1970473 B1 EP1970473 B1 EP 1970473B1
Authority
EP
European Patent Office
Prior art keywords
titanium
electrolyte
electropolishing
acids
methanesulfonic acid
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
EP08003975A
Other languages
German (de)
English (en)
Other versions
EP1970473A2 (fr
EP1970473A3 (fr
Inventor
Olaf BÖHME
Siegfried Pießlinger-Schweiger
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.)
Poligrat GmbH
Original Assignee
Poligrat GmbH
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Filing date
Publication date
Application filed by Poligrat GmbH filed Critical Poligrat GmbH
Publication of EP1970473A2 publication Critical patent/EP1970473A2/fr
Publication of EP1970473A3 publication Critical patent/EP1970473A3/fr
Application granted granted Critical
Publication of EP1970473B1 publication Critical patent/EP1970473B1/fr
Not-in-force legal-status Critical Current
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F3/00—Electrolytic etching or polishing
    • C25F3/16—Polishing
    • C25F3/22—Polishing of heavy metals
    • C25F3/26—Polishing of heavy metals of refractory metals

Definitions

  • the present invention relates to a process for the electrochemical polishing of surfaces of titanium or titanium-containing alloys. This method is particularly useful for alloys having a titanium content of at least about 50 mole percent, such as the nickel-titanium alloy nitinol.
  • an electrolyte is used which comprises methanesulfonic acid and one or more, optionally substituted alkanediphosphonic acids.
  • the present invention also relates to the use of such an electrolyte for electropolishing surfaces of titanium and / or titanium-containing alloys, such as nitinol.
  • Electrochemical polishing or electropolishing, as well as the glazing and deburring of metal surfaces is a technique commonly used in the art to treat the surfaces of metal workpieces and articles. Such a treatment serves to improve the surface quality, for example by removing burrs on edges and surfaces, by smoothing, cleaning and glazing, both for decorative and technical purposes. Furthermore, by the electropolishing stresses in the outer material layers can be removed.
  • the workpieces to be machined are arranged on suitable, electrically conductive holding devices, or in baskets or drums of electrically conductive material. These workpieces are immersed in a polishing bath containing an electrolyte and connected anodically, applying a direct current. As a result of the action of the current and of the electrolyte, metal is removed from the material surface, whereby the surface is smoothed and deburred. The workpiece is then removed from the polishing bath and rinsed off.
  • EP 1 354 986 A2 For example, there is described an apparatus and method for electropolishing titanium and titanium alloys (Titanium Grade 1 to 10) using an electrolyte of sulfuric acid and alcohols.
  • this method has the further disadvantage that due to the flammability of this electrolyte requires a complex cooling of the electrolyte to temperatures below 15 ° C. is, in conjunction with automatic extinguishing systems for fire protection.
  • the patent application DE 100 37 337 A1 describes a method and fixture for electropolishing bodies of titanium alloys or nickel-titanium alloys such as Nitinol, wherein the electrolyte comprises formamide and sulfamic acid.
  • the present invention is an electropolishing process for the electrochemical smoothing and / or deburring of surfaces of titanium or titanium-containing alloys, which does not have the aforementioned disadvantages. These methods are based on the use of an electrolyte comprising methanesulfonic acid and one or more alkanediphosphonic acids, wherein the one or more alkanediphosphonic acids may optionally be substituted with one or more hydroxy and / or amino groups.
  • the concentration of methanesulfonic acid in the electrolyte is at least 95% by weight, based on the total weight of the electrolyte.
  • concentrated methanesulfonic acid with a content of at least 98% by weight for example methanesulfonic acid with a content of more than 99% by weight, is used, to which the one or more alkanediphosphonic acids are added as pure substance (s).
  • a particularly suitable alkane diphosphonic acid for use in the processes described herein is 1-hydroxyethane-1,1-diphosphonic acid (HEDP, also referred to as etidronic acid).
  • HEDP 1-hydroxyethane-1,1-diphosphonic acid
  • electrolyte used in the process described herein HEDP may be used alone or in combination with other alkane diphosphonic acids in concentrated methanesulfonic acid as previously defined.
  • the concentration of the one or more alkanediphosphonic acids in the electrolyte is preferably between 1 and 50 g / kg of electrolyte, for example between 3 and 25 g / kg of electrolyte.
  • the one or more alkane diphosphonic acids be used between 5 and 20 g / kg of electrolyte.
  • the electrolyte consists essentially of methanesulfonic acid and one or more alkane diphosphonic acids This means that no other substances are added and such other substances only in small amounts, for example less than 3 wt .-%, are present, such as by impurities of methanesulfonic acid or alkanediphosphonic, or due to the operation in the course of electropolishing (for example ablated ions).
  • the electrolyte used in accordance with the present process contains no or only minor amounts of water.
  • the water content of the electrolyte is therefore preferably at most 2 wt .-%, more preferably below 1 wt .-%, based on the total weight of the electrolyte.
  • the electropolishing is preferably carried out at a temperature in the range of 20 ° C to 70 ° C, for example between room temperature and 60 ° C, and in particular at a temperature between 25 ° C and 50 ° C.
  • the anodic current density at which the workpieces are electropolished can be chosen from a wide range. This is preferably in the range from 2 to 50 A / dm 2 , in particular between 5 and 30 A / dm 2 .
  • the applied voltage can often be in the range of 10 to 35 volts.
  • the duration of the electropolishing process of course depends on the particular roughness of the workpiece to be machined and the desired smoothing or deburring.
  • the optimum exposure time can be determined by the average person skilled in the art within the scope of routine experiments as a function of the current density used, the temperature, the electrolyte and the device used without any particular effort. As a rule, a treatment of the workpiece is sufficient for a few minutes.
  • the machined workpiece is removed from the electropolishing bath and rinsed with water, preferably deionized water. It is not crucial that the workpiece is immediately freed from the electrolyte.
  • the electrolyte described here does not attack the machined surface, which facilitates the processing and makes no further demands on the equipment used.
  • This electrolyte described here can be used both for pure titanium and for titanium-containing alloys.
  • These titanium-containing alloys may in particular comprise titanium in a proportion of at least 50 mol%.
  • An important such alloy comprising titanium at a level of about 50 mole percent is the nickel-titanium alloy nitinol, also referred to as a "memory alloy”.
  • an electrolyte comprising methanesulfonic acid and one or more alkanediphosphonic acids to electropolish surfaces of titanium, titanium-containing alloys, and nickel-titanium alloys, such as nitinol, is also an aspect of the invention described herein.
  • electrolytes require in their use - in contrast to the electrolytes used in the prior art - no technically complex facilities, but can in conventional industrial electropolishing, as used for example for the treatment of stainless steel, are used.
  • an electrolyte as used in accordance with the present invention is nonflammable, not very corrosive, and easy to handle. With normal handling, there is no increased risk for the people who operate the electropolishing system or work in the vicinity of this system, as well as for the environment. In particular, the electrolyte described herein releases no harmful gases or vapors.
  • the methods and electrolytes described herein are not only easier to handle in the treatment of titanium-containing surfaces, but also make it possible to achieve a smoothening or de-burring of the surfaces as described in the prior art. at least equal, if not superior in many cases.
  • a sheet measuring 50 ⁇ 50 ⁇ 1.0 mm with a ground surface and a roughness of Ra 0.8 ⁇ m was used in an electrolyte consisting of 990 g of methanesulfonic acid 100% and 10 g of 1-hydroxyethyl-1,1-diphosphonic acid electropolished.
  • the sheet was degreased before treatment, rinsed with water and dried. After electropolishing, the sheet was removed from the electrolyte and rinsed in deionized water after a waiting time of 5 minutes and dried.
  • the edges were smooth and burr-free.
  • a 0.8 mm diameter nitinol wire was electropolished in an electrolyte according to Example 1.
  • the wire was pretreated and post-treated according to Example 1.
  • the result was a high gloss and smooth surface without etching attack on the microstructure.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
  • ing And Chemical Polishing (AREA)

Claims (13)

  1. Procédé d'électropolissage et/ou d'ébavurage électrochimique de surfaces en titane ou en des alliages base titane, caractérisé en ce que l'électrolyte utilisé à cette occasion comprend de l'acide méthanesulfonique et un ou plusieurs acides alcane-diphosphoniques, ledit un ou lesdits plusieurs acides alcane-diphosphoniques pouvant, le cas échéant, être substitués avec des groupes hydroxyle ou amino.
  2. Procédé selon la revendication 1, caractérisé en ce que la concentration de l'acide méthanesulfonique dans l'électrolyte a une valeur d'au moins 95 % en poids, par rapport au poids total de l'électrolyte.
  3. Procédé selon l'une des revendications précédentes, caractérisé en ce que ledit un ou lesdits plusieurs acides alcane-diphosphoniques comprennent de l'acide 1-hydroxyéthane-1,1-diphosphonique.
  4. Procédé selon l'une des revendications précédentes, caractérisé en ce que la concentration dudit un ou desdits plusieurs acides alcane-diphosphoniques se situe entre 1 et 50 g/kg d'électrolyte.
  5. Procédé selon l'une des revendications 1 à 3, caractérisé en ce que la concentration dudit un ou desdits plusieurs acides alcane-diphosphoniques se situe entre 5 et 20 g/kg d'électrolyte.
  6. Procédé selon l'une des revendications précédentes, caractérisé en ce que l'électrolyte est essentiellement constitué d'acide méthanesulfonique et d'un ou plusieurs acides alcane-diphosphoniques.
  7. Procédé selon l'une des revendications précédentes, caractérisé en ce qu'il est mis en oeuvre à une température entre 20 °C et 70 °C.
  8. Procédé selon l'une des revendications précédentes, caractérisé en ce que le procédé est mis en oeuvre avec une densité de courant anodique de 2 à 50 A/dm2.
  9. Procédé selon l'une des revendications 1 à 7, caractérisé en ce que le procédé est mis en oeuvre avec une intensité de courant anodique de 5 à 30 A/dm2.
  10. Procédé selon l'une des revendications précédentes, caractérisé en ce que les alliages base titane contiennent du titane selon une teneur d'un pourcentage molaire d'au moins environ 50 %.
  11. Procédé selon la revendication 10, caractérisé en ce que l'alliage base titane est du Nitinol.
  12. Utilisation d'un électrolyte selon l'une des revendications 1 à 6 pour l'électro-polissage de surfaces en titane ou en des alliages base titane.
  13. Utilisation selon la revendication 12, caractérisée en ce que l'alliage base titane est du Nitinol.
EP08003975A 2007-03-09 2008-03-04 Procédé d'électropolissage pour titane Not-in-force EP1970473B1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE102007011632A DE102007011632B3 (de) 2007-03-09 2007-03-09 Elektropolierverfahren für Titan

Publications (3)

Publication Number Publication Date
EP1970473A2 EP1970473A2 (fr) 2008-09-17
EP1970473A3 EP1970473A3 (fr) 2010-08-25
EP1970473B1 true EP1970473B1 (fr) 2011-08-31

Family

ID=39365667

Family Applications (1)

Application Number Title Priority Date Filing Date
EP08003975A Not-in-force EP1970473B1 (fr) 2007-03-09 2008-03-04 Procédé d'électropolissage pour titane

Country Status (6)

Country Link
US (1) US20080217186A1 (fr)
EP (1) EP1970473B1 (fr)
JP (1) JP5145083B2 (fr)
AT (1) ATE522642T1 (fr)
DE (1) DE102007011632B3 (fr)
ES (1) ES2369942T3 (fr)

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TR201815028T4 (tr) * 2009-11-23 2018-11-21 MetCon LLC Elektro parlatma yöntemleri.
US8580103B2 (en) 2010-11-22 2013-11-12 Metcon, Llc Electrolyte solution and electrochemical surface modification methods
WO2014087414A1 (fr) 2012-12-03 2014-06-12 Amrita Vishwa Vidya Peetham University Endoprothèse cardiovasculaire à base de titane métallique avec une surface nanostructurée et procédé pour la fabriquer
EP2878713A1 (fr) * 2013-11-28 2015-06-03 Abbott Laboratories Vascular Enterprises Limited Composition électrolytique et procédé pour le traitement de polissage électrolytique d'alliages de nickel-titane et/ou d'autres substrats métalliques comprenant des alliages de tungstène, niobate et tantale
CN104668677A (zh) * 2013-12-02 2015-06-03 天津大学 用于钛合金电解加工的非水基电解液及其制备方法
ES2604830B1 (es) 2016-04-28 2017-12-18 Drylyte, S.L. Proceso para alisado y pulido de metales por transporte iónico mediante cuerpos sólidos libres, y cuerpos sólidos para llevar a cabo dicho proceso.
JP2017214614A (ja) * 2016-05-31 2017-12-07 株式会社カネカ 電解研磨された金属成形体の製造方法
JP6752626B2 (ja) * 2016-05-31 2020-09-09 株式会社カネカ 電解研磨液および電解研磨された金属成形体の製造方法
WO2018102845A1 (fr) 2016-12-09 2018-06-14 Hirtenberger Engineered Surfaces Gmbh Procédé d'électropolissage et électrolyte pour ce procédé
AT520365B1 (de) * 2017-08-29 2019-10-15 Hirtenberger Eng Surfaces Gmbh Elektrolyt zum elektropolieren von metalloberflächen
ES2734499B2 (es) * 2018-11-12 2020-06-03 Drylyte Sl Uso de ácidos sulfónicos en electrolitos secos para pulir superficies metálicas a través del transporte de iones
US11492723B2 (en) * 2019-11-05 2022-11-08 Cilag Gmbh International Electrolyte solutions for electropolishing of nitinol needles
EP4073294B1 (fr) * 2019-12-10 2024-01-03 Biotronik Ag Nouvel électrolyte pour le polissage électrolytique d'alliages de titane
ES2831105B2 (es) 2020-02-04 2021-10-20 Steros Gpa Innovative S L Dispositivo para el electropulido de multiples piezas sin sujecion firme mediante electrolitos solidos
DE102021120263A1 (de) * 2021-08-04 2023-02-09 Bayerische Motoren Werke Aktiengesellschaft Verfahren und Vorrichtung zum Herstellen eines beschichteten Strukturbauteils
WO2023157410A1 (fr) 2022-02-15 2023-08-24 日本軽金属株式会社 Élément métallique à surface lissée et son procédé de fabrication
CN115652401B (zh) * 2022-11-07 2025-03-25 东北大学 一种激光增材制造钛合金工件的等离子抛光液及其制备和应用
JP7603350B1 (ja) 2024-05-28 2024-12-20 東京ステンレス研磨興業株式会社 純チタン若しくはチタン合金又はニッケル基合金製の被減面材を減面する方法

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Also Published As

Publication number Publication date
ATE522642T1 (de) 2011-09-15
JP5145083B2 (ja) 2013-02-13
DE102007011632B3 (de) 2008-06-26
EP1970473A2 (fr) 2008-09-17
EP1970473A3 (fr) 2010-08-25
JP2008223139A (ja) 2008-09-25
ES2369942T3 (es) 2011-12-09
US20080217186A1 (en) 2008-09-11

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