EP1911862A2 - Procédé d'électropolissage pour niobium et tantale - Google Patents

Procédé d'électropolissage pour niobium et tantale Download PDF

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Publication number
EP1911862A2
EP1911862A2 EP07018328A EP07018328A EP1911862A2 EP 1911862 A2 EP1911862 A2 EP 1911862A2 EP 07018328 A EP07018328 A EP 07018328A EP 07018328 A EP07018328 A EP 07018328A EP 1911862 A2 EP1911862 A2 EP 1911862A2
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EP
European Patent Office
Prior art keywords
electrolyte
niobium
tantalum
electropolishing
concentration
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.)
Granted
Application number
EP07018328A
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German (de)
English (en)
Other versions
EP1911862B1 (fr
EP1911862A3 (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 EP1911862A3 publication Critical patent/EP1911862A3/fr
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    • 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 metals and metal alloys, in particular of such metals and metal alloys, which are selected from the group consisting of niobium, niobium alloys, tantalum and tantalum alloys.
  • the present invention includes an electrolyte for electropolishing surfaces of these metals and metal alloys. This electrolyte contains methanesulfonic acid and ammonium bifluoride, NH 4 HF 2 .
  • the process of electrochemical polishing or electropolishing serves to produce metal surfaces of high purity, to smooth and deburr metal surfaces. Smoothing in the micro-region causes the surfaces thus treated to be high-gloss. In addition, by the electropolishing stresses in the outer material layers can be removed.
  • the prior art discloses a variety of different electropolishing methods that can be used to process various metals and metal alloys. In general, these methods are based on the use of electrolytes containing a concentrated mineral acid or a mixture of concentrated mineral acids, to which additives are often added in order to further improve the effect of the electrolytes, and thus to obtain smoother and more lustrous metal surfaces.
  • Niobium often called niobium
  • niobium and tantalum are used both as pure metals and as constituents of alloys with one another and / or with other metals in the production of workpieces, for example of gas turbines or in engine construction.
  • a method using an electrolyte consisting of a mixture of concentrated sulfuric acid and hydrofluoric acid in the ratio of about 90:10 is used for the electropolishing of niobium.
  • this electrolyte releases large quantities of gaseous hydrogen fluoride, which is toxic and corrosive. In order to minimize the risk to humans and the environment, this procedure can therefore only be carried out under the strictest and most complex safety measures.
  • Another disadvantage of this method is that this electrolyte also chemically attacks the niobium surface, especially when the current flow is interrupted. Significant amounts of hydrogen are released, some of which also diffuse into the metal surface and then have to be removed again at great expense by heating under vacuum.
  • the machined workpieces In order to keep the chemical attack of the electrolyte on the electropolished surface as low as possible, therefore, the machined workpieces usually have to be cooled very rapidly after switching off the current. be taken out of the bath within a few seconds and be completely rinsed. This rapid flushing often requires special equipment and is therefore also associated with high costs. Therefore, the method quickly reaches its limits, especially when working with larger components, and has limited application.
  • the patent application WO 01/71068 A1 discloses electrolytic polishing processes wherein, among others, tantalum and niobium are electropolished with an electrolyte of methanesulfonic acid and methanol. While this tantalum electropolishing process appears to have good results, there is no indication of the quality of the electropolishing process in niobium surface processing.
  • the Japanese Patent Application JP 60092500 A2 uses a mixture of sulfuric acid and fluorosulfonic acid (fluorosulfuric acid). Although no toxic hydrofluoric acid gases are released, the use of fluorosulphonic acid is extremely complex and expensive because of the high reactivity to a contact between fluorosulfonic acid and air to avoid largely, as this toxic vapors may also arise.
  • Figure 1 shows the decrease of the roughness values Ra and Rz in the electropolishing of a sheet of pure niobium according to the method according to the present invention (see Example 1).
  • the present invention is a process for electropolishing surfaces of metals and metal alloys, which is particularly suitable for the processing of surfaces of niobium, niobium alloys, tantalum and tantalum alloys.
  • Niobium and tantalum alloys are understood as meaning both solid phase mixtures and compounds of niobium and tantalum with one another and of one or both metals with other elements which have a metallic character or else form intermetallic compounds.
  • the application of this procedure is largely safe for humans and the environment.
  • an electrolyte containing methanesulfonic acid and ammonium bifluoride (ammonium hydrogen difluoride, NH 4 + HF 2 - ) is used. This electrolyte is also an object of the present invention.
  • the concentration of methanesulfonic acid used in the electrolyte is more than 80%.
  • concentration of methanesulfonic acid in the electrolyte is at least 90%.
  • the concentration of ammonium hydrogendifluoride in the electrolyte is between 5 and 100 g / l, preferably between 20 and 70 g / l. If the metal surface is a niobium or niobium alloy surface is particularly preferred that the concentration of ammonium hydrogen difluoride in the electrolyte is about 40 g / l. If the metal surface consists predominantly or exclusively of tantalum or a tantalum alloy, the best results can be obtained with a concentration of ammonium hydrogen difluoride of about 60 g / l in the electrolyte.
  • the electrolyte contains no further acids in addition to the methanesulfonic acid.
  • the electrolyte contains no appreciable constituents of phosphoric acid, sulfuric acid, nitric acid and free hydrofluoric acid.
  • an electrolyte according to the present invention may form about a binary system consisting only of methanesulfonic acid and ammonium bifluoride.
  • electropolishing method allows the rinsing of the machined workpieces not to take place within a few seconds, but can take place in a period of time which is usual for other metals in the conventional electropolishing method. This makes it possible for the first time also a trouble-free electrochemical polishing of surfaces of larger components or components with difficult to flush surfaces.
  • the process according to the invention is carried out at a temperature between 10 ° C and 50 ° C.
  • the electrolyte can safely remain on the electropolished surfaces for a long time Components remain and are subsequently rinsed with water without the surfaces being attacked during one of the steps.
  • a significant advantage of using the method described here is that no special measures for the protection of man and the environment are required.
  • the handling of an electrolyte containing methanesulfonic acid and ammonium bifluoride can be carried out without further safety precautions, which go beyond the usual protective measures for the handling of strong concentrated acids.
  • the fluoride ions from the ammonium hydrogen difluoride are chemically bound by the metal removed in the course of the electropolishing process.
  • Example 1 Electropolishing of niobium
  • the sheet was rinsed in demineralized water and dried in air.
  • the sheet was rinsed in demineralized water and dried in air.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • ing And Chemical Polishing (AREA)
  • Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)
  • Electroplating Methods And Accessories (AREA)
EP07018328.0A 2006-10-09 2007-09-18 Procédé d'électropolissage pour niobium et tantale Not-in-force EP1911862B1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE102006047713A DE102006047713B3 (de) 2006-10-09 2006-10-09 Elektropolierverfahren für Niob und Tantal und Elektrolyt

Publications (3)

Publication Number Publication Date
EP1911862A2 true EP1911862A2 (fr) 2008-04-16
EP1911862A3 EP1911862A3 (fr) 2010-08-25
EP1911862B1 EP1911862B1 (fr) 2017-03-01

Family

ID=38786963

Family Applications (1)

Application Number Title Priority Date Filing Date
EP07018328.0A Not-in-force EP1911862B1 (fr) 2006-10-09 2007-09-18 Procédé d'électropolissage pour niobium et tantale

Country Status (5)

Country Link
US (1) US20080099345A1 (fr)
EP (1) EP1911862B1 (fr)
JP (1) JP2008095192A (fr)
CA (1) CA2605859A1 (fr)
DE (1) DE102006047713B3 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9499919B2 (en) 2010-11-22 2016-11-22 MetCon LLC Electrolyte solution and electrochemical surface modification methods
EA036890B1 (ru) * 2010-11-22 2021-01-12 МЕТКОН, ЭлЭлСи Раствор электролита и электрохимические способы модификации поверхности
RU2817245C1 (ru) * 2023-12-18 2024-04-12 федеральное государственное бюджетное образовательное учреждение высшего образования "Уфимский университет науки и технологий" Способ электролитно-плазменного полирования детали в разреженной атмосфере

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100213078A1 (en) * 2009-02-25 2010-08-26 Ryszard Rokicki Electrolyte composition for electropolishing niobium and tantalum and method for using same
WO2011063353A2 (fr) * 2009-11-23 2011-05-26 Metcon, Llc Solution d'électrolyte et procédés d'électropolissage
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.
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
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

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4663005A (en) * 1985-11-15 1987-05-05 Edson Gwynne I Electropolishing process
US5632966A (en) * 1996-03-07 1997-05-27 Alliedsignal Inc. Process for hydrogen fluoride separation
US6352636B1 (en) * 1999-10-18 2002-03-05 General Electric Company Electrochemical system and process for stripping metallic coatings
US6407047B1 (en) * 2000-02-16 2002-06-18 Atotech Deutschland Gmbh Composition for desmutting aluminum
NL1014727C2 (nl) * 2000-03-23 2001-09-25 Univ Eindhoven Tech Werkwijze voor het elektrolytisch polijsten van een metaal in aanwezigheid van een elektrolytsamenstelling, alsmede een vormdeel verkregen volgens een dergelijke werkwijze.
DE10259934B3 (de) * 2002-12-20 2004-10-14 H.C. Starck Gmbh Verfahren zur Herstellung von Formteilen aus Niob oder Tantal durch elektrochemisches Ätzen und so erhältliche Formteile
DE10320909A1 (de) * 2003-05-09 2004-11-18 Poligrat Holding Gmbh Elektrolyt zum elektrochemischen Polieren von Metalloberflächen

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9499919B2 (en) 2010-11-22 2016-11-22 MetCon LLC Electrolyte solution and electrochemical surface modification methods
EA036890B1 (ru) * 2010-11-22 2021-01-12 МЕТКОН, ЭлЭлСи Раствор электролита и электрохимические способы модификации поверхности
RU2817245C1 (ru) * 2023-12-18 2024-04-12 федеральное государственное бюджетное образовательное учреждение высшего образования "Уфимский университет науки и технологий" Способ электролитно-плазменного полирования детали в разреженной атмосфере

Also Published As

Publication number Publication date
EP1911862B1 (fr) 2017-03-01
JP2008095192A (ja) 2008-04-24
US20080099345A1 (en) 2008-05-01
EP1911862A3 (fr) 2010-08-25
CA2605859A1 (fr) 2008-04-09
DE102006047713B3 (de) 2008-03-27

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