EP1903132B1 - Procédé d'électropolissage pour cobalt et alliages de cobalt - Google Patents

Procédé d'électropolissage pour cobalt et alliages de cobalt Download PDF

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Publication number
EP1903132B1
EP1903132B1 EP07018326A EP07018326A EP1903132B1 EP 1903132 B1 EP1903132 B1 EP 1903132B1 EP 07018326 A EP07018326 A EP 07018326A EP 07018326 A EP07018326 A EP 07018326A EP 1903132 B1 EP1903132 B1 EP 1903132B1
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EP
European Patent Office
Prior art keywords
cobalt
acid
electrolyte
sulfonic acid
alloys
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.)
Active
Application number
EP07018326A
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German (de)
English (en)
Other versions
EP1903132A3 (fr
EP1903132A2 (fr
Inventor
Siegfried Pießlinger-Schweiger
Olaf BÖHME
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
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Poligrat GmbH
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Publication of EP1903132A3 publication Critical patent/EP1903132A3/fr
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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

Definitions

  • the present invention relates to a process for the electrochemical polishing of surfaces of cobalt or cobalt alloys.
  • the electrolyte comprises glycolic acid and at least one alkanesulfonic acid.
  • cobalt alloys consisting of cobalt or cobalt alloys, or having surfaces of cobalt or cobalt alloys, are becoming increasingly important.
  • cobalt alloys are used in various fields because of their high resistance to corrosion and wear.
  • Applications include areas as diverse as mechanical engineering, where cobalt alloys are used to protect against wear, and medical technology, where cobalt alloys are used for implants because of their high corrosion resistance, strength, and absence of nickel.
  • US 6,679,980 B1 describes an electropolishing process that can be used to electropolish stents that may be cobalt-chromium-tungsten.
  • the electrolyte used contains concentrated hydrochloric acid and concentrated sulfuric acid.
  • An electrolyte containing sulfuric acid and hydrochloric acid, which also contains glycol, is also available in Automated Design of Fuzzy Systems ", H. Surmann, VDI Verlag, Erasmus 8, Nr. 452 described.
  • the methods described in these documents focus primarily on special equipment and controls of the electropolishing process. This is not surprising since with the electrolytes described therein under conventional electropolishing conditions smoothing or deburring of the desired quality surfaces is frequently not possible is. This too can be attributed to the carbides contained in the structure of the workpieces, since these are not removed to the same extent as the metal or the metallic alloy and can thus in some cases even lead to an increase in the roughness of the surfaces.
  • cobalt alloys are becoming increasingly important in the field of medical technology.
  • One of the reasons for this is that an increasing proportion of the population suffers from allergies to nickel. For this reason, efforts are increasingly being made to restrict the use of nickel-containing stainless steels for medical implants.
  • cobalt-chromium alloys are considered as a substitute for this.
  • implant alloys cobalt-chromium alloys
  • the surfaces of these workpieces must be polished to a high quality.
  • chromium-nickel steels this is done mainly by electrochemical polishing, since this method gives the best results.
  • cobalt-chromium alloys so far no comparable suitable electropolishing available.
  • Cobalt-based hard metals are also frequently used in mechanical and plant engineering, as their hardness and high wear resistance significantly exceed those of other materials.
  • the surfaces of pumps, valves, bearings, and other components, which are particularly at risk from wear are often armored with the cobalt alloy Stellite.
  • the mechanical polish of stellite often creates stresses that are at the expense of the corrosion resistance of the workpieces.
  • Subsequent heat treatment of the surfaces to relieve these stresses is cumbersome and often not possible to the extent that would be required due to the nature of the machine parts. Because of these drawbacks, there has long been a need for electropolishing methods that enable smoothing and deburring of surfaces of cobalt or cobalt alloy workpieces of comparable quality as can be achieved in electropolishing stainless steel surfaces.
  • the present invention is a process for electrochemically polishing cobalt-containing surfaces using the electrolyte described below.
  • These electropolishing methods according to the invention are suitable for producing high-quality, micro-smooth surfaces of workpieces made of cobalt or cobalt alloys.
  • the electrolyte enables the production of shiny, smooth and deburred surfaces of cobalt or cobalt alloys.
  • This electrolyte comprises at least one alkanesulfonic acid having an alkyl radical having 1, 2 or 3 carbon atoms and glycolic acid.
  • the at least one alkanesulfonic acid comprises methanesulfonic acid.
  • Such Elek trolyte may for example consist of glycolic acid, methanesulfonic acid and water.
  • an electrolyte consisting of a mixture of alkanesulfonic acid (or more alkanesulfonic acids) having an alkyl group of 1 to 3 carbon atoms and glycolic acid is capable of smoothing cobalt-based surfaces to an unprecedented extent was completely surprising and unexpected .
  • this mixture as electrolyte, cobalt and cobalt alloys, including alloys such as stellite, can be electropolished without any appreciable grain boundary attack.
  • Such an electropolishing process makes it possible to routinely obtain surfaces of cobalt-containing workpieces in a previously unattained gloss and smoothness grade.
  • the electrolyte has a ratio of alkanesulfonic acid to glycolic acid in the range from 30:70 to 80:20, based on the pure substances. Further preferred is a mixture having a ratio of alkanesulfonic acid to glycolic acid in the range of 60:40 to 70:30, based on the pure substances.
  • the active substances alkanesulfonic acid and glycolic acid are present in the electrolyte in high concentration. So contains the Electrolyte in one embodiment, a maximum of 35 wt .-% water. Preferably, the electrolyte contains a maximum of 25 wt .-% water.
  • the active substances either as pure substance or as concentrated solutions.
  • the glycolic acid is suitably used as a concentrated aqueous solution containing 60-80% by weight of glycolic acid, preferably ⁇ 70% by weight.
  • Such solutions are commercially available.
  • alkanesulfonic acid or alkanesulfonic acids are preferably used in highly concentrated form.
  • methanesulfonic acid can be used as about 85% or as ⁇ 99% solution as it is commercially available.
  • the electrolyte contains no explosive substances, in particular no perchloric acid or salts of perchloric acid.
  • the process according to the invention can be carried out under any conditions which are customary in the art and known to the person skilled in the art. Process temperatures in the range between 40 ° C and 70 ° C have proven particularly suitable. The regulation and monitoring of the temperature may be carried out in any manner known to those skilled in the art.
  • the process is performed at an anodic current density that is between 5 and 25 A / dm 2 . In a further embodiment of the invention, the anodic current density is about 10 A / dm 2 .
  • the duration of the electropolishing process depends on the roughness of the workpiece to be polished and the desired smoothing.
  • the optimum exposure time the expert in the context of routine experiments depending on determine the current density used, the temperature, the composition of the electrolyte and the electropolishing apparatus in routine experiments.
  • the treated workpiece is removed from the polishing bath and typically rinsed with demineralized water and optionally dried.
  • inventive methods are particularly suitable for the electrochemical polishing of workpieces with a surface consisting of a cobalt-chromium alloy.
  • cobalt-chromium alloys may contain other constituents in addition to the elements cobalt and chromium.
  • Such cobalt-chrome alloy surfaces smoothed and deburred by methods of the present invention may be used as medical implants because of their high compatibility with human or general biological tissue.
  • the cobalt-chromium alloy stellite which consists of about 50-60% cobalt, 30-40% chromium and 8-20% tungsten, but may also contain smaller amounts of other elements, can be with the methods described herein in a hitherto Smooth and deburr unrecognized quality.
  • the electropolishing methods described here for workpieces made of cobalt alloys, such as stellite can be used in particular in nuclear technology both in the manufacture of new components prior to their use, as well as for cleaning and decontamination of cobalt-containing components that are already in use or in use to allow a safer repair or disposal of these components.
  • the electropolishing method according to the invention is also suitable for producing high-quality smooth wear protection layers based on cobalt or cobalt alloy, which are applied to workpieces made of other materials.
  • the treatment was carried out at a current density of 10 A / dm 2 and temperatures between 40 ° C and 70 ° C in an electrolyte consisting of a mixture of ⁇ 99% methanesulfonic acid and ⁇ 70% glycolic acid (in water) in a mixing ratio from 55:45. This corresponds to a ratio of the pure substances of about 65:35 and a water content of less than 15%.

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)
  • Electroplating And Plating Baths Therefor (AREA)

Claims (13)

  1. Procédé pour l'électropolissage de surfaces en cobalt ou en alliages de cobalt, à l'aide d'un électrolyte qui comprend au moins un acide alcanesulfonique avec un reste alkyle présentant 1, 2 ou 3 atomes de carbone, et de l'acide glycolique.
  2. Procédé selon la revendication 1, caractérisé en ce que ledit au moins un acide alcanesulfonique comprend de l'acide méthanesulfonique.
  3. Procédé selon la revendication 1 ou la revendication 2, caractérisé en ce que la proportion de l'acide alcanesulfonique par rapport à l'acide glycolique se situe dans une plage de 30:70 à 80:20, rapportée au poids des substances pures.
  4. Procédé selon la revendication 1 ou la revendication 2, caractérisé en ce que la proportion de l'acide alcanesulfonique par rapport à l'acide glycolique se situe dans une plage de 60:40 à 70:30, rapportée au poids des substances pures.
  5. Procédé selon l'une des revendications précédentes, caractérisé en ce que l'électrolyte renferme au maximum 35 % en poids d'eau.
  6. Procédé selon l'une des revendications 1 à 4, caractérisé en ce que l'électrolyte renferme au maximum 25 % en poids d'eau.
  7. Procédé selon l'une des revendications précédentes, caractérisé en ce que l'électrolyte ne renferme pas d'acide perchlorique ni de perchlorates.
  8. Procédé selon la revendication 1, caractérisé en ce que le procédé est mis en oeuvre à une température entre 40 °C et 70 °C.
  9. Procédé selon la revendication 1 ou la revendication 2, caractérisé en ce que le procédé est mis en oeuvre avec une densité de courant anodique de 5 à 25 A/dm2.
  10. Procédé selon la revendication 1 ou la revendication 2, caractérisé en ce que le procédé est mis en oeuvre avec une densité de courant anodique d'environ 10 A/dm2 .
  11. Procédé selon l'une des revendications 1 à 10, caractérisé en ce que la surface est constituée d'un alliage chrome-cobalt.
  12. Procédé selon la revendication 11, caractérisé en ce que la surface est une surface d'un implant médical.
  13. Procédé selon la revendication 11, caractérisé en ce que l'alliage chrome-cobalt est du stellite.
EP07018326A 2006-09-25 2007-09-18 Procédé d'électropolissage pour cobalt et alliages de cobalt Active EP1903132B1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE102006045221A DE102006045221B3 (de) 2006-09-25 2006-09-25 Elektropolierverfahren für Kobalt und Kobaltlegierungen und Elektrolyt

Publications (3)

Publication Number Publication Date
EP1903132A2 EP1903132A2 (fr) 2008-03-26
EP1903132A3 EP1903132A3 (fr) 2010-08-25
EP1903132B1 true EP1903132B1 (fr) 2011-11-02

Family

ID=38616337

Family Applications (1)

Application Number Title Priority Date Filing Date
EP07018326A Active EP1903132B1 (fr) 2006-09-25 2007-09-18 Procédé d'électropolissage pour cobalt et alliages de cobalt

Country Status (7)

Country Link
US (1) US8080148B2 (fr)
EP (1) EP1903132B1 (fr)
JP (1) JP2008121110A (fr)
AT (1) ATE531836T1 (fr)
CA (1) CA2604387C (fr)
DE (1) DE102006045221B3 (fr)
ES (1) ES2374310T3 (fr)

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9039887B2 (en) * 2012-05-14 2015-05-26 United Technologies Corporation Component finishing method and assembly
US10399166B2 (en) 2015-10-30 2019-09-03 General Electric Company System and method for machining workpiece of lattice structure and article machined therefrom
US11549194B2 (en) 2016-12-09 2023-01-10 Hirtenberger Engineered Surfaces Gmbh Electropolishing method and electrolyte for same
AT520365B1 (de) * 2017-08-29 2019-10-15 Hirtenberger Eng Surfaces Gmbh Elektrolyt zum elektropolieren von metalloberflächen
CN109778297B (zh) * 2019-03-25 2020-12-15 山东吉威医疗制品有限公司 一种用于Co-Cr合金支架的电化学抛光液及其抛光方法
CN110724999B (zh) * 2019-10-23 2021-09-28 沈阳航空航天大学 一种用于高Cr含量的CoCrNi多主元合金的电解液及腐蚀工艺
CN112710529B (zh) * 2020-12-18 2022-09-20 国电浙江北仑第三发电有限公司 同时用于服役后hr3c析出物观察和ebsd表征的试样的制备方法
CN113481583B (zh) * 2021-07-30 2022-07-12 南京铖联激光科技有限公司 3d打印用钴铬合金电解腐蚀的电解质溶液与电解方法
CN114908411A (zh) * 2022-05-18 2022-08-16 潍坊赛宝工业技术研究院有限公司 钴铬合金精密零部件表面电解抛光处理材料及其制备方法

Family Cites Families (12)

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AT54186B (de) 1911-03-06 1912-07-10 Wenzel Jirasko Kartothekkasten.
US2378002A (en) * 1940-12-20 1945-06-12 Himmel Brothers Company Electrolytic apparatus
US2645611A (en) * 1948-09-20 1953-07-14 Shwayder Bros Inc Method of and bath for electrolytic polishing
US2928777A (en) * 1950-12-16 1960-03-15 Electro Process Inc Electrolytic polishing of metals
JPS56152999A (en) * 1980-04-25 1981-11-26 Kinki Yakuhin Kogyo Kk Electrolytic polishing liqid of co-cr-type alloy
US4678552A (en) * 1986-04-22 1987-07-07 Pennwalt Corporation Selective electrolytic stripping of metal coatings from base metal substrates
DE19640201A1 (de) * 1996-09-30 1998-04-02 Henkel Ecolab Gmbh & Co Ohg Mittel zur Reinigung von Oberflächen
US7128825B2 (en) * 2001-03-14 2006-10-31 Applied Materials, Inc. Method and composition for polishing a substrate
US6679980B1 (en) 2001-06-13 2004-01-20 Advanced Cardiovascular Systems, Inc. Apparatus for electropolishing a stent
WO2004072332A1 (fr) * 2003-02-12 2004-08-26 Ebara Corporation Fluide de polissage, methode de polissage, et appareil de polissage
DE102004045297A1 (de) * 2004-09-16 2006-03-23 Basf Ag Verfahren zum Behandeln von metallischen Oberflächen unter Verwendung von Formulierungen auf Basis von wasserarmer Methansulfonsäure
US20080067077A1 (en) * 2006-09-04 2008-03-20 Akira Kodera Electrolytic liquid for electrolytic polishing and electrolytic polishing method

Also Published As

Publication number Publication date
EP1903132A3 (fr) 2010-08-25
EP1903132A2 (fr) 2008-03-26
CA2604387C (fr) 2012-07-03
US8080148B2 (en) 2011-12-20
CA2604387A1 (fr) 2008-03-25
US20080289970A1 (en) 2008-11-27
DE102006045221B3 (de) 2008-04-03
JP2008121110A (ja) 2008-05-29
ES2374310T3 (es) 2012-02-15
ATE531836T1 (de) 2011-11-15

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