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EP2584069A1 - Pre-treatment for fluoride-ion cleaning and method - Google Patents

Pre-treatment for fluoride-ion cleaning and method Download PDF

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Publication number
EP2584069A1
EP2584069A1 EP11186215.7A EP11186215A EP2584069A1 EP 2584069 A1 EP2584069 A1 EP 2584069A1 EP 11186215 A EP11186215 A EP 11186215A EP 2584069 A1 EP2584069 A1 EP 2584069A1
Authority
EP
European Patent Office
Prior art keywords
pretreatment solution
solution according
acid
surfactant
halogen compound
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Withdrawn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
EP11186215.7A
Other languages
German (de)
French (fr)
Inventor
Christopher Degel
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.)
Siemens AG
Siemens Corp
Original Assignee
Siemens AG
Siemens Corp
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 Siemens AG, Siemens Corp filed Critical Siemens AG
Priority to EP11186215.7A priority Critical patent/EP2584069A1/en
Priority to PCT/EP2012/065462 priority patent/WO2013056869A1/en
Publication of EP2584069A1 publication Critical patent/EP2584069A1/en
Withdrawn legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G5/00Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/10Other heavy metals

Definitions

  • the invention relates to a pretreatment of a component which is supplied to a fluoride ion cleaning and a method.
  • a fluoride ion cleaning is often used in which the components in a low-pressure chamber (see WO 2009/049637 A1 ) and be exposed at high temperature with fluoride ions.
  • the oxide is removed and the cracks or depressions can be well wetted and filled by solder or weld metal.
  • the object is achieved by a pretreatment solution according to claim 1 and a method according to claim 10.
  • the component to be cleaned is preferably a gas turbine blade and comprises a nickel or cobalt base alloy having an oxide to be soldered, welded or machined which is removed should.
  • the surface to be cleaned is immersed in a pretreatment solution prior to the high temperature fluoride ion cleaning, or the pretreatment solution is applied to the surface or into the crack.
  • the composition has an acid, especially only one acid.
  • an 8% to 12%, in particular 10% sulfuric acid H 2 SO 4 is used.
  • the pretreatment solution contains a halogen compound, in particular only one.
  • a halogen compound in particular only one.
  • This is preferably ammonium hydrogen difluoride, preferably in a concentration of 10g to 20g per liter.
  • a surfactant in particular a salt, very particularly sodium dodecyl sulfate added to improve the wetting.
  • the residence time of a pretreatment solution is at least 5 minutes at room temperature. After that it can be removed.
  • the pretreatment solution may remain on the component and then into the high temperature chamber (preferably as in FIG WO 2009/049637 A1 described) are carried out according to a known purification scheme at high temperatures, but with a shorter residence time.
  • the components are typically exposed to halide ions at about 1000 ° C by a halogen-containing pretreatment solution and subsequent fluoride ion purification of the prior art.
  • An embodiment consists in the combination of the respective preferred variants.

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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)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)

Abstract

Durch die Vorbehandlung eines Risses mit Oxiden durch eine halogenidhaltige und säurehaltige Lösung wird eine anschließende Hochtemperaturfluoridionen-Reinigung deutlich verbessert und verkürzt.Pre-treatment of a crack with oxides by a halide-containing and acid-containing solution significantly improves and shortens subsequent high-temperature fluoride ion purification.

Description

Die Erfindung betrifft eine Vorbehandlung eines Bauteils, das einer Fluoridionen-Reinigung zugeführt wird und ein Verfahren.The invention relates to a pretreatment of a component which is supplied to a fluoride ion cleaning and a method.

Vor dem Löten oder vor dem Schweißen von Hochtemperaturbauteilen, wie z.B. von Gasturbinenschaufeln, die insbesondere aus Nickel- oder Kobaltbasislegierungen bestehen, müssen die zu reparierenden Oberflächen von Oxiden befreit werden. Dazu wird oft eine Fluoridionen-Reinigung verwendet, bei dem die Bauteile in eine Niederdruckkammer (siehe WO 2009/049637 A1 ) gelangen und bei hoher Temperatur mit Fluoridionen beaufschlagt werden.Prior to brazing or before welding high temperature components, such as gas turbine blades, which are particularly made of nickel or cobalt base alloys, the surfaces to be repaired must be freed of oxides. For this purpose, a fluoride ion cleaning is often used in which the components in a low-pressure chamber (see WO 2009/049637 A1 ) and be exposed at high temperature with fluoride ions.

Das Oxid wird entfernt und die Risse bzw. die Vertiefungen können durch Lot oder Schweißgut gut benetzt und befüllt werden.The oxide is removed and the cracks or depressions can be well wetted and filled by solder or weld metal.

Der Prozess läuft manchmal nicht schnell genug ab.Sometimes the process does not run fast enough.

Es ist daher Aufgabe der Erfindung, o.g. Problem zu lösen.It is therefore an object of the invention, o.g. Solve a problem.

Die Aufgabe wird gelöst durch eine Vorbehandlungslösung gemäß Anspruch 1 und ein Verfahren gemäß Anspruch 10.The object is achieved by a pretreatment solution according to claim 1 and a method according to claim 10.

In den Unteransprüchen sind weitere vorteilhafte Maßnahmen aufgelistet, die beliebig miteinander kombiniert werden können, um weitere Vorteile zu erzielen.In the dependent claims further advantageous measures are listed, which can be combined with each other in order to achieve further advantages.

Die Beschreibung stellt nur ein Ausführungsbeispiel der Erfindung dar.The description represents only one embodiment of the invention.

Das zu reinigende Bauteil ist vorzugsweise eine Gasturbinenschaufel und weist eine Nickel- oder Kobaltbasislegierung auf, das in einer zu lötenden, zu schweißenden oder zu bearbeitenden Stelle ein Oxid aufweist, das entfernt werden soll. Die zu reinigende Oberfläche wird vor der Hochtemperatur-Fluoridionen-Reinigung in eine Vorbehandlungslösung eingetaucht oder die Vorbehandlungslösung wird auf die Oberfläche oder in den Riss eingebracht.The component to be cleaned is preferably a gas turbine blade and comprises a nickel or cobalt base alloy having an oxide to be soldered, welded or machined which is removed should. The surface to be cleaned is immersed in a pretreatment solution prior to the high temperature fluoride ion cleaning, or the pretreatment solution is applied to the surface or into the crack.

Die Zusammensetzung weist eine Säure auf, insbesondere nur eine Säure.The composition has an acid, especially only one acid.

Vorzugsweise wird eine 8%ige bis 12%ige, insbesondere 10%ige Schwefelsäure H2SO4 verwendet.Preferably, an 8% to 12%, in particular 10% sulfuric acid H 2 SO 4 is used.

Außerdem enthält die Vorbehandlungslösung eine Halogenverbindung, insbesondere nur eine. Dies ist vorzugsweise Ammoniumhydrogendifluorid, vorzugsweise in einer Konzentration von 10g bis 20g pro Liter.In addition, the pretreatment solution contains a halogen compound, in particular only one. This is preferably ammonium hydrogen difluoride, preferably in a concentration of 10g to 20g per liter.

Optional wird noch 0,1g bis 0,5g pro Liter ein Tensid, insbesondere ein Salz, ganz insbesondere Natriumdodecylsulfat hinzugegeben zur Verbesserung der Benetzung.Optionally, 0.1 g to 0.5 g per liter of a surfactant, in particular a salt, very particularly sodium dodecyl sulfate added to improve the wetting.

Die Verweildauer einer Vorbehandlungslösung beträgt bei Raumtemperatur mindestens 5 Minuten. Danach kann sie entfernt werden.The residence time of a pretreatment solution is at least 5 minutes at room temperature. After that it can be removed.

Ebenso kann die Vorbehandlungslösung auf dem Bauteil verbleiben und dann in die Hochtemperaturkammer (vorzugsweise wie in WO 2009/049637 A1 beschrieben) nach einem bekannten Reinigungsschema bei hohen Temperaturen, aber bei verkürzter Verweildauer durchgeführt werden.Likewise, the pretreatment solution may remain on the component and then into the high temperature chamber (preferably as in FIG WO 2009/049637 A1 described) are carried out according to a known purification scheme at high temperatures, but with a shorter residence time.

Dies bedeutet, dass die Bauteile durch eine halogenhaltige Vorbehandlungslösung und durch die anschließende Fluoridionen-Reinigung nach dem Stand der Technik typischerweise bei ungefähr 1000°C Halogenidionen ausgesetzt sind.That is, the components are typically exposed to halide ions at about 1000 ° C by a halogen-containing pretreatment solution and subsequent fluoride ion purification of the prior art.

Ein Ausführungsbeispiel besteht in der Kombination der jeweils bevorzugten Varianten.An embodiment consists in the combination of the respective preferred variants.

Claims (12)

Vorbehandlungslösung vor einer Hochtemperatur-luoridionen-Reinigung,
die zumindest aufweist: eine Säure, eine Halogenverbindung, optional ein Tensid, insbesondere in Form eines oder mehrerer Salze.
Pretreatment solution prior to high temperature luoride ion purification,
which at least has: an acid, a halogen compound, optionally a surfactant, especially in the form of one or more salts.
Vorbehandlungslösung nach Anspruch 1,
die als Säure eine Schwefelsäure aufweist,
insbesondere 8%ig bis 12%ig,
ganz insbesondere 10%ig.
Pretreatment solution according to claim 1,
which has a sulfuric acid as the acid,
in particular 8% to 12%,
especially 10%.
Vorbehandlungslösung nach einem oder beiden der Ansprüche 1 oder 2,
bei dem die Halogenverbindung ein Fluorid,
insbesondere Ammoniumhydrogendifluorid darstellt,
ganz insbesondere mit 10g bis 20g pro Liter.
Pretreatment solution according to one or both of claims 1 or 2,
in which the halogen compound is a fluoride,
in particular ammonium hydrogen difluoride,
especially with 10g to 20g per liter.
Vorbehandlungslösung nach einem oder mehreren Ansprüchen 1 bis 3,
die ein Tensid enthält,
insbesondere Natriumdodecylsulfat enthält.
Pretreatment solution according to one or more of claims 1 to 3,
containing a surfactant,
especially sodium dodecyl sulfate.
Vorbehandlungslösung nach einem oder beiden der Ansprüche 4,
mit einer Konzentration des Tensids von 0,1g bis 0,5g pro Liter.
Pretreatment solution according to one or both of claims 4,
with a concentration of the surfactant of 0.1g to 0.5g per liter.
Vorbehandlungslösung nach einem oder mehreren Ansprüchen 1 bis 5,
die aus Säure, Halogenverbindung, Salz besteht.
Pretreatment solution according to one or more of claims 1 to 5,
which consists of acid, halogen compound, salt.
Vorbehandlungslösung nach einem oder mehreren Ansprüchen 1 bis 6,
die nur eine Säure aufweist.
Pretreatment solution according to one or more of claims 1 to 6,
which has only one acid.
Vorbehandlungslösung nach einem oder mehreren Ansprüchen 1 bis 7,
die nur eine Halogenverbindung aufweist.
Pretreatment solution according to one or more of claims 1 to 7,
which has only one halogen compound.
Vorbehandlungslösung nach einem oder mehreren Ansprüchen 1 bis 8,
die nur ein Tensid aufweist.
Pretreatment solution according to one or more of claims 1 to 8,
which has only one surfactant.
Verfahren zur Fluoridionen-Reinigung,
bei dem das zu reinigende Bauteil mit einer Vorbehandlungslösung nach einem oder mehreren der Ansprüche 1 bis 9 vorbehandelt wird, und
dann in eine Hochtemperaturkammer eingeführt wird,
bei der das Bauteil bei hohen Temperaturen gasförmigen Halogenidionen ausgesetzt ist.
Process for fluoride ion purification,
in which the component to be cleaned is pretreated with a pretreatment solution according to one or more of claims 1 to 9, and
then introduced into a high temperature chamber,
in which the component is exposed to gaseous halide ions at high temperatures.
Verfahren nach Anspruch 10,
bei dem die Verweildauer der Vorbehandlungslösung um oder in dem Riss mindestens 5 Minuten beträgt.
Method according to claim 10,
in which the residence time of the pretreatment solution around or in the crack is at least 5 minutes.
Verfahren nach einem oder beiden der Ansprüche 10 oder 11,
bei der die Behandlung mit der Vorbehandlungslösung bei Raumtemperatur stattfindet.
Method according to one or both of claims 10 or 11,
in which the treatment with the pretreatment solution takes place at room temperature.
EP11186215.7A 2011-10-21 2011-10-21 Pre-treatment for fluoride-ion cleaning and method Withdrawn EP2584069A1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP11186215.7A EP2584069A1 (en) 2011-10-21 2011-10-21 Pre-treatment for fluoride-ion cleaning and method
PCT/EP2012/065462 WO2013056869A1 (en) 2011-10-21 2012-08-07 Pretreatment in a fluoride ion cleaning operation and process

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP11186215.7A EP2584069A1 (en) 2011-10-21 2011-10-21 Pre-treatment for fluoride-ion cleaning and method

Publications (1)

Publication Number Publication Date
EP2584069A1 true EP2584069A1 (en) 2013-04-24

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Country Status (2)

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EP (1) EP2584069A1 (en)
WO (1) WO2013056869A1 (en)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3562013A (en) * 1967-10-23 1971-02-09 Diversey Corp Process of deoxidizing titanium and its alloys
US20010009246A1 (en) * 2000-01-20 2001-07-26 Zimmerman Robert George Method of removing ceramic coatings
US20040074873A1 (en) * 2002-10-21 2004-04-22 General Electric Company Process for removing aluminosilicate material from a substrate, and related compositions
EP1674561A1 (en) * 2004-12-27 2006-06-28 General Electric Company Method for removing engine deposits from turbine components and composition for use in same
WO2007048698A1 (en) * 2005-10-26 2007-05-03 Siemens Aktiengesellschaft Technology for cleaning thermal fatigue cracks in nickel-based superalloys with a high chromium content
WO2009049637A1 (en) 2007-10-10 2009-04-23 Siemens Aktiengesellschaft Fic installation and method for operating a fic installation in the pressure range above atmospheric pressure

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3562013A (en) * 1967-10-23 1971-02-09 Diversey Corp Process of deoxidizing titanium and its alloys
US20010009246A1 (en) * 2000-01-20 2001-07-26 Zimmerman Robert George Method of removing ceramic coatings
US20040074873A1 (en) * 2002-10-21 2004-04-22 General Electric Company Process for removing aluminosilicate material from a substrate, and related compositions
EP1674561A1 (en) * 2004-12-27 2006-06-28 General Electric Company Method for removing engine deposits from turbine components and composition for use in same
WO2007048698A1 (en) * 2005-10-26 2007-05-03 Siemens Aktiengesellschaft Technology for cleaning thermal fatigue cracks in nickel-based superalloys with a high chromium content
WO2009049637A1 (en) 2007-10-10 2009-04-23 Siemens Aktiengesellschaft Fic installation and method for operating a fic installation in the pressure range above atmospheric pressure

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Publication number Publication date
WO2013056869A1 (en) 2013-04-25

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