EP1111089A1 - Procédé pour sceller une couche poreuse à la surface d'un objet, en particulier pour sceller une couche obtenue par pulvérisation thermique - Google Patents

Procédé pour sceller une couche poreuse à la surface d'un objet, en particulier pour sceller une couche obtenue par pulvérisation thermique Download PDF

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Publication number
EP1111089A1
EP1111089A1 EP00811072A EP00811072A EP1111089A1 EP 1111089 A1 EP1111089 A1 EP 1111089A1 EP 00811072 A EP00811072 A EP 00811072A EP 00811072 A EP00811072 A EP 00811072A EP 1111089 A1 EP1111089 A1 EP 1111089A1
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EP
European Patent Office
Prior art keywords
coating
sealing
layer
sealant
metal
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Withdrawn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
EP00811072A
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German (de)
English (en)
Inventor
Raoul Patrick Villiger
Emad Dr. Batawi
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.)
Sulzer Markets and Technology AG
Original Assignee
Sulzer Markets and Technology AG
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 Sulzer Markets and Technology AG filed Critical Sulzer Markets and Technology AG
Priority to EP00811072A priority Critical patent/EP1111089A1/fr
Publication of EP1111089A1 publication Critical patent/EP1111089A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/18—After-treatment
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
    • C23C18/1208—Oxides, e.g. ceramics
    • C23C18/1216—Metal oxides
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1225—Deposition of multilayers of inorganic material
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1229—Composition of the substrate
    • C23C18/1245—Inorganic substrates other than metallic

Definitions

  • the invention relates to a method for sealing a porous layer the surface of a body, especially for sealing one thermal spray coating. It also refers to a machine component, one surface at least partially sealed with the method has, as well as on applications of the method.
  • the one to be sealed Surface can also be the surface of, for example, one made of metal powders sintered body.
  • Functional layers are produced using thermal spray processes which, for example, have improved corrosion resistance Machine component should be achieved.
  • More functions of such Coatings are: wear, abrasion, erosion resistance, increased operating temperature due to thermal protective layers, protection against High temperature oxidation of the primer.
  • Ceramic and / or metallic wettable powder When using ceramic and / or metallic wettable powder usually form coatings, which have capillary spaces formed by pores and open crack structures. These capillary spaces can be communicating connecting spaces between a substrate or a primer of the coating and the Form layer surface so that the coating for a corrosive medium is permeable.
  • the object of the invention is to provide a method with which for example, a ceramic spray coating can be treated in such a way that communicating capillary spaces of the coating filled for sealing, i.e. be sealed.
  • a seal should also resistant to elevated temperatures of over 400 ° C.
  • a seal is obtained porous coating, in which pores and cracks below the Layer surface are filled with metal oxides.
  • Such a seal or Sealing is also with a surface layer of a porous body possible. This seal is - in contrast to seals with for example organic polymers - even at elevated temperatures resistant.
  • the dependent claims 2 to 5 relate to advantageous embodiments of the inventive method.
  • the subject of claims 6 to 8 is each a machine component with a coating that with the method according to the invention has been sealed.
  • Claim 9 relates on applications of the process.
  • the layer 10 can also be a surface layer of a porous body.
  • a surface 11 of the surface layer or coating 10 that has a certain roughness is approximately a surface that is largely parallel to a substrate surface, not shown.
  • Communicating capillary spaces 12 in the coating 10 are connected to the layer surface 11.
  • the capillary spaces 12 are formed by an open crack structure and pores 13.
  • a drop 20 of a liquid 2 (FIG. 2), which is used as a sealant, is applied to the surface 11.
  • the further environment 29 of the drop 20 is gaseous, and the gas phase can be formed by vaporous solvent.
  • a point 21 lies on the surface 11 and on the edge of the drop 20.
  • ⁇ SV ⁇ SL + ⁇ LV cos ⁇ , where ⁇ is the wetting angle. Due to capillary forces, liquid 2 penetrates into the capillary spaces 12. During a time period t, penetration to a depth x (t) takes place. According to model calculations, this penetration depth is proportional (factor f a ) to the square root of t. The square of the proportionality factor f a is proportional (factor fb) to the surface tension ⁇ LV and cos ⁇ and inversely proportional to the viscosity ⁇ .
  • Layer properties such as roughness and chemical activity of the Surface 11, shape and size of the capillary spaces 12 have an influence on the penetration.
  • chemical activity related to pH it is advantageous if the sealing agent has a pH either less than 7 or greater than 7 is provided, depending on whether the layer surface 11 has a basic or acidic character.
  • the crack geometry is also crucial. If the diameter is one Cracks from the surface 11 to the substrate continuously larger, see above the capillary force steadily decreases. The penetration can be after a limited depth of penetration come to a standstill.
  • the roughness must be between a true and an effective wetting angle be distinguished.
  • the parameters ⁇ LV , ⁇ and ⁇ must be matched to the properties of the coating 10 and its capillary spaces 12.
  • the coating 10 can be a thermal spray layer, wherein one of the following ceramic or metallic materials or mixtures of these materials can be used as the coating material: oxides of Cr, Al, Ti, Zr, Ca, Si or Y; also metals, in particular iron-based alloys, which can be mixed with hard metals such as WC or Cr carbides to form a composite.
  • the coating material can be made, for example, from a mixture of aluminum and titanium oxide (eg Al 2 O 3 /13% TiO 2 , Al 2 O 3 /40% TiO 2 , data in% by weight) or zirconium and yttrium oxide (e.g. ZrO 2 /8% Y 2 O 3 ).
  • the method according to the invention comprises the following steps (see FIG. 2):
  • the sealing agent 2 on the layer surface 11 a component 1 applied.
  • this application 3 there is also a time period t included, during which the solution 2 partially in the capillary 11th penetrates.
  • the application 3 of the sealing agent 2 can by means of various processes such as spraying, brushing or dipping become.
  • step 4 heat is introduced. It evaporates the solvent content of liquid 2 and the previously dissolved metals oxidize using oxygen from the environment 29 or Oxidizing agents that are dissolved in the liquid 2. The oxidation takes place at a temperature that is greater than one of the oxidizable metal dependent transformation temperature.
  • the heat input 4 can be carried out in different ways: in a thermal oven, in a microwave oven, with a Radiant heater, especially a carbon radiator (wavelength range 2-3.5 ⁇ m, i.e. fast medium wave), and / or with a flame, in particular a flame from a plasma torch.
  • a Radiant heater especially a carbon radiator (wavelength range 2-3.5 ⁇ m, i.e. fast medium wave)
  • a flame in particular a flame from a plasma torch.
  • the heat input 4 for oxidation can also only take place when the body is used for the first time, whose surface 11 has been treated with process step a), the evaporation of the solvent fraction before the first Operations can be carried out.
  • the further process step 5 is not necessary. It concerns cleaning, i. H. an at least partial removal of a covering from the original Surface 11, the solid residues of the sealing agent 2nd is formed. Such a covering can increase the roughness of the surface reduce and represent an additional protective layer. In this case one advantageously refrains from cleaning or at least complete cleaning Cleaning. Superficial cleaning can be done with compressed air and / or under Use brushes.
  • the sealant 2 can be an aqueous solution which contains a salt of the oxidizable metal in solution.
  • the metal salt is preferably a nitrate of the metals Co, Mn, Mg, Ca, Sr, Y, Zr, Al, Ti and / or a lanthanide, in particular one of the lanthanides Ce, Eu or Gd.
  • the metal converted into an oxide is in Water insoluble.
  • These metal nitrates are generally available as crystalline hydrates, for example Ce (NO 3 ) 3 • 6H 2 O, which are readily soluble in water.
  • Heavy metal nitrates decompose at elevated temperatures into the corresponding oxides (e.g. Ce203) with the simultaneous formation of NO2.
  • the transition temperature at which oxide formation occurs is at values greater than around 300 ° C. As the temperature rises, the treatment time is reduced (for example 15 minutes at 350 ° C, 10 minutes at 400 ° C). When using a plasma torch, the conversion takes place in a few seconds thanks to the high energy input.
  • the sealant 2 is advantageously a saturated, solids-free solution, whose viscosity at 20 ° C is less than 110 mPa s, preferably less than 35 mPa s. Solid particles suspended in the solution can be removed using Filtration can be removed. As a rule, the sealing means 2 only one moderately good resistance, the solution is produced with advantage shortly before application.
  • an organic liquid can also be used as a solvent, for example ethyl alcohol or propanol.
  • the metal salt can also be used in the form of an acetate (for example Ce (C 2 H 3 O 2 ) 3 • 3/2 H 2 O).
  • At least one surfactant is advantageously added to the sealing agent 2, so that the wetting angle ⁇ and the surface tension ⁇ LV of this liquid are suitably reduced with respect to the coating material. This should result in the greatest possible depth of penetration or the largest possible volume of the sealant 2 which has penetrated into the capillary spaces 12. Good results were achieved with the nonionic surfactants Triton X-100 (polyethylene glycol monoether C 8 H 17 -C 6 H 4 - (OCH 2 CH 2 ) n OH) and Tergitol TMN 3. Additional use of ionic surfactants can be advantageous.
  • Sintering aids such as H 3 BO 3 were also used as further additives for the sealing agent 2, with the aim of reducing the transition temperature.
  • tests have shown that the transition temperature and time cannot be significantly influenced with the selected sintering aids.
  • sealed coatings There are various uses of sealed coatings possible, namely applications to reduce the Surface roughness, to increase the hardness of the coating and / or to improve resistance to corrosion, Abrasion and / or erosion.
  • the sealer - the solid residues of the sealant 2 after the application - can adhere in part to the surface 11, the Roughness of the coating 10 can be reduced.
  • a smoothing effect of 10 - 20% is possible. This effect can be particularly advantageous in gas turbines his. As suspected, rough surfaces cause thermal Spray layers on blades of a gas turbine that are not sealed, one Vortex formation on the surfaces and thus a reduction in Efficiency of the turbine. This would result in a seal improved efficiency.
  • the porosity of a coating is determined by closing open pores partially eliminated. However, closed and large pores can be do not seal. Thus, a coating that is closed and contains relatively large pores as a thermal protective layer with reduced Use thermal conductivity but increased corrosion resistance.
  • Sealant was used with a saturated cerium nitrate solution Water as a solvent and Triton X-100 as a surfactant (maximum 3% by weight in In relation to the water content).
  • the layer hardness is significantly positive through a seal influenced.
  • An increase in hardness depends on the number Repetitions of the application. After one treatment, Try an increase of 15 to 20% that is observed after a fourth repetition increased to 50%.
  • the experiments were carried out with the above thermal spray layers made of aluminum and titanium oxide or Zirconium and yttrium oxide performed.
  • the ZrO 2 /8% Y 2 O 3 layers were subjected to thermal cycling in a corrosive medium, the temperature being changed periodically between 25 and 900 ° C. Conditions such as those found in a diesel engine were set. Unsealed samples showed a strongly corrosive and oxidative attack at the interface between the functional layer and the adhesive layer after 1000 cycles. Large-scale delaminations were observed. Corrosive attacks were also found on sealed layers. But delamination occurred to a very limited extent, although cracks had developed parallel and perpendicular to surface 11. The increased cohesion probably prevented the coating from flaking off here.
  • a machine component 1 with an at least local coating 10, which with the method according to the invention has been sealed one of the following examples are: a blade of a gas turbine, a roller for the Printing, paper or film industry, a transport roll, a profiled one Deflection roller for threads in a spinning mill, heat exchanger tube for one Boiler system and a sensor of measurement technology with an electrical insulating coating.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Thermal Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Plasma & Fusion (AREA)
  • Ceramic Engineering (AREA)
  • Coating By Spraying Or Casting (AREA)
EP00811072A 1999-12-13 2000-11-14 Procédé pour sceller une couche poreuse à la surface d'un objet, en particulier pour sceller une couche obtenue par pulvérisation thermique Withdrawn EP1111089A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP00811072A EP1111089A1 (fr) 1999-12-13 2000-11-14 Procédé pour sceller une couche poreuse à la surface d'un objet, en particulier pour sceller une couche obtenue par pulvérisation thermique

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP99811152 1999-12-13
EP99811152 1999-12-13
EP00811072A EP1111089A1 (fr) 1999-12-13 2000-11-14 Procédé pour sceller une couche poreuse à la surface d'un objet, en particulier pour sceller une couche obtenue par pulvérisation thermique

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EP1111089A1 true EP1111089A1 (fr) 2001-06-27

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EP00811072A Withdrawn EP1111089A1 (fr) 1999-12-13 2000-11-14 Procédé pour sceller une couche poreuse à la surface d'un objet, en particulier pour sceller une couche obtenue par pulvérisation thermique

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7141110B2 (en) 2003-11-21 2006-11-28 General Electric Company Erosion resistant coatings and methods thereof
DE102006045617A1 (de) * 2006-09-22 2008-03-27 Innovent E.V. Technologieentwicklung Verfahren zur Herstellung einer anorganisch-anorganischen bzw. anorganisch-organischen Gradientenkompositschicht
WO2008044128A3 (fr) * 2006-10-12 2008-06-12 Inglass Spa Technique innovante visant à améliorer les caractéristiques diélectriques et anticorrosion de revêtements obtenus au moyen de technologies de projection thermique, aps, hvof et analogues, en particulier de couches isolantes telles que al2o3
EP2025772A1 (fr) * 2007-08-16 2009-02-18 Sulzer Metco AG Procédé destiné à la fabrication d'une couche fonctionnelle
EP2524973A1 (fr) * 2011-05-18 2012-11-21 Sulzer Metco AG Procédé d'injection à arc lumineux pour la fabrication d'une couche poreuse
DE202012012592U1 (de) 2012-05-04 2013-07-19 Voith Patent Gmbh Walze

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3928845A1 (de) * 1989-08-31 1991-03-07 Boehler Ag Prothese
US5830537A (en) * 1995-10-23 1998-11-03 Valmet Corporation Method for manufacturing a roll for use in the production of paper

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3928845A1 (de) * 1989-08-31 1991-03-07 Boehler Ag Prothese
US5830537A (en) * 1995-10-23 1998-11-03 Valmet Corporation Method for manufacturing a roll for use in the production of paper

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7141110B2 (en) 2003-11-21 2006-11-28 General Electric Company Erosion resistant coatings and methods thereof
US7431566B2 (en) 2003-11-21 2008-10-07 General Electric Company Erosion resistant coatings and methods thereof
DE102006045617A1 (de) * 2006-09-22 2008-03-27 Innovent E.V. Technologieentwicklung Verfahren zur Herstellung einer anorganisch-anorganischen bzw. anorganisch-organischen Gradientenkompositschicht
DE102006045617B4 (de) * 2006-09-22 2010-06-10 Innovent E.V. Technologieentwicklung Verfahren zur Herstellung einer anorganisch-anorganischen Gradientenverbundschicht
WO2008044128A3 (fr) * 2006-10-12 2008-06-12 Inglass Spa Technique innovante visant à améliorer les caractéristiques diélectriques et anticorrosion de revêtements obtenus au moyen de technologies de projection thermique, aps, hvof et analogues, en particulier de couches isolantes telles que al2o3
EP2025772A1 (fr) * 2007-08-16 2009-02-18 Sulzer Metco AG Procédé destiné à la fabrication d'une couche fonctionnelle
EP2524973A1 (fr) * 2011-05-18 2012-11-21 Sulzer Metco AG Procédé d'injection à arc lumineux pour la fabrication d'une couche poreuse
DE202012012592U1 (de) 2012-05-04 2013-07-19 Voith Patent Gmbh Walze
DE102012207398A1 (de) 2012-05-04 2013-09-19 Voith Patent Gmbh Verfahren zum Herstellen einer Walze und Walze

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