US3562013A - Process of deoxidizing titanium and its alloys - Google Patents

Process of deoxidizing titanium and its alloys Download PDF

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Publication number
US3562013A
US3562013A US677086A US3562013DA US3562013A US 3562013 A US3562013 A US 3562013A US 677086 A US677086 A US 677086A US 3562013D A US3562013D A US 3562013DA US 3562013 A US3562013 A US 3562013A
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US
United States
Prior art keywords
titanium
acid
bath
nitric acid
alloys
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Expired - Lifetime
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US677086A
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English (en)
Inventor
Floyd Louis Mickelson
Wilbert Joseph Roberts
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Diversey Wyandotte Corp
Diversey Corp USA
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Diversey Corp USA
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Assigned to DIVERSEY WYANDOTTE CORPORATION, A CORP. OF DE. reassignment DIVERSEY WYANDOTTE CORPORATION, A CORP. OF DE. ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: DIVERSEY CORPORATION THE
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/10—Other heavy metals
    • C23G1/106—Other heavy metals refractory metals
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F3/00—Brightening metals by chemical means
    • C23F3/04—Heavy metals
    • C23F3/06—Heavy metals with acidic solutions

Definitions

  • This invention relates to processes for cleaning, deoxidizing and brightening titanium and its alloys.
  • Titanium and titanium alloys develop a resistant oxide scale during manufacturing processes involving heat treatment and fabrication. Proper finishing requires that this adherent oxide be removed with minimum or no adverse eifects to the article.
  • Molten salt baths require extremely high temperatures and normally produce a stained surface.
  • the stain is usually removed with a post-treatment to complete the process. It is impractical to descale large articles with this process.
  • Hydrogen embrittlment represents a major problem in treating titanium and its alloys after heat treating, welding and other scale forming processes. Removing the heavy oxide with the standard aqueous hydrofluoric acid, nitric acid and hydrochloric acid baths produces hydrogen absorption. Hydrogen absorption into the titanium intergranular structure produces hydrogen embrittlement causing structural cracks and failure under stress. This absoption of hydrogen is irreversible. It cannot be baked out, as with high strength steels.
  • this invention is a process for cleaning and deoxidizing titanium and its alloys which produces a stain free, smooth bright surface with inhibition of hydrogen absorption and consequent embrittlement.
  • the process also gives substantially or essentially smut free surfaces even with titanium alloys which normally produce smutty surfaces with other processes.
  • the surfaces of titanium and titanium-based alloys can be deoxidized and cleaned by bringing the surface into contact with a bath of the following composition:
  • hydrofluoric acid is considered to encompass hydrofluoric acid as well as the resulting acids formed by the utilization of salts in the solutions to provide the needed bydrofluoric acid and/or the equivalent acid fluoride ion.
  • the salts which can be used are the alkali metal silicofluorides such as sodium or potassium silicofluoride, ammonium bifluoride, calcium bifluoride, and alkali metal bifluorides such as sodium or potassium bifluoride, an alkali metal fluoride and particularly sodium, potassium or lithium fluoride, or fluoro boric acid.
  • the bath can also be used with a mixture of such hydrofluoric acid or acid fluoride ion supplying materials.
  • the described baths dissolve or remove surface oxides from titanium and titanium-based alloys Without etching the surface, leaving it clean and bright, with low hydrogen absorption thus minimizing or eliminating hydrogen embrittlement.
  • the process is also characterized by an essential lack of smut adherence on the surface.
  • the surfaces also seem to be made passive by the treatment.
  • Phosphoric acid also serves to suppress etching. It is accordingly usually beneficial to include at least 5% phosphoric acid in the bath.
  • a particularly useful deoxidizing bath for titanium and its alloys can have 025% Water, 1055% sulfuric acid, 3052% nitric acid, 0-25 phosphoric acid and l-l0% ammonium bifluoride with the percentages of the acids and bifluoride being on an anhydrous basis.
  • surfactants it is acceptable, but generally unnecessary, to include one or more surfactants in the deoxidizing bath.
  • Some surfactants which can be used are metal sulfates such as alkali metal alkyl sulfates such as sodium lauryl sulfate and sodium nonyl sulfate, and sulfated alcohols such as sulfated tridecyl alcohol. From about 0.01% to 5% of a surfactant can be included if advisable.
  • Deoxidizing, cleaning and/or brightening of titanium and its alloys is readily effected by contacting the metal surface with the bath. Although this can be done successfully with the bath at ambient temperature, it is usually more satisfactory to employ the bath at about 30-140" F. Contact times of about 30 seconds to 25 minutes are often adequate for effecting the desired treatment.
  • the titanium or titanium alloy surface can be rinsed with cold water and air dried.
  • EXAMPLE 1 Unalloyed titanium, TiA, was treated in a solution consisting of 23.4% sulfuric acid, 37.9% nitric acid, 20.9% phosphoric acid, 5.9% ammonium bifluoride, 3.9% sodium silicofluoride and the remainder water. This treatment at 75 F., for 5 minutes produced a bright oxide free surface. Analysis revealed hydrogen absorption was in the order of 78 ppm.
  • EXAMPLE 2 Unalloyed titanium, heat treated at 1000 F., was treated as described in Example 1 for three minutes at 80 F. The treated titanium surface was bright, clean and oxide free. On analysis, the hydrogen absorption was found to be 69 ppm.
  • Example 1 was repeated adding 0.5% sodium lauryl sulfate surfactant to the solution. After 1 minute at 78 F, the surface was clean and bright. Chemical analysis revealed hydrogen absorption was in the order of 66 ppm.
  • Example 1 was repeated using 3.9% calcium fluoride in place of 3.9% sodium silicofluoride. This treatment produced a bright, clean oxide free surface.
  • Example 1 was repeated using the alloy Ti-8Al-lMo-1V consisting of 8% aluminum, 1% molybdenum, 1% va- 30 nadium and the remainder titanium. Microscopic analysis of the bright clean surface revealed no titanium hydride formation. In contrast, treating the alloy with the standard bath of 1 part hydrofluoric acid and 10 parts nitric acid, used under the same conditions, produced a dark, rough surface showing titanium hydride formation sufficient to produce hydrogen embrittlement.
  • Example 1 was repeated using the alpha-beta alloy Ti-6Al-4V consisting of 6% aluminum, 4% vanadium and the remainder titanium. The heavy marking ink on the surface was removed and a bright clean surface was produced.
  • Example 9 Example 6 was repeated with an annealed sheet of alpha-beta alloy Ti-8Mn containing 8% manganese as its principal alloying constituent. Black marking ink stencil was removed and a bright clean surface produced. Analysis revealed no titanium hydride formation.
  • Example 5 was repeated with a titanium alpha alloy forging RSllC containing aluminum and 2.5% tin as the principal alloying constituents. A clean bright smutfree surface was produced. By contrast, a nitric acid-hydrofluoric acid bath consisting of 5% hydrofluoric acid, nitric acid and the remainder water at room temperature for 3 minutes produced a dark smutty surface.
  • Example 1 was repeated using a titanium alpha alloy sheet Ti-5Al-2.5Sn containing 5% aluminum and 2.5% tin as the principal alloying constituents. A bright clean surface having less than 0.0001 inch per side dimensional change was produced. By contrast, a conventional bath consisting of nitric acid, 20% hydrochloric acid, 5% hydrofluoric acid and the remainder water produced a rough smutty surface with a dimensional change of 0.003 inch per side.
  • EXAMPLE 12 Unalloyed titanium alloy Ti65, having a nominal composition of 99% titanium was treated in a bath consisting of 55% sulfuric acid, 40% nitric acid and 5% ammonium bifluoride at F for 10 minutes. A green marking ink was removed and a bright, oxide free surface was produced. This deoxidized article retained its bright satin finish for several days. By contrast, the same alloy deoxidized in a bath consisting of 10% nitric acid, 1% hydrofluoric acid and the remainder water produced a rough surface with smut and failed to remove the marking ink. Standing overnight, the treated surface developed a bluish stain or discoloration.
  • EXAMPLE l3 Unalloyed titanium Ti65 was treated with the first bath described in Example 12, at 120 F. for 5 minutes, instead of 80 F. for 10 minutes. A bright smut free surface was produced. By contrast, a 10% nitric acid, 1% hydrofluoric acid bath at 120 F. produced deep etching, heavy gasing and a dark smut.
  • EXAMPLE 14 Titanium alloy RS-70 was treated in the bath described in Example 14 at 120 F. for 5 minutes, instead of 75 F. for 10 minutes. A bright smut free surface was produced. By contrast, a bath of 10% nitric acid, 1% hydrochloric acid and the remainder water at F. for 3 minutes produced a dark rough finish.
  • Titanium alloy Ti65 nominally consisting of 99 %titanium was treated in a bath consisting of 40% sulfuric acid, 20% phosphoric acid, 30% nitric acid, 5% water and 5% ammonium bifluoride at F. for 10 minutes. A bright, smut free surface was produced. By contrast, a bath consisting of 30% nitric acid, 3% hydrofluoric acid and the remainder water at 120 F. for 5 minutes produced a dark rough surface.
  • the method of claim 1 in which the minimum phos phoric acid content is 5% 6.
  • the method of deoxidizing and cleaning a titanium or titanium-lfised alloy surface which comprises contacting the surface with a bath consisting essentially of 1050% by weight of sulfuric acid, 3052% by weight of nitric acid, -25% by weight of phosphoric acid, 0--25% by weight of water and l30% by weight of ammonium bifluoride, calcium bifluoride, an alkali metal bifiuoride, alkali metal silicofiuoride, an alkali metal fluoride or an alkali metal fiuoro boric acid.
  • the bath consists essentially of 25% sulfuric acid, 5% phosphoric acid, 40% nitric acid, 5% ammonium bifluoride and 25% water.
  • the bath consists essentially of 40% sulfuric acid, 20% phosphoric acid, nitric acid, 5% water and 5% ammonium bifluoride.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • ing And Chemical Polishing (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
US677086A 1967-10-23 1967-10-23 Process of deoxidizing titanium and its alloys Expired - Lifetime US3562013A (en)

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US67708667A 1967-10-23 1967-10-23

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US (1) US3562013A (xx)
BE (1) BE722726A (xx)
CH (1) CH505916A (xx)
FR (1) FR1589844A (xx)

Cited By (24)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3753815A (en) * 1971-09-22 1973-08-21 Armco Steel Corp Method and bath for treating titanium
US3994817A (en) * 1975-07-28 1976-11-30 Rockwell International Corporation Etchant for etching silicon
US4002489A (en) * 1973-06-21 1977-01-11 Nyby Bruk Ab Method of pickling metallic material
US4220706A (en) * 1978-05-10 1980-09-02 Rca Corporation Etchant solution containing HF-HnO3 -H2 SO4 -H2 O2
US4277289A (en) * 1978-07-19 1981-07-07 Aluminum Pechiney Process for removing titaniferous and silico-aluminous incrustations from surfaces
US4322264A (en) * 1975-12-09 1982-03-30 U.S. Philips Corporation Method for selective etching of titaniumdioxide relative to aluminum
US4525250A (en) * 1980-12-19 1985-06-25 Ludwig Fahrmbacher-Lutz Method for chemical removal of oxide layers from objects of metal
US4704126A (en) * 1985-04-15 1987-11-03 Richards Medical Company Chemical polishing process for titanium and titanium alloy surgical implants
US5376236A (en) * 1993-10-29 1994-12-27 At&T Corp. Process for etching titanium at a controllable rate
US20040188261A1 (en) * 2003-03-27 2004-09-30 Scimed Life Systems, Inc. Methods of forming medical devices
WO2007059730A2 (de) * 2005-11-21 2007-05-31 Mtu Aero Engines Gmbh Verfahren zur vorbehandlung von titanbauteilen zur nachfolgenden beschichtung derselben
US20080038625A1 (en) * 2006-08-10 2008-02-14 Gm Global Technology Operations, Inc. Fast Recycling Process For Ruthenium, Gold and Titanium Coatings From Hydrophilic PEM Fuel Cell Bipolar Plates
WO2008056010A1 (es) * 2006-11-06 2008-05-15 GUTIERREZ RODRIGUEZ, José Ignacio Producto limpiador ácido de múltiples aplicaciones
US20080169270A1 (en) * 2007-01-17 2008-07-17 United Technologies Corporation Method of removing a case layer from a metal alloy
US20100213793A1 (en) * 2007-09-12 2010-08-26 Valeo Schalter Und Sensoren Gmbh Process for the surface treatment of aluminium and a layerwise construction of an aluminium component having an electric contact
EP2584069A1 (de) * 2011-10-21 2013-04-24 Siemens Aktiengesellschaft Vorbehandlung bei einer Fluoridionen-Reinigung und Verfahren
WO2014177777A1 (fr) * 2013-05-03 2014-11-06 Technett Solution de decapage chimique exempte d'agent oxydant applicable sur les métaux du groupe ivb et leurs alliages
ITPR20130068A1 (it) * 2013-09-13 2015-03-14 Borrozzino Carlo Metodo per la preparazione di superfici di dispositivi di titanio-ceramica-zirconia impiantabili nel corpo umano o animale, avente risultato di rugosita' nanometrica, formazione di biossido di titanio superficiale autoindotto, elevata pulizia anti me
US20180237919A1 (en) * 2015-09-15 2018-08-23 Chemetall Gmbh Pre-treating aluminum surfaces with zirconium-and molybdenum-containing compositions
GB2575365A (en) * 2018-07-05 2020-01-08 South West Metal Finishing Ltd Process
US20200032412A1 (en) * 2018-07-25 2020-01-30 The Boeing Company Compositions and Methods for Activating Titanium Substrates
US20200032409A1 (en) * 2018-07-25 2020-01-30 The Boeing Company Compositions and Methods for Electrodepositing Tin-Bismuth Alloys on Metallic Substrates
US20200032411A1 (en) * 2018-07-25 2020-01-30 The Boeing Company Compositions and Methods for Activating Titanium Substrates
US20200235374A1 (en) * 2014-03-31 2020-07-23 Technion Research & Development Foundation Limited Method for passive metal activation and uses thereof

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1290752A (xx) * 1970-06-04 1972-09-27
FR3140890A1 (fr) * 2022-10-14 2024-04-19 Institut De Recherche Technologique Matériaux, Métallurgie, Procédés Bain de polissage chimique pour titane et alliages de titane, et procédé utilisant un tel bain

Cited By (39)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3753815A (en) * 1971-09-22 1973-08-21 Armco Steel Corp Method and bath for treating titanium
US4002489A (en) * 1973-06-21 1977-01-11 Nyby Bruk Ab Method of pickling metallic material
US3994817A (en) * 1975-07-28 1976-11-30 Rockwell International Corporation Etchant for etching silicon
US4322264A (en) * 1975-12-09 1982-03-30 U.S. Philips Corporation Method for selective etching of titaniumdioxide relative to aluminum
US4220706A (en) * 1978-05-10 1980-09-02 Rca Corporation Etchant solution containing HF-HnO3 -H2 SO4 -H2 O2
US4277289A (en) * 1978-07-19 1981-07-07 Aluminum Pechiney Process for removing titaniferous and silico-aluminous incrustations from surfaces
US4525250A (en) * 1980-12-19 1985-06-25 Ludwig Fahrmbacher-Lutz Method for chemical removal of oxide layers from objects of metal
US4704126A (en) * 1985-04-15 1987-11-03 Richards Medical Company Chemical polishing process for titanium and titanium alloy surgical implants
US5376236A (en) * 1993-10-29 1994-12-27 At&T Corp. Process for etching titanium at a controllable rate
US20040188261A1 (en) * 2003-03-27 2004-09-30 Scimed Life Systems, Inc. Methods of forming medical devices
US6960370B2 (en) 2003-03-27 2005-11-01 Scimed Life Systems, Inc. Methods of forming medical devices
US20090218232A1 (en) * 2005-11-21 2009-09-03 Mtu Aero Engines Gmbh Method for the Pre-Treatment of Titanium Components for the Subsequent Coating Thereof
WO2007059730A2 (de) * 2005-11-21 2007-05-31 Mtu Aero Engines Gmbh Verfahren zur vorbehandlung von titanbauteilen zur nachfolgenden beschichtung derselben
WO2007059730A3 (de) * 2005-11-21 2007-10-11 Mtu Aero Engines Gmbh Verfahren zur vorbehandlung von titanbauteilen zur nachfolgenden beschichtung derselben
US8354036B2 (en) 2005-11-21 2013-01-15 Mtu Aero Engines Gmbh Method for the pre-treatment of titanium components for the subsequent coating thereof
DE102007037246B4 (de) 2006-08-10 2018-05-17 GM Global Technology Operations LLC (n. d. Ges. d. Staates Delaware) Verfahren zum recyceln einer beschichteten bipolaren platte aus rostfreiem stahl
US8323415B2 (en) 2006-08-10 2012-12-04 GM Global Technology Operations LLC Fast recycling process for ruthenium, gold and titanium coatings from hydrophilic PEM fuel cell bipolar plates
US20080038625A1 (en) * 2006-08-10 2008-02-14 Gm Global Technology Operations, Inc. Fast Recycling Process For Ruthenium, Gold and Titanium Coatings From Hydrophilic PEM Fuel Cell Bipolar Plates
ES2299381A1 (es) * 2006-11-06 2008-05-16 Javier Diaz Rodriguez Producto limpiador acido de multiples aplicaciones.
WO2008056010A1 (es) * 2006-11-06 2008-05-15 GUTIERREZ RODRIGUEZ, José Ignacio Producto limpiador ácido de múltiples aplicaciones
US20080169270A1 (en) * 2007-01-17 2008-07-17 United Technologies Corporation Method of removing a case layer from a metal alloy
EP1947217A1 (en) * 2007-01-17 2008-07-23 United Technologies Corporation Method of removing an alpha-case titanium layer from a beta-phase titanium alloy
US20100213793A1 (en) * 2007-09-12 2010-08-26 Valeo Schalter Und Sensoren Gmbh Process for the surface treatment of aluminium and a layerwise construction of an aluminium component having an electric contact
US8549746B2 (en) * 2007-09-12 2013-10-08 Valeo Schalter Und Sensoren Gmbh Process for the surface treatment of aluminium
EP2584069A1 (de) * 2011-10-21 2013-04-24 Siemens Aktiengesellschaft Vorbehandlung bei einer Fluoridionen-Reinigung und Verfahren
WO2013056869A1 (de) * 2011-10-21 2013-04-25 Siemens Aktiengesellschaft Vorbehandlung bei einer fluoridionen-reinigung und verfahren
FR3005318A1 (fr) * 2013-05-03 2014-11-07 Technett Solution de decapage chimique exempte d'acide fluorhydrique applicable sur le titane et ses alliages
WO2014177777A1 (fr) * 2013-05-03 2014-11-06 Technett Solution de decapage chimique exempte d'agent oxydant applicable sur les métaux du groupe ivb et leurs alliages
ITPR20130068A1 (it) * 2013-09-13 2015-03-14 Borrozzino Carlo Metodo per la preparazione di superfici di dispositivi di titanio-ceramica-zirconia impiantabili nel corpo umano o animale, avente risultato di rugosita' nanometrica, formazione di biossido di titanio superficiale autoindotto, elevata pulizia anti me
EP2893942A1 (en) * 2013-09-13 2015-07-15 Cristiano Ugo Ciranni Method for the preparation of surfaces of devices made of titanium or titanium alloys, zirconium, zirconia, alumina or zirconia/alumina compounds, stainless steels for medical use and cobalt-base superalloys for medical use implantable in the human or animal body, having as a result nanometer roughness, formation of self-induced surface oxide, high anti-metalosis cleaning and possible preparation of parts with surface antimicrobial treatment.
US9308153B2 (en) 2013-09-13 2016-04-12 Cristiano Ugo CIRANNI Method for the preparation of surfaces of dental or orthopedic implants
US20200235374A1 (en) * 2014-03-31 2020-07-23 Technion Research & Development Foundation Limited Method for passive metal activation and uses thereof
US11688845B2 (en) * 2014-03-31 2023-06-27 Technion Research & Development Foundation Limited Method for passive metal activation and uses thereof
US20180237919A1 (en) * 2015-09-15 2018-08-23 Chemetall Gmbh Pre-treating aluminum surfaces with zirconium-and molybdenum-containing compositions
GB2575365A (en) * 2018-07-05 2020-01-08 South West Metal Finishing Ltd Process
GB2575365B (en) * 2018-07-05 2023-01-18 South West Metal Finishing Ltd Process
US20200032412A1 (en) * 2018-07-25 2020-01-30 The Boeing Company Compositions and Methods for Activating Titanium Substrates
US20200032409A1 (en) * 2018-07-25 2020-01-30 The Boeing Company Compositions and Methods for Electrodepositing Tin-Bismuth Alloys on Metallic Substrates
US20200032411A1 (en) * 2018-07-25 2020-01-30 The Boeing Company Compositions and Methods for Activating Titanium Substrates

Also Published As

Publication number Publication date
CH505916A (fr) 1971-04-15
FR1589844A (xx) 1970-04-06
BE722726A (xx) 1969-04-23

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