EP1625246B1 - Elektrolyt zum elektrochemischen polieren von metalloberflächen - Google Patents

Elektrolyt zum elektrochemischen polieren von metalloberflächen Download PDF

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Publication number
EP1625246B1
EP1625246B1 EP04730514A EP04730514A EP1625246B1 EP 1625246 B1 EP1625246 B1 EP 1625246B1 EP 04730514 A EP04730514 A EP 04730514A EP 04730514 A EP04730514 A EP 04730514A EP 1625246 B1 EP1625246 B1 EP 1625246B1
Authority
EP
European Patent Office
Prior art keywords
electrolyte
alloys
titanium
niobium
tantalum
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.)
Expired - Lifetime
Application number
EP04730514A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP1625246A2 (de
Inventor
Siegfried Piesslinger-Schweiger
Razmik Abedian
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-HOLDING GmbH
Original Assignee
Poligrat-Holding GmbH
Poligrat Holding 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
Application filed by Poligrat-Holding GmbH, Poligrat Holding GmbH filed Critical Poligrat-Holding GmbH
Priority to PL04730514T priority Critical patent/PL1625246T3/pl
Publication of EP1625246A2 publication Critical patent/EP1625246A2/de
Application granted granted Critical
Publication of EP1625246B1 publication Critical patent/EP1625246B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime 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 electrolytes for the electrochemical polishing of workpieces of titanium, titanium alloys, niobium, niobium alloys, tantalum and tantalum alloys, and to a process for electrochemical polishing.
  • the electrochemical polishing or glazing of metal surfaces is widely used in the art to treat smaller or larger metal objects. Due to the rapidly increasing use of titanium and titanium alloys in the field of apparatus engineering, vehicle construction, aircraft construction or even medical technology, the surface treatment of these materials by electropolishing is becoming increasingly important.
  • electropolishing the articles to be polished which hang on respective support members or are arranged in baskets or the like are introduced into the electrolyte, i. H. the polishing bath, sunk and lifted out of this after a certain polishing time. After draining the bath liquid from the polished surfaces, the articles are then immersed in rinsing baths to remove the electrolyte.
  • Electrolytes which contain hydrofluoric acid in significant concentrations as described in the French patent FR 2795433 involve a significant safety and health risk due to the high toxicity and corrosivity of the hydrofluoric acid, which escapes in significant amounts from the electrolyte during the electropolishing process.
  • the operation of electropolishing with such electrolyte requires complex safety precautions.
  • the loss of hydrofluoric acid via the exhaust air must be added regularly in order to keep the electropolishing process stable.
  • the contacting of the electropolishing workpieces in the aforementioned electrolyte must either consist of similar material or pure titanium.
  • the contact material is attacked equally and must be renewed regularly. This represents a significant cost factor in terms of the value of these metals and leads to premature wear of the electrolytes. Furthermore, it is thus not possible to unambiguously allocate the current distribution and thus the respective removal rates to the individual workpieces and the contact material. In the case of high demands on the accuracy of the electropolishing process, this represents an additional factor of uncertainty.
  • the workpieces must be individually stable, eg. B. by clamping, and can not be processed loosely as bulk material in drums or baskets. This causes at small mass parts such. B. screws considerable costs by the necessary manual assembly of the contact frames.
  • the object of the invention is to provide an electrolyte which is suitable for the electropolishing of titanium, titanium alloys including nickel-titanium alloys (nitinol), niobium, niobium alloys including niobium-zirconium alloys as well as tantalum and tantalum alloys.
  • an electropolishing process for such metals is to be provided that can be carried out easily and safely.
  • the electrolytes according to the invention consist of mixtures of sulfuric acid, ammonium bifluoride and at least one hydroxycarboxylic acid.
  • electrolytes according to the invention are neither explosive nor combustible. In addition, they contain no hydrofluoric acid in excess, which could escape during the electropolishing process as hydrofluoric acid gaseous and cause no odor.
  • metals can be electropolished with the electrolytes according to the invention. These include titanium, titanium alloys including nickel-titanium alloys, niobium, niobium alloys including niobium-zirconium alloys, as well as tantalum and tantalum alloys.
  • electrolytes according to the invention are suitable for electropolishing nitinol, which is a high-strength nickel-titanium alloy with 55% Ni.
  • the electropolishing result can be optimized by changing the mixing ratio of the three components within certain concentration ranges.
  • Hydroxycarboxylic acids used are preferably hydroxylated C 1 -C 6 -carboxylic acids.
  • the hydroxycarboxylic acids can be present in the electrolyte according to the invention in a concentration of 10-80% by volume, preferably 20-60% by volume.
  • Preferred hydroxycarboxylic acids include glycolic acid and hydroxypropionic acid.
  • the hydroxycarboxylic acids are preferably introduced as 60-80% solutions. It is also possible to use combinations of different hydroxycarboxylic acids.
  • An electrolyte according to the present invention may contain the sulfuric acid in a concentration of 90-20% by volume, preferably 80-40% by volume. Preferably, 96% sulfuric acid is used.
  • ammonium bifluoride can be used in the electrolyte according to the invention in a concentration of 10-150 g per liter, preferably 40-85 g per liter.
  • the corresponding metals can be electropolished efficiently and cleanly.
  • Part of the invention is also a method for the electrochemical polishing of workpieces made of titanium, titanium alloys, niobium, niobium alloys, tantalum and tantalum alloys, in which an inventive electrolyte is used.
  • an advantage of the method according to the invention is that the application parameters of the method can be varied within a wide range, which considerably facilitates the process control. In the prior art, however, the application parameters had to be kept within narrow limits.
  • the inventive method for polishing workpieces made of nickel-titanium alloys, such as nitinol, or niobium-zirconium alloys is used.
  • the method can be carried out at a temperature of 0 ° C to 40 ° C, a DC electrical voltage of 10 V to 35 V and a current density of 0.5 to 10 A / dm 2 .
  • Another advantage of the present invention is that not only the materials to be electropolished can be used as the contact material, but also that aluminum can be used which is inexpensive to purchase and is not attacked by the electropolishing process. This makes it possible to unambiguously allocate the current density to the workpieces to be electropolished and thus control the removal within narrower tolerances.
  • Another advantage of the method according to the invention is that free-flowing mass parts can be processed inexpensively in drums or baskets made of aluminum as loose bulk material.

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)
EP04730514A 2003-05-09 2004-04-30 Elektrolyt zum elektrochemischen polieren von metalloberflächen Expired - Lifetime EP1625246B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PL04730514T PL1625246T3 (pl) 2003-05-09 2004-04-30 Elektrolit do elektrochemicznego polerowania powierzchni metalowych

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10320909A DE10320909A1 (de) 2003-05-09 2003-05-09 Elektrolyt zum elektrochemischen Polieren von Metalloberflächen
PCT/EP2004/004600 WO2004100283A2 (de) 2003-05-09 2004-04-30 Elektrolyt zum elektrochemischen polieren von metalloberflächen

Publications (2)

Publication Number Publication Date
EP1625246A2 EP1625246A2 (de) 2006-02-15
EP1625246B1 true EP1625246B1 (de) 2006-09-13

Family

ID=33305203

Family Applications (1)

Application Number Title Priority Date Filing Date
EP04730514A Expired - Lifetime EP1625246B1 (de) 2003-05-09 2004-04-30 Elektrolyt zum elektrochemischen polieren von metalloberflächen

Country Status (10)

Country Link
US (1) US7807039B2 (pl)
EP (1) EP1625246B1 (pl)
JP (1) JP4592683B2 (pl)
AT (1) ATE339534T1 (pl)
CA (1) CA2525138A1 (pl)
DE (2) DE10320909A1 (pl)
DK (1) DK1625246T3 (pl)
ES (1) ES2271882T3 (pl)
PL (1) PL1625246T3 (pl)
WO (1) WO2004100283A2 (pl)

Families Citing this family (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102006047713B3 (de) * 2006-10-09 2008-03-27 Poligrat Gmbh Elektropolierverfahren für Niob und Tantal und Elektrolyt
DE102007011632B3 (de) 2007-03-09 2008-06-26 Poligrat Gmbh Elektropolierverfahren für Titan
US20100213078A1 (en) * 2009-02-25 2010-08-26 Ryszard Rokicki Electrolyte composition for electropolishing niobium and tantalum and method for using same
US20110017608A1 (en) * 2009-07-27 2011-01-27 Faraday Technology, Inc. Electrochemical etching and polishing of conductive substrates
WO2011063353A2 (en) * 2009-11-23 2011-05-26 Metcon, Llc Electrolyte solution and electropolishing methods
US20110303553A1 (en) * 2010-06-11 2011-12-15 Inman Maria E Electrochemical system and method for machining strongly passivating metals
US8580103B2 (en) 2010-11-22 2013-11-12 Metcon, Llc Electrolyte solution and electrochemical surface modification methods
CN102225504B (zh) * 2011-04-06 2013-12-25 宝鸡鑫泽钛镍有限公司 高精度钛及钛合金板制备工艺
CN102677142B (zh) * 2012-05-16 2015-07-08 安徽华东光电技术研究所 一种用于行波管螺旋线的电化学抛光方法
KR101600428B1 (ko) * 2014-07-15 2016-03-07 한국화학연구원 중이온 가속관의 나이오븀 식각방법
EP3109348B1 (en) * 2015-06-24 2020-06-03 Airbus Defence and Space GmbH Electrolyte and process for the electrolytic polishing of a metallic substrate
WO2018102845A1 (de) * 2016-12-09 2018-06-14 Hirtenberger Engineered Surfaces Gmbh Elektropolierverfahren und elektrolyt hierzu
CN107937977A (zh) * 2017-12-20 2018-04-20 西安泰金工业电化学技术有限公司 一种阴极辊电解抛光液及抛光方法
JP6671763B2 (ja) * 2018-02-28 2020-03-25 三愛プラント工業株式会社 電解研磨液及び電解研磨方法
JP7313664B2 (ja) * 2019-06-17 2023-07-25 マルイ鍍金工業株式会社 電解研磨方法
DE102020200815A1 (de) 2020-01-23 2021-07-29 Mahle International Gmbh Zusammensetzung als Elektrolyt zum Auflösen und/oder Abscheiden von Metallen, Metalloxiden und/oder Metalllegierungen sowie Verwendungen dieser Zusammensetzung

Family Cites Families (15)

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Publication number Priority date Publication date Assignee Title
NL93969C (pl) 1955-05-09
DK574274A (pl) * 1973-12-06 1975-07-28 Ciba Geigy Ag
DE3461202D1 (en) * 1983-08-23 1986-12-11 Bbc Brown Boveri & Cie Process for electrolytically polishing a work piece made of a nickel, cobalt or iron based alloy
JPH02310400A (ja) * 1989-05-22 1990-12-26 Nec Corp マグネシウム上のめっき皮膜を剥離する方法
JPH0394100A (ja) * 1989-09-04 1991-04-18 Canon Inc 電解研磨液及び電解研磨方法
JP3291512B2 (ja) * 1995-03-16 2002-06-10 日本パーオキサイド株式会社 過酸化水素、フッ化水素アンモニウム、及び硫酸を含有する酸性溶液の安定剤、及びこれを用いた鉄−ニッケル合金の化学的溶解処理液
US5861535A (en) * 1997-09-23 1999-01-19 Eastman Kodak Company Reductive alkylation process to prepare tertiary aminoaryl compounds
US6447664B1 (en) 1999-01-08 2002-09-10 Scimed Life Systems, Inc. Methods for coating metallic articles
JP3318656B2 (ja) * 1999-04-08 2002-08-26 独立行政法人産業技術総合研究所 チタン複合材料
FR2795433B1 (fr) 1999-06-25 2001-08-31 Org Europeene De Rech Composition de bain pour le polissage electrolytique du titane, et son procede d'utilisation
US6352636B1 (en) * 1999-10-18 2002-03-05 General Electric Company Electrochemical system and process for stripping metallic coatings
KR100400030B1 (ko) 2000-06-05 2003-09-29 삼성전자주식회사 금속막의 화학 및 기계적 연마용 슬러리 및 그 제조방법과상기 슬러리를 이용한 반도체 소자의 금속 배선 형성 방법
US7128825B2 (en) * 2001-03-14 2006-10-31 Applied Materials, Inc. Method and composition for polishing a substrate
JP3484525B2 (ja) * 2001-07-06 2004-01-06 株式会社ケミカル山本 ステンレス鋼表面の清浄、不動態化処理方法
US7357854B1 (en) * 2002-08-19 2008-04-15 Advanced Cardiovascular Systems, Inc. Process for electropolishing a device made from cobalt-chromium

Also Published As

Publication number Publication date
JP2006526071A (ja) 2006-11-16
PL1625246T3 (pl) 2006-12-29
ATE339534T1 (de) 2006-10-15
DE10320909A1 (de) 2004-11-18
ES2271882T3 (es) 2007-04-16
DE502004001497D1 (de) 2006-10-26
US20070029209A1 (en) 2007-02-08
WO2004100283A2 (de) 2004-11-18
DK1625246T3 (da) 2006-11-13
WO2004100283A3 (de) 2004-12-09
EP1625246A2 (de) 2006-02-15
US7807039B2 (en) 2010-10-05
CA2525138A1 (en) 2004-11-18
JP4592683B2 (ja) 2010-12-01

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