EP1678095A1 - Substrat, notamment substrat verrier, portant au moins un empilement couche a propriete photocatalytique / sous-couche de croissance heteroepitaxiale de ladite couche - Google Patents

Substrat, notamment substrat verrier, portant au moins un empilement couche a propriete photocatalytique / sous-couche de croissance heteroepitaxiale de ladite couche

Info

Publication number
EP1678095A1
EP1678095A1 EP04805775A EP04805775A EP1678095A1 EP 1678095 A1 EP1678095 A1 EP 1678095A1 EP 04805775 A EP04805775 A EP 04805775A EP 04805775 A EP04805775 A EP 04805775A EP 1678095 A1 EP1678095 A1 EP 1678095A1
Authority
EP
European Patent Office
Prior art keywords
layer
glass
ati0
sublayer
structure according
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Withdrawn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
EP04805775A
Other languages
German (de)
English (en)
French (fr)
Inventor
Laurent Labrousse
Nicolas Nadaud
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.)
Saint Gobain Glass France SAS
Compagnie de Saint Gobain SA
Original Assignee
Saint Gobain Glass France SAS
Compagnie de Saint Gobain SA
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 Saint Gobain Glass France SAS, Compagnie de Saint Gobain SA filed Critical Saint Gobain Glass France SAS
Publication of EP1678095A1 publication Critical patent/EP1678095A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • C03C17/23—Oxides
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
    • C03C17/3417—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials all coatings being oxide coatings
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B18/00—Layered products essentially comprising ceramics, e.g. refractory products
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
    • C03C17/3429—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating
    • C03C17/3435—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating comprising a nitride, oxynitride, boronitride or carbonitride
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10—Coating
    • C03C25/48—Coating with two or more coatings having different compositions
    • C03C25/52—Coatings containing inorganic materials only
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/70—Properties of coatings
    • C03C2217/71—Photocatalytic coatings

Definitions

  • the present invention relates to substrates such as substrates made of glass, glass-ceramic material or plastic which have been provided with a coating with photocatalytic property to give them a so-called anti-soiling or self-cleaning function.
  • An important application of these substrates relates to glazing, which can be of very diverse applications, from utility glazing to glazing used in household appliances, glazing for vehicles to glazing for buildings. It also applies to reflective glazing of the mirror type (home mirror or vehicle rear view mirror) and opaque glazing of the light type.
  • the invention also applies, similarly, to non-transparent substrates, such as ceramic substrates or any other substrate which can in particular be used as an architectural material (metal, tiles, etc.). It preferably applies, whatever the nature of the substrate, to substantially planar or slightly curved substrates.
  • Photocatalytic coatings have already been studied, in particular those based on titanium oxide crystallized in anatase form. Their ability to degrade dirt of organic origin or microorganisms under the effect of UV radiation is very interesting. They also often have a hydrophilic nature, which allows the evacuation of mineral soiling by spraying water or, for exterior glazing, by rain. This type of coating with anti-fouling, bactericidal and algicidal properties has already been described, in particular in patent WO 97/10186, which describes several methods of obtaining it. To exercise its anti-fouling function
  • Ti0 2 must be at least partially crystallized in the atanase structure. Otherwise Ti0 2 is not functional and requires heat treatment after deposition in order to acquire the crystallographic structure which makes it effective. Thus, since Ti0 2 is deposited by a gas phase pyrolysis technique (CVD type) involving a high temperature, it spontaneously has the right structure. If it is deposited cold (room temperature), in particular by a vacuum deposition technique, it becomes functional only after a suitable heat treatment.
  • CVD type gas phase pyrolysis technique
  • the present invention aims to provide a solution for obtaining the good state of Ti0 2 without necessarily calling for a heating step.
  • the present invention therefore firstly relates to a structure comprising a substrate carrying, on at least part of its surface, a layer with photocatalytic property, anti-fouling, based on titanium dioxide (Ti0 2 ) at least in part crystallized in its anatase form, characterized in that it comprises, immediately below at least one layer of Ti0 2 , an under-layer (SC) having a crystallographic structure having enabled assistance to crystallization by heteroepitaxial growth in the anatase form of the upper layer based on Ti0 2 , the photocatalytic property having been acquired without any heating step.
  • Ti0 2 titanium dioxide
  • SC under-layer
  • sublayer (SC) is in particular based on a compound crystallized in a cubic or tetragonal system and having a mesh whose dimension is that of Ti0 2 crystallized in anatase form to within 8%, in particular to within 6% .
  • the sublayer (SC) consists of ATi0 3 , A denoting barium or strontium.
  • the thickness of the underlay (SC) is not critical. Mention may in particular be made of values between 10 and 100 nm for this thickness.
  • the substrate consists, for example, of a plate, flat or with curved or curved faces, of monolithic or laminated glass, of glass-ceramic material or of a hard thermoplastic material, such as polycarbonate, or also of glass fibers or glass-ceramic, said plates or said fibers having, where appropriate, received at least one other layer functional before the application of the sublayer (SC) (in the case of more than one layer, we can also speak of stacking of layers).
  • SC sublayer
  • the applications of the plates have been mentioned above.
  • fibers mention may be made of their application to the filtration of air or water, as well as bactericidal applications.
  • At least one functional layer underlying the sublayer (SC) can be a layer which forms a barrier to the migration of alkalis from the glass or ceramic glass material. Such migration may result from the application of temperatures in excess of 600 C C.
  • layers forming alkali-barrier are known, and there may be mentioned layers of Si0 2, SiOC, SiO x Ny, thickness of e.g. 'at least 50 will, as described in international PCT application WO 02/24971.
  • At least one functional layer underlying the sublayer (SC) can be an optically functional layer (advantageously for adjusting the optics in reflection), a thermal control layer or a conductive layer.
  • the layers with optical functionality are in particular anti-reflection layers, light radiation filtration, coloring, diffusing, etc. Mention may be made of the layers of Si0 2 , Si 3 N, Ti0 2 amorphous or crystallized and photocatalytic, Sn0 2 , ZnO.
  • the thermal control layers are in particular the solar control layers, or the so-called low-emissivity layers.
  • the conductive layers are in particular the heating, antenna or anti-static layers, among these layers, one can count the networks of conductive wires.
  • substrates made of glass or glass-ceramic material in particular of plate type, having received a layer forming a barrier to the migration of alkalis from glass or glass-ceramic material, then a mono-, bi- or three-layer with optical functionality.
  • the Ti0 2- based layer consists of
  • the Ti0 2 layer was deposited at room temperature by sputtering under vacuum, if necessary assisted by magnetic field (magnetron) and / or ion beam; - the sublayer (SC) was deposited at room temperature by cathodic sputtering under vacuum, if necessary assisted by magnetic field and / or ion beam; ATi0 3 was deposited at room temperature by cathode sputtering under vacuum, if necessary assisted by magnetic field and / or ion beam, " with the use of ceramic targets chosen from ATi0 3 , ATi0 3 _ x with 0 ⁇ x ⁇ 3 , and ATi; the power supply being a radiofrequency power supply and the atmosphere of the sputtering enclosure containing only argon when ATi0 3 is used as target; the power supply being a power supply direct or alternating current and the reactive atmosphere of the sputtering enclosure containing oxygen and argon in the case of the use of ATi or ATi0 3 - x as target; the layer
  • the layer of Ti0 2 can be coated with at least one over-layer of a material which does not disturb the anti-fouling function of the layer of Ti0 2 , such as Si0 2 .
  • the layers intended to be in contact with the atmosphere in the finished structure are, depending on the case, hydrophilic or hydrophobic layers.
  • the present invention also relates to the application of ATi0 3 to the constitution of an assisting layer for crystallization in the anatase form by heteroepitaxial growth of an upper layer based on optionally doped Ti0 2 , A denoting barium or strontium.
  • the present invention also relates to a method of manufacturing a structure as defined above, characterized in that one deposits on a substrate of glass or glass-ceramic material or hard plastic material of polycarbonate type, plate type, or on glass or glass-ceramic fibers, an ATi0 3 sublayer, A representing barium or strontium, then a layer of Ti0 2 possibly doped, at least one overlay of a material which does not disturb not the anti-fouling function of the Ti0 2 layer which can then be deposited if necessary on the latter.
  • the deposition of the ATi0 sublayer (SC) and that of the Ti0 2 layer can be carried out successively at room temperature by sputtering, under vacuum, if necessary assisted by magnetic field and / or ion beam, in the same enclosure, the targets used for the deposition of said sublayer being chosen from ATi0 3 , ATi0 3 - x with 0 ⁇ x ⁇ 3, and ATi, the supply being a radiofrequency supply and the atmosphere of the sputtering enclosure containing only argon when using ATi0 3 as a target; the power supply being a DC or AC power supply and the reactive atmosphere of the sputtering enclosure containing oxygen and argon, in the case of the use of ATi or ATi0 3 - x as target; and the target used for the deposition of Ti0 2 being Ti or TiO x , 0 ⁇ x ⁇ 2.
  • the pressure can be between 10 "1 and 2.5 Pa.
  • the supply is generally a direct current or alternating current supply, and the pressure is advantageously of the order of 1-3 Pa.
  • the coating of a substrate is made of glass or glass-ceramic material
  • SC undercoat
  • deposit on the substrate at least one layer forming a barrier to the migration of alkalis present in the glass or glass-ceramic material an annealing or quenching which can then be made after the filing of the co uche of Ti0 2 and, where appropriate, of the overcoat (s) at a temperature between 250 ° C. and 550 ° C., preferably between 350 ° C. and 500 ° C. for annealing, and at a temperature of at least 600 ° C for quenching.
  • the quenching or annealing operations can be carried out in cases where it is desired to improve the activity of the Ti0 2 layer.
  • Such layers can be deposited by sputtering, optionally assisted by magnetic field, from known targets (for example Si: Al in the case of a layer of Si0 2 doped aluminum), advantageously in pulsed mode, AC (alternating current) or DC (direct current), under a pressure of 10 "1 to 1 Pa, and under argon and oxygen gas.
  • targets for example Si: Al in the case of a layer of Si0 2 doped aluminum
  • AC alternating current
  • DC direct current
  • the present invention also relates to a single or multiple glazing unit comprising respectively one or more of a structure as defined above, the anti-fouling layer based on Ti0 2 and its associated undercoat (SC) being present on at least one of its external faces, the faces not having the anti-fouling layer based on Ti0 2 and its associated undercoat which may comprise at least ins another functional layer.
  • These functional layers can be chosen from those described above.
  • Such glazing finds its application as "self-cleaning" glazing, in particular anti-fogging, anti-condensation and anti-fouling, in particular glazing for the building of the double-glazing type, glazing for vehicle of the windshield type, rear window, side windows automotive, rear view mirror, glazing for train, plane, boat, utility glazing like aquarium glass, display case, greenhouse, interior furniture, street furniture (bus shelters, advertising panel %), mirror, display system computer, television, telephone, electrically controllable glazing such as electrochromic, liquid crystal, electroluminescent, photovoltaic glazing.
  • the following examples illustrate the present invention without, however, limiting its scope.
  • Example 1 (of the invention): Stacking - glass / Si0 2 / BaTi0 3 / Ti0 2
  • the following successive layers were deposited on a glass plate 4 mm thick: - a layer of Si0 2 150 nm thick; - a layer of BaTi0 3 10 nm thick; and - a layer of Ti0 2 100 nm thick.
  • the three above layers of Si0 2 , BaTi0 3 and Ti0 2 were deposited by sputtering assisted by magnetic field (magnetron) under the following respective conditions: layer of Si0 2 from a target Si: Al, with a supply in pulsed mode (frequency of polarity change of 30 kHz) under a pressure of 2 x 10 "3 mbar (0.2 Pa), a power of 2000 W, and 15 sccm of Ar and 15 sccm of 0 2 ; layer of BaTi0 3 from a target of BaTi0 3 , with a radio frequency supply, under a pressure of 4.4 x 10 "3 mbar (0.44 Pa), a power of 350 W, and 50 sccm d 'argon; Ti0 2 layer deposited from a TiO x target, with a DC power supply, under a pressure of 24 x 10 ⁇ 3 mbar (2.4 Pa), a power of 2000 W, 200 sccm of Ar and 2 sccm
  • Example 3 (comparative): Glass stack / SiQ 2 / TiQ 2
  • the above stack was made under the same conditions as in Example 1, except that the layer of BaTi0 3 was not deposited.
  • the photocatalytic activity of the layer of Ti0 2 of each of the stacks of Examples 1 to 3 was evaluated, as well as of the layer of Ti0 2 of a stack sold by the Company Saint-Gobain Glass France under the brand “Bioclean TM ”, The evaluation having been made without annealing, and after annealing carried out under the following conditions: rise in the ambient temperature to 500 ° C. at a speed of 5 ° C / min, 2 hours at 500 ° C., natural cooling.
  • the evaluation test is the photodegradation test of stearic acid followed by infrared transmission, described in international PCT application WO 00/75087. The results are collated in Table I.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Surface Treatment Of Glass (AREA)
  • Catalysts (AREA)
  • Laminated Bodies (AREA)
  • Physical Vapour Deposition (AREA)
  • Finishing Walls (AREA)
EP04805775A 2003-10-23 2004-10-22 Substrat, notamment substrat verrier, portant au moins un empilement couche a propriete photocatalytique / sous-couche de croissance heteroepitaxiale de ladite couche Withdrawn EP1678095A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR0350729A FR2861385B1 (fr) 2003-10-23 2003-10-23 Substrat, notamment substrat verrier, portant au moins un empilement couche a propriete photocatalytique sous couche de croissance heteroepitaxiale de ladite couche
PCT/FR2004/050532 WO2005040058A1 (fr) 2003-10-23 2004-10-22 Substrat, notamment substrat verrier, portant au moins un empilement couche a propriete photocatalytique / sous-couche de croissance heteroepitaxiale de ladite couche

Publications (1)

Publication Number Publication Date
EP1678095A1 true EP1678095A1 (fr) 2006-07-12

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Family Applications (1)

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EP04805775A Withdrawn EP1678095A1 (fr) 2003-10-23 2004-10-22 Substrat, notamment substrat verrier, portant au moins un empilement couche a propriete photocatalytique / sous-couche de croissance heteroepitaxiale de ladite couche

Country Status (8)

Country Link
US (1) US7737080B2 (zh)
EP (1) EP1678095A1 (zh)
JP (1) JP5290519B2 (zh)
KR (1) KR101131532B1 (zh)
CN (1) CN1898173B (zh)
CA (1) CA2543075C (zh)
FR (1) FR2861385B1 (zh)
WO (1) WO2005040058A1 (zh)

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CN1898173A (zh) 2007-01-17
US7737080B2 (en) 2010-06-15
JP5290519B2 (ja) 2013-09-18
FR2861385A1 (fr) 2005-04-29
JP2007508933A (ja) 2007-04-12
CA2543075C (fr) 2013-05-28
US20070129248A1 (en) 2007-06-07
KR101131532B1 (ko) 2012-04-04
WO2005040058A1 (fr) 2005-05-06
FR2861385B1 (fr) 2006-02-17
KR20060090830A (ko) 2006-08-16
CA2543075A1 (fr) 2005-05-06
CN1898173B (zh) 2012-11-14

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