EP0409785A1 - Electrolyte pour obtenir des couches de conversions noires sur des métaux légers - Google Patents

Electrolyte pour obtenir des couches de conversions noires sur des métaux légers Download PDF

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Publication number
EP0409785A1
EP0409785A1 EP90810539A EP90810539A EP0409785A1 EP 0409785 A1 EP0409785 A1 EP 0409785A1 EP 90810539 A EP90810539 A EP 90810539A EP 90810539 A EP90810539 A EP 90810539A EP 0409785 A1 EP0409785 A1 EP 0409785A1
Authority
EP
European Patent Office
Prior art keywords
mol
electrolyte
layers
conversion layers
potassium
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Withdrawn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
EP90810539A
Other languages
German (de)
English (en)
Inventor
Jürgen Schmidt
Thomas Furche
Roland Erdmann
Marion Reichert
Ullrich Bayer
Peter Dr. Kurze
Thomas Dr. Schwarz
Joachim Dr. Schreckenbach
Hans-Jürgen Kletke
Andreas Dr. Hoffmann
Martin Heppner
Anja Hasse
Dorith Schmidt
Annette Klaus
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.)
Jenoptik AG
Original Assignee
Jenoptik Jena 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 DD33100389A external-priority patent/DD299595A7/de
Priority claimed from DD33100489A external-priority patent/DD299596A7/de
Application filed by Jenoptik Jena GmbH filed Critical Jenoptik Jena GmbH
Publication of EP0409785A1 publication Critical patent/EP0409785A1/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Withdrawn legal-status Critical Current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
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/26—Anodisation of refractory metals or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/026—Anodisation with spark discharge
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12806—Refractory [Group IVB, VB, or VIB] metal-base component
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12806—Refractory [Group IVB, VB, or VIB] metal-base component
    • Y10T428/12812—Diverse refractory group metal-base components: alternative to or next to each other

Definitions

  • the invention relates to electrolytes for producing black, finely matted conversion layers as functional surfaces of assemblies made of lightweight materials, especially titanium materials, by the process of anodic oxidation with spark discharge (ANOF).
  • ANOF anodic oxidation with spark discharge
  • a number of electrolytes for producing conversion layers by means of anodic oxidation with spark discharge on lightweight materials, especially on valve metals such as Ti, Ta, Zr, Nb or Al, are known from the specialist and patent literature.
  • DD-221 762 and DD-229 163 black or gray-black conversion layers on light metals such as Al are described which are achieved by the ANOF process.
  • the disadvantage of these solutions is that they use electrolyte solutions which contain fluorides in particular as NaF or NH4F in addition to dihydrogen phosphates as NaH2PO4, tetraborates as Borax Na2B4O7 and chromates and other third-party additives.
  • the possibility of incorporating non-metallic (carbides, oxides) and metallic components as dispersion layers using fluoride-containing ANOF electrolytes on titanium materials includes the disadvantage of the electrolyte containing fluoride, as well as the disadvantage of poor solubility the components in the electrolyte and all other disadvantages of dispersion layers, such as inhomogeneous structure and the like.
  • the possibility of blackening is not described.
  • DD-A-257 275 refers to decorative coatings, inter alia, on titanium materials which are produced by means of the ANOF process and an electrolyte consisting of NAF, NaH2PO4, Na2B4O7 and potassium hexacyanoferrate-K4 [FE [CN] 6].
  • This solution harbors the great problems of health and environmental protection due to the toxic cyanide-containing electrolyte.
  • the black color is achieved only through the use of hexacyanoferrate, which, similar to the black iron-aluminum spinel, forms a titanium spinel and only serves decorative purposes.
  • valve metals such as Ti, Ta, Zr, Nb, Al, whose radiation physical size optical absorption ( ⁇ ) and thermal emission ( ⁇ ) are almost the same.
  • DD-A-236 978 describes solar-selective absorption layers which consist of dark-colored, chromium-doped oxide layers on valve metals, such as Ti, Ta, Zr, Nb, Al, and which also contain an electrolyte containing fluoride, dihydrogen phosphate, tetraborate and chromate in the ANOF process be generated.
  • valve metals such as Ti, Ta, Zr, Nb, Al
  • these layers have a high absorption capacity of ⁇ > 0.92, they have such a rough surface structure effect that multiple reflections result, so that the incident radiation emits its energy in the form of heat to the absorber layer, which is then transferred to the collector body .
  • a very low thermal emission ⁇ is achieved in relation to the optical absorption.
  • the aim of the invention is to provide an inexpensive, low-pollutant electrolyte for producing simply constructed, optically black, finely matted conversion layers on light metals or their alloys, especially titanium, with high long-term stability and which are characterized by universal applicability.
  • the invention has for its object to develop a fluoride and cyanide-free electrolyte that enables the production of optically black layers with almost the same optical absorption and thermal emissivity, combined with high stability and simultaneous thermal vacuum stability.
  • Black conversion layers are formed on the electrolyte according to the invention
  • Light metals or their alloys, preferably titanium, are obtained by means of anodic oxidation with spark discharge.
  • the electrolyte preferably consists of a 2 to 6 volume percent ammoniacal aqueous solution of 0.3 to 0.6 mol / l potassium dihydrogen phosphate; 0.08 to 0.3 mol / l potassium chromate and acetate ions in concentrations of 0.08 to 1.0 mol / l, preferably 0.08 to 0.5 mol / l.
  • An advantageous embodiment of the solution is that the acetate ions are added in the form of copper acetate.
  • a lens housing made of titanium material degreased in technical acetone is made by means of plasma-chemical anodic oxidation in an aqueous electrolyte consisting of a 4.5 volume percent ammoniacal solution with 0.5 mol / l KH2PO4; 0.1 mol / l K2CrO4 and 0.35 mol / l [CH3 COO] 2Cu coated at a current density of 0.045A.cm ⁇ 2.
  • the ⁇ / ⁇ ratio is 0.95.
  • thermovacuum stability shows no changes in optically relevant areas.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Secondary Cells (AREA)
EP90810539A 1989-07-19 1990-07-16 Electrolyte pour obtenir des couches de conversions noires sur des métaux légers Withdrawn EP0409785A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DD33100389A DD299595A7 (de) 1989-07-19 1989-07-19 Schwarze konversionsschichten auf titanwerkstoffen
DD331004 1989-07-19
DD331003 1989-07-19
DD33100489A DD299596A7 (de) 1989-07-19 1989-07-19 Elektrolyt zur erzeugung schwarzer konversionsschichten auf leichtmetallen

Publications (1)

Publication Number Publication Date
EP0409785A1 true EP0409785A1 (fr) 1991-01-23

Family

ID=25748286

Family Applications (1)

Application Number Title Priority Date Filing Date
EP90810539A Withdrawn EP0409785A1 (fr) 1989-07-19 1990-07-16 Electrolyte pour obtenir des couches de conversions noires sur des métaux légers

Country Status (3)

Country Link
US (2) US5035781A (fr)
EP (1) EP0409785A1 (fr)
DE (1) DE4017711A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ITMI20082275A1 (it) * 2008-12-19 2010-06-20 Italfinish Spa Procedimento elettrolitico per l'ottenimento di rivestimenti scuri o neri su materiali metallici non ferrosi

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4239391C2 (de) * 1991-11-27 1996-11-21 Electro Chem Eng Gmbh Gegenstände aus Aluminium, Magnesium oder Titan mit einer mit Fluorpolymeren gefüllten Oxidkeramikschicht und Verfahren zu ihrer Herstellung
DE4139006C3 (de) * 1991-11-27 2003-07-10 Electro Chem Eng Gmbh Verfahren zur Erzeugung von Oxidkeramikschichten auf sperrschichtbildenden Metallen und auf diese Weise erzeugte Gegenstände aus Aluminium, Magnesium, Titan oder deren Legierungen mit einer Oxidkeramikschicht
DE202004020372U1 (de) * 2003-04-16 2005-06-02 AHC-Oberflächentechnik GmbH Gegenstand
EP1587348A1 (fr) * 2004-03-30 2005-10-19 Feng Chia University Plaque de base conductrice
TW201621096A (zh) * 2014-12-05 2016-06-16 財團法人金屬工業研究發展中心 黑色含鈦氧化層及其製備方法、以及植入物
CN105177672B (zh) * 2015-09-15 2017-10-03 哈尔滨工业大学 一种钛合金表面高太阳能吸收率高发射率黑色消光膜层的制备方法

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE236978C (fr) *
DD229163A1 (de) * 1984-11-21 1985-10-30 Karl Marx Stadt Tech Hochschul Elektrolyte zur erzeugung eigenfarbiger schichten auf sperrschichtbildenden metallen

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2330170A (en) * 1939-09-08 1943-09-21 Crane Co Electrolytic polishing of metal
US3268306A (en) * 1962-03-28 1966-08-23 Trw Inc Titanium pretreatment for protective coating of refractory alloys
US3446606A (en) * 1965-07-14 1969-05-27 United Aircraft Corp Refractory metal articles having oxidation-resistant coating
US3489522A (en) * 1965-10-15 1970-01-13 Synvar Ass Electron spin resonance labeling of biomolecules
SU742493A1 (ru) * 1978-11-01 1980-06-25 Харьковский Ордена Ленина Политехнический Институт Им.В.И.Ленина Раствор дл электрохимического полировани металлов
DE3102207A1 (de) * 1980-01-29 1981-11-19 Mitsubishi Denki K.K., Tokyo Funkenerrosionsbearbeitungsloesung und deren anwendung
US4305998A (en) * 1980-02-04 1981-12-15 The United States Of America As Represented By The Secretary Of The Navy Protective coating
US4448853A (en) * 1981-04-15 1984-05-15 Bbc Brown, Boveri & Company, Limited Layered active brazing material and method for producing it
JPS58143919A (ja) * 1982-02-16 1983-08-26 Fanuc Ltd 放電加工方法

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE236978C (fr) *
DD229163A1 (de) * 1984-11-21 1985-10-30 Karl Marx Stadt Tech Hochschul Elektrolyte zur erzeugung eigenfarbiger schichten auf sperrschichtbildenden metallen

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
CRYSTAL RES. TECHN., Band 22, 1987, Seiten 53-58; P. KURZE et al.: "Coloured ANOF layers on aluminium" *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ITMI20082275A1 (it) * 2008-12-19 2010-06-20 Italfinish Spa Procedimento elettrolitico per l'ottenimento di rivestimenti scuri o neri su materiali metallici non ferrosi

Also Published As

Publication number Publication date
US5075178A (en) 1991-12-24
DE4017711A1 (de) 1991-01-31
US5035781A (en) 1991-07-30

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