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WO2012120194A1 - Processus et appareil de revêtement, ainsi que son utilisation - Google Patents

Processus et appareil de revêtement, ainsi que son utilisation Download PDF

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Publication number
WO2012120194A1
WO2012120194A1 PCT/FI2012/050219 FI2012050219W WO2012120194A1 WO 2012120194 A1 WO2012120194 A1 WO 2012120194A1 FI 2012050219 W FI2012050219 W FI 2012050219W WO 2012120194 A1 WO2012120194 A1 WO 2012120194A1
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WO
WIPO (PCT)
Prior art keywords
precursor
droplets
coating
precursor flow
substrate
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.)
Ceased
Application number
PCT/FI2012/050219
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English (en)
Inventor
Markku Rajala
Erkki SEPPÄLÄINEN
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.)
Beneq Oy
Original Assignee
Beneq Oy
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 Beneq Oy filed Critical Beneq Oy
Publication of WO2012120194A1 publication Critical patent/WO2012120194A1/fr
Anticipated expiration legal-status Critical
Ceased 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
    • C23C16/4486—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by producing an aerosol and subsequent evaporation of the droplets or particles
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40—Oxides
    • C23C16/407—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45514—Mixing in close vicinity to the substrate
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45595—Atmospheric CVD gas inlets with no enclosed reaction chamber
    • 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
    • C23C18/1229—Composition of the substrate
    • C23C18/1241—Metallic substrates
    • 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
    • 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
    • C23C18/125—Process of deposition of the inorganic material
    • C23C18/1258—Spray pyrolysis
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B7/00—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
    • B05B7/02—Spray pistols; Apparatus for discharge
    • B05B7/06—Spray pistols; Apparatus for discharge with at least one outlet orifice surrounding another approximately in the same plane
    • B05B7/062—Spray pistols; Apparatus for discharge with at least one outlet orifice surrounding another approximately in the same plane with only one liquid outlet and at least one gas outlet
    • B05B7/066—Spray pistols; Apparatus for discharge with at least one outlet orifice surrounding another approximately in the same plane with only one liquid outlet and at least one gas outlet with an inner liquid outlet surrounded by at least one annular gas outlet
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B7/00—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
    • B05B7/02—Spray pistols; Apparatus for discharge
    • B05B7/08—Spray pistols; Apparatus for discharge with separate outlet orifices, e.g. to form parallel jets, i.e. the axis of the jets being parallel, to form intersecting jets, i.e. the axis of the jets converging but not necessarily intersecting at a point
    • B05B7/0807—Spray pistols; Apparatus for discharge with separate outlet orifices, e.g. to form parallel jets, i.e. the axis of the jets being parallel, to form intersecting jets, i.e. the axis of the jets converging but not necessarily intersecting at a point to form intersecting jets
    • B05B7/0815—Spray pistols; Apparatus for discharge with separate outlet orifices, e.g. to form parallel jets, i.e. the axis of the jets being parallel, to form intersecting jets, i.e. the axis of the jets converging but not necessarily intersecting at a point to form intersecting jets with at least one gas jet intersecting a jet constituted by a liquid or a mixture containing a liquid for controlling the shape of the latter
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B7/00—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
    • B05B7/02—Spray pistols; Apparatus for discharge
    • B05B7/08—Spray pistols; Apparatus for discharge with separate outlet orifices, e.g. to form parallel jets, i.e. the axis of the jets being parallel, to form intersecting jets, i.e. the axis of the jets converging but not necessarily intersecting at a point
    • B05B7/0807—Spray pistols; Apparatus for discharge with separate outlet orifices, e.g. to form parallel jets, i.e. the axis of the jets being parallel, to form intersecting jets, i.e. the axis of the jets converging but not necessarily intersecting at a point to form intersecting jets
    • B05B7/0846—Spray pistols; Apparatus for discharge with separate outlet orifices, e.g. to form parallel jets, i.e. the axis of the jets being parallel, to form intersecting jets, i.e. the axis of the jets converging but not necessarily intersecting at a point to form intersecting jets with jets being only jets constituted by a liquid or a mixture containing a liquid

Definitions

  • the invention relates to an aerosol-assisted coating deposition process, especially to a pyrolytic aerosol assisted coating processes where the precursors are allowed to react on the substrate surface or at the vicinity of the substrate surface.
  • the aerosol flow in the first conduit is kept free from at least one reactant required for the coating formation.
  • Said reactant and its flow is fed to the deposition chamber as a second precursor flow, for example from a second conduit.
  • spray coating is a known method for applying a coating.
  • Typical examples of spray-coating are, for example, spray painting and pigment coating of paper.
  • Patent publication US 4,656,963, 14 April 1987, Takashi Yonehara et al. discloses a method for forming an extremely thin film on the surface of an object.
  • aerosol is produced from the precursor material and introduced onto the surface of the substrate to be coated, and after evaporation of the solvent, a thin film is formed on the surface.
  • the publication discloses the production of aerosol particles by ultrasonics, ranging in size from 1.5 to 10 micrometres.
  • the publication provides no description of how the aerosol particles are introduced onto the surface of the substrate.
  • Patent publication US 4,728,353, Glaverbel, 1 March 1988 discloses an apparatus for forming a pyrolytic metal compound coating on a hot glass substrate.
  • the gas atmosphere in the immediate vicinity of the face of the glass substrate is controlled by means of supplying preheated gas thereto that forms a protective atmosphere in the vicinity of the face of the glass substrate.
  • the protective atmosphere makes it possible to prevent the entry of ambient air into the coating area.
  • the publication discloses that the preheated gas is preheated air, meaning that the coating reactions take place in an oxygen-rich atmosphere.
  • the feeding of coating precursor material by means of spraying is disclosed in the
  • Patent publication US 5,540,959, Xingwu Wang, 30 June 1996 discloses a method for preparing a coated substrate using mist particles.
  • small droplets are produced that are heated with radio frequency energy to vaporise the droplets, after which the vapour is deposited onto a substrate.
  • the prior art does not disclose the advantages of having the fluid dispersed into small droplets and keeping the droplets away from a reactive precursor before the droplets are in close contact with the substrate surface.
  • the invention solves the problems of the prior art by an aerosol-assisted coating deposition process where the reaction of the precursor at too early stage is avoided.
  • the aerosol-assisted coating deposition process is preferably a pyrolytic coating deposition process, such as an aerosol-assisted chemical vapor deposition (AACVD) process or a spray pyrolysis processes, but other deposition processes where aerosols are applied are within the scope of this invention.
  • An aerosol is a mixture of at least one gas component and particles, in this case especially liquid particles, or droplets.
  • the premature reaction of the coating precursor is avoided by feeding at least one precursor, i.e.
  • first precursor flow in aerosol form and keeping this aerosol flow essentially free from reactant-containing compounds, e.g. free from oxygen or sulfur, which may be either in gaseous or liquid form.
  • reactant-containing compounds e.g. free from oxygen or sulfur, which may be either in gaseous or liquid form.
  • first precursor flow and “first precursor flow” are used interchangeably in this application. It is also to be noted that even though “first precursor flow” is a singular word, it can contain one or many different precursor chemicals. At the coating formation zone of the process said at least one precursor is allowed to react with the reactant-containing compound, i.e. second precursor flow, and a coating is formed.
  • second precursor flow and “reactant flow” are used interchangeably. It is also to be noted that even though “second precursor flow” is a singular word, it can contain one or many different precursor or reactant chemicals.
  • the droplets are evaporated at or near a substrate which may be e.g. glass, ceramic or metal substrate.
  • Typical substrates include thin silicon substrate and flat glass substrate.
  • the substrate is a flat glass substrate, typically having a thickness of 1 to 6 mm.
  • the substrate may form an essentially continuous ribbon or the substrate may consist of separate pieces or wafers.
  • the droplets are preferably evaporated before hitting the surface.
  • a precursor such as cadmium sulfide (CdS) coatings
  • the present invention is valid in both coating processes.
  • the coating process may require several precursors which are not miscible with each other.
  • An example of such precursor system is the production of fluorine doped tin oxide (FTO) coating from an organic compound of tin, such as monobutyltin trichloride (MBTC) and a tin-doping fluorine source, such as hydrogen fluorine (HF) or an organic source, such as trifluoroacetic acid (TFA, C2HF3O2).
  • MBTC and TFA cannot be mixed together without an additional solvent, which usually comprises oxygen, such as methyl alcohol (CH 3 OH).
  • the process described in the present invention allows atomizing MBTC and TFA from different atomizing nozzles, evaporating both precursors and then allowing them to react with an oxygen- containing precursor.
  • the small amount of oxygen in the TFA does not affect the coating process adversely.
  • An analogue process applies for other tin doping materials, such as antimony (Sb).
  • Droplet charging may be realized in various ways, such as by diffusion charging or by field charging, both methods familiar for a person skilled in the art.
  • the droplets are charged essentially in similar way independent on their composition. When the atomized droplets have a diameter of less than 10 micrometers they may be charged to carry an absolute charge equivalent to some tens of elementary charges and their mobility in an electric field is reasonably high so that the charged droplets can be effectively guided.
  • the reactant-containing compound may be fed into the coating formation zone either as gases or as an aerosol.
  • the reactant-containing compound is preferably water (H 2 O), as water radically increases the coating growth rate of FTO coatings.
  • H 2 O water
  • For optimal growth of a FTO coating it is found to be helpful to supply part of the reactant-containing compound as gaseous oxygen.
  • Fig. 1 shows the principle drawing of the invented process and apparatus
  • Fig. 2 shows an embodiment of the invented apparatus, where the atomized aerosol is guided by additional gas flows;
  • Fig. 3 shows an embodiment for the atomizing nozzle
  • Fig. 4 shows an embodiment with two atomizing nozzles for different liquid precursors.
  • Figure 1 shows a principle drawing of the process and apparatus 3 for depositing coating 2 on substrate 1.
  • Apparatus 3 includes first conduit 6 for a liquid precursor which is atomized to droplets 8 by an atomizer 7.
  • the mean diameter of droplet 8 is preferably low enough so that the gravitational forces affecting the droplet settling are low.
  • the droplet 8 diameter is preferably less than 10 micrometers and more preferably less than 3 micrometers.
  • the droplets 8 and the gas used for atomizing the droplets essentially do not contain a reactant which is required to turn the precursor in the droplet to the material of coating 2.
  • the gas flow does not comprise oxygen in the form of e.g. gaseous oxygen (0 2 ) or water vapor (H 2 0).
  • gaseous oxygen (0 2 ) or water vapor (H 2 0).
  • H 2 0 water vapor
  • the word 'essentially' is used in here to clarify that small amounts of oxygen can be included e.g. in doping materials as long as their amount is so low that they do not adversely create unwanted gas-phase reactions.
  • the droplets 8 may include small amounts of trifluoroacetic acid, C 2 HF 3 0 2 .
  • First conduit 6 leads into deposition chamber 5 where the growth of coating 2 takes place.
  • the coating 2 growth requires a second precursor flow, also defined as a reactant flow from the second conduit 9.
  • Such flow can be for example the flow of an oxygen-containing precursor when forming the tin oxide coating from MBTC.
  • the second conduit 9 includes at least one precursor supply channel 10, but may include other supplies 11 as well.
  • channel 10 is used to supply water vapor and channel 11 is used to supply gaseous oxygen or air and the vapor and gas flows are mixed in the second conduit 9 before feeding into the deposition chamber 5.
  • the invented process and apparatus are used to form a coating 2 by chemical vapor deposition.
  • CVD thermal CVD coating growth of e.g. Sn0 2 coatings.
  • droplets 8 are charged by a charger 101 and an electric field created between electrode 103 and co- electrode 104 is used to guide droplets 8 close to the surface of substrate 1.
  • the charger 101 is a corona charger and the required high voltage is supplied from a high voltage generator 02.
  • the second precursor flow from second conduit 9 may comprise other precursors required for the coating formation.
  • the precursor flow from second conduit 9 may comprise fluorine precursor flow.
  • Figure 3 shows the preferred atomizer 7 used to realize the present invention.
  • Liquid comprising a precursor is fed into the atomizer from channel 14 and the atomizing gas from channel 15.
  • a pressure chamber 16 is used to provide uniform gas flow through channel 17.
  • the gas flow atomizes the liquid into primary droplets. Chokes 19 homogenize the droplets and fine droplets 8 with narrow droplet size distribution exit from the atomizer 7.
  • the atomizer gas fed through channel 15 may also contain a gaseous precursor or a dopant such as a gaseous fluorine source used in the production of fluorine-doped tin oxide coatings.
  • Figure 2 shows an embodiment for such precursors where two different atomizers 7 (first atomizer) and 7* (second atomizer) or set of two different atomizers 7 and 7 * (first and second atomizers, respectively) are coupled into first conduit 6 and different precursor are atomized in atomizer 7 and atomizer 7* or in a set of two different atomizers 7 and 7 * to droplets 8 and 8*. Additional gas flows 13 are used to guide droplets 8 and 8 * so that they move sideways in first conduit 6 and a homogeneous mixture of droplets 8 and 8* is achieved before the droplets 8 and 8* evaporate on or at the vicinity of substrate 1.
  • Gas flows 13 widen the aerosol flow pattern.
  • Gas flow 13 may include a precursor or a dopant such as a gaseous fluorine source for the production of fluorine doped tin oxide.
  • the atomizers may also be arranged towards each other as shown in Figure 4. When atomizers 7 and 7* are directed essentially towards each other, the droplets 8 and 8 * are effectively mixed.
  • the atomizing gases 14 may differ from each other in different atomizers.
  • the inventors have referred to the formation of doped or undoped Sn0 2 coating in the text above. However, the invention is not limited to the formation of this particular coating, but the invented process and apparatus can be used e.g.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Metallurgy (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Ceramic Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

L'invention concerne un processus de dépôt assisté par aérosol d'un revêtement (2) sur un substrat (1). Le processus comprend un premier flux de précurseur comprenant un aérosol et un deuxième flux de précurseur comprenant au moins un réactif. Le premier flux comprend des gouttelettes et ne contient pratiquement pas de réactif nécessaire pour la formation du revêtement (2). L'invention concerne aussi un appareil de réalisation du processus ainsi que l'utilisation d'un tel appareil.
PCT/FI2012/050219 2011-03-09 2012-03-06 Processus et appareil de revêtement, ainsi que son utilisation Ceased WO2012120194A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FI20115236 2011-03-09
FI20115236A FI20115236A0 (fi) 2011-03-09 2011-03-09 Pinnoitusmenetelmä, laite ja käyttö

Publications (1)

Publication Number Publication Date
WO2012120194A1 true WO2012120194A1 (fr) 2012-09-13

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Application Number Title Priority Date Filing Date
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FI (1) FI20115236A0 (fr)
WO (1) WO2012120194A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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JP2016533890A (ja) * 2013-09-09 2016-11-04 ベネク・オサケユキテュアＢｅｎｅｑ Ｏｙ エアロゾルを製造するための装置および方法、ならびに、焦点調節部品
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US10919799B2 (en) 2015-08-21 2021-02-16 Corning Incorporated Methods and apparatus for processing glass

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