WO2002049979A1 - Procede pour la fabrication d'un produit multicouche, utilisation d'un promoteur d'adhesion associe et application du procede - Google Patents

Procede pour la fabrication d'un produit multicouche, utilisation d'un promoteur d'adhesion associe et application du procede Download PDF

Info

Publication number
WO2002049979A1
WO2002049979A1 PCT/FR2001/003956 FR0103956W WO0249979A1 WO 2002049979 A1 WO2002049979 A1 WO 2002049979A1 FR 0103956 W FR0103956 W FR 0103956W WO 0249979 A1 WO0249979 A1 WO 0249979A1
Authority
WO
WIPO (PCT)
Prior art keywords
inorganic
layer
substrate
glass
product
Prior art date
Application number
PCT/FR2001/003956
Other languages
English (en)
French (fr)
Inventor
Yves Demars
Christophe Rogier
Marco Natali
Christophe Mazzara
Original Assignee
Saint-Gobain Glass France
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 filed Critical Saint-Gobain Glass France
Priority to KR10-2003-7007687A priority Critical patent/KR20030069180A/ko
Priority to EP01271098A priority patent/EP1345863A1/fr
Priority to AU2002219289A priority patent/AU2002219289A1/en
Priority to JP2002551484A priority patent/JP2004516215A/ja
Priority to PL01360948A priority patent/PL360948A1/xx
Publication of WO2002049979A1 publication Critical patent/WO2002049979A1/fr

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/38Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal at least one coating being a coating of an organic material
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/42Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating of an organic material and at least one non-metal coating

Definitions

  • the present invention relates generally to multilayer elements formed from at least one inorganic substrate, in particular made of glass, coated with an inorganic product, in particular a metallic layer.
  • the invention relates to the manufacture of a mirror formed from a glass substrate coated with a metallic layer, for example silver.
  • silver mirrors are produced in the following way: the glass substrate is first polished and then its surface is treated with an aqueous solution of SnCI 2 . This treatment is commonly called sensitization treatment. After rinsing, the glass surface is usually activated by means of an ammoniacal silver nitrate treatment. The silvering solution is then applied to form an opaque silver coating. The silver coating is then usually covered with a protective layer of copper and then with one or more layers of paint to produce the finished mirror.
  • the silver coating does not always adhere sufficiently to the glass substrate. In the case of certain prior products, it has been observed that the silver coating peels off spontaneously from the glass substrate. This is the case, for example, when the silver layer is formed from traditionally manufactured silver microbeads incorporated into a plastic matrix.
  • French patent FR 2 719 839 is known, for example, which describes a method for obtaining good adhesion of a silver coating on the surface of a glassy substrate.
  • the activation step is carried out by bringing the glassy substrate into contact not with ammoniacal silver nitrate but with a particular activation solution such as an aqueous solution of palladium chloride.
  • a particular activation solution such as an aqueous solution of palladium chloride.
  • this document teaches that the awareness step must precede the activation step.
  • the activation step here aims to obtain on the glass surface, palladium chloride nodules strongly linked to the glass and which serve as a sort of attachment points for the silver layer which is then deposited.
  • the present invention relates to a process for manufacturing a multilayer product comprising an inorganic substrate, in particular made of soda-lime-silica glass (glass obtained by the float process) coated with an inorganic product such as a metallic layer.
  • the method consists in using an adhesion promoter to achieve adhesion between an inorganic substrate and an inorganic product, said promoter being chosen from the family of mercaptosilanes having a covalent double bond.
  • the present invention relates to the use of an adhesion promoter to achieve adhesion between an inorganic substrate and an inorganic product.
  • the inorganic substrate is a glass substrate and the inorganic product is a metal, in particular a metallic layer. More specifically, said metallic layer can be a silver layer.
  • the mercaptosilane is chosen from the mercaptosilanes of general formula:
  • the surface of the glass substrate is treated and sensitized before using the mercaptosilane.
  • the deposition of mercaptosilane is carried out by spraying an aqueous solution or emulsion containing it, onto the glass substrate. Furthermore, the treatment of the glass surface consists of washing and brightening (or polishing).
  • awareness consists in forming a layer based on tin.
  • the present invention proposes, as part of a process for manufacturing a multilayer product, an improvement in the interface between two of the layers. and more particularly between a metal-based layer and a layer and / or a glass substrate.
  • the invention particularly relates to a process for manufacturing a multilayer product comprising an inorganic substrate, in particular glass, said substrate undergoing the following treatments:
  • an adhesion promoter being chosen from, the family of mercaptosilanes having a covalent double bond
  • the treatment according to the invention is preferably applied to glass substrates on which a silver coating is applied to form a mirror.
  • the silver coating formed during a so-called silvering step, commonly has a thickness of between 70 nm and 100 nm.
  • the usual step of activating the glass is in fact a treatment of the glass with a given and adapted activation solution and often presents implementation difficulties.
  • this step is replaced by a treatment of said surface with a particular silane, more precisely by a mercaptosilane which is easy to use as will be explained below.
  • Mercaptosilanes are known for their ability to adhere an inorganic element such as a metal to an organic element.
  • the present invention aims to use a mercaptosilane not to adhere an organic element to an inorganic element, but to adhere an inorganic to an inorganic and this very effectively.
  • mirrors - samples - were subjected to attack by hydrochloric acid vapors; the mirrors are placed on the cover of a closed enclosure containing a bath of 37% hydrochloric acid. The silver side of the mirrors is placed towards the bath so that the hydrochloric acid vapors directly attack the silver side of the mirrors.
  • the second ⁇ is a mirror in which the glass has been sensitized
  • the third ® mirror is sensitized and then activated with zero silver ', that is to say with a solution of ammoniacal silver nitrate;
  • the fourth ⁇ D sample is a mirror which has also undergone sensitization and then activation with palladium chloride;
  • the samples were thus exposed for 18 hours in a closed enclosure.
  • a so-called “dishesion by ultrasound tank in HCI bath” test was carried out with the samples ⁇ (D® and ⁇ described above; the test consists in preferably simultaneously immersing the samples in a tank containing a bath hydrochloric acid, and emit ultrasound in the bath. We note the times necessary to completely take off the money on each of the samples.
  • the detachment times are comparable for the ® and ⁇ cases.
  • the bonds created according to the invention are by their nature different from those known previously: the bonds according to the invention are covalent bonds (therefore strong) and numerous with both the inorganic substrate and the inorganic coating product, whereas according to the prior art the bonds are rather of metallic type.
  • the present invention allows real cost reductions since the mercaptosilanes cost a few francs per kilo whereas palladium chloride currently costs around 200 francs per kilo, ie three times the price of gold.
  • a technical advantage is linked to the invention; more specifically, the use of mercaptosilane is easier than that of palladium chloride. Indeed, the palladium chloride precipitates as soon as it is diluted so that when it is then a question of spraying it, there are obstructions of nozzles carrying out the spraying; this leads to lower quality spraying and to the formation of a more or less homogeneous layer. No concern of this nature is possible with the mercaptosilane according to the invention.
  • the metal layer can be based on copper or gold.
  • concentration of mercaptosilane is of the order of 2% in a solution which is preferably aqueous but which could be alcoholic.

Landscapes

  • 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)
  • Surface Treatment Of Glass (AREA)
  • Chemically Coating (AREA)
  • Laminated Bodies (AREA)
  • Optical Elements Other Than Lenses (AREA)
PCT/FR2001/003956 2000-12-20 2001-12-12 Procede pour la fabrication d'un produit multicouche, utilisation d'un promoteur d'adhesion associe et application du procede WO2002049979A1 (fr)

Priority Applications (5)

Application Number Priority Date Filing Date Title
KR10-2003-7007687A KR20030069180A (ko) 2000-12-20 2001-12-12 다층 제품의 제조 방법, 관련된 접착력 증진제의 사용방법 및 상기 제조 방법을 적용하는 방법
EP01271098A EP1345863A1 (fr) 2000-12-20 2001-12-12 Procede pour la fabrication d'un produit multicouche, utilisation d'un promoteur d'adhesion associe et application du procede
AU2002219289A AU2002219289A1 (en) 2000-12-20 2001-12-12 Method for making a multilayer product, use of an associated adhesion promoter and application of said method
JP2002551484A JP2004516215A (ja) 2000-12-20 2001-12-12 多層製品の製造方法、その方法の応用及び付随する接着促進剤の使用
PL01360948A PL360948A1 (en) 2000-12-20 2001-12-12 Method for making a multilayer product, use of an associated adhesion promoter and application of said method

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR00/16648 2000-12-20
FR0016648A FR2818271B1 (fr) 2000-12-20 2000-12-20 Procede pour la fabrication d'un produit multitouche, application du procede et utilisation d'un promoteur d'adhesion associee

Publications (1)

Publication Number Publication Date
WO2002049979A1 true WO2002049979A1 (fr) 2002-06-27

Family

ID=8857915

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/FR2001/003956 WO2002049979A1 (fr) 2000-12-20 2001-12-12 Procede pour la fabrication d'un produit multicouche, utilisation d'un promoteur d'adhesion associe et application du procede

Country Status (9)

Country Link
EP (1) EP1345863A1 (cs)
JP (1) JP2004516215A (cs)
KR (1) KR20030069180A (cs)
CN (1) CN1481341A (cs)
AU (1) AU2002219289A1 (cs)
CZ (1) CZ20031755A3 (cs)
FR (1) FR2818271B1 (cs)
PL (1) PL360948A1 (cs)
WO (1) WO2002049979A1 (cs)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102439491A (zh) * 2009-03-13 2012-05-02 喷射金属技术公司 耐腐蚀镜子、其生产方法及其在太阳能采集中的用途
US8450931B2 (en) 2005-05-10 2013-05-28 Dow Corning Corporation Process for minimizing electromigration in an electronic device

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4521444A (en) * 1982-12-10 1985-06-04 U.S. Philips Corporation Method of providing a metal layer on a substrate
EP0372405A2 (en) * 1988-12-08 1990-06-13 Ppg Industries, Inc. Corrosion inhibitive pretreatment for "copper-free" mirrors
WO1996007487A1 (en) * 1994-09-10 1996-03-14 The University Of Liverpool Method of synthesising materials having controlled electronic, magnetic and/or optical properties

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB9409538D0 (en) 1994-05-12 1994-06-29 Glaverbel Forming a silver coating on a vitreous substrate

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4521444A (en) * 1982-12-10 1985-06-04 U.S. Philips Corporation Method of providing a metal layer on a substrate
EP0372405A2 (en) * 1988-12-08 1990-06-13 Ppg Industries, Inc. Corrosion inhibitive pretreatment for "copper-free" mirrors
WO1996007487A1 (en) * 1994-09-10 1996-03-14 The University Of Liverpool Method of synthesising materials having controlled electronic, magnetic and/or optical properties

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8450931B2 (en) 2005-05-10 2013-05-28 Dow Corning Corporation Process for minimizing electromigration in an electronic device
CN102439491A (zh) * 2009-03-13 2012-05-02 喷射金属技术公司 耐腐蚀镜子、其生产方法及其在太阳能采集中的用途

Also Published As

Publication number Publication date
FR2818271B1 (fr) 2003-08-29
EP1345863A1 (fr) 2003-09-24
CZ20031755A3 (cs) 2004-09-15
FR2818271A1 (fr) 2002-06-21
CN1481341A (zh) 2004-03-10
AU2002219289A1 (en) 2002-07-01
PL360948A1 (en) 2004-09-20
JP2004516215A (ja) 2004-06-03
KR20030069180A (ko) 2003-08-25

Similar Documents

Publication Publication Date Title
BE1008678A3 (fr) Formation d'une couche d'argent sur un substrat vitreux.
CA2054916C (fr) Fabrication d'objets reflechissants
US6127052A (en) Substrate and method for producing it
FR2488831A1 (cs)
FR2727984A1 (fr) Procede pour la catalyse dans le depot chimique
FR2796084A1 (fr) Procede et solution de placage chimique
US2278722A (en) Metallic coating
EP1345863A1 (fr) Procede pour la fabrication d'un produit multicouche, utilisation d'un promoteur d'adhesion associe et application du procede
FR2509744A1 (fr) Protection de films minces d'argent ou de cuivre
JP7196288B2 (ja) 銀変色から保護された銀メッキ表面を含む基材およびそのような基材の製造方法
FR2933105A1 (fr) Procede de depot non-electrolytique
US4937055A (en) Surface treatment for thin metal or semiconductor oxide coatings
RU2010121497A (ru) Зеркало
FR3124805A1 (fr) Substrat revêtu d’au moins une couche de carbone de type diamant protégée par une couche temporaire à base de germanium ou à base d’oxyde de germanium
FR2617291A1 (fr) Miroir cuivre et procede de fabrication d'un tel miroir
WO2014040870A1 (fr) Procede de fabrication d'un miroir sans couche de cuivre
JP2002357709A (ja) 高反射性銀鏡及び反射型光学部品
JP4358950B2 (ja) 光学素子とその製造方法
WO2002040419A1 (fr) Objet a couche metallique, procede de fabrication et applications
FR2741336A1 (fr) Procede de formation d'une couche protectrice sur une couche metallique reflechissante depourvue de cuivre
FR2643775A1 (fr) Procede de realisation de lignes electriquement conductrices sur substrat isolant et circuit hyperfrequence en comportant application
EP0708744B1 (fr) Procede de depot d'un revetement conducteur sur un substrat de verre
CN115198242A (zh) 一种首饰耐磨黄金镀层的制备方法
SU1123999A1 (ru) Способ обработки поверхности диэлектриков перед химической металлизацией
FR2554046A1 (fr) Stratifie recouvert de metal et procede de fabrication

Legal Events

Date Code Title Description
AK Designated states

Kind code of ref document: A1

Designated state(s): AE AG AL AM AT AU AZ BA BB BG BR BY BZ CA CH CN CO CR CU CZ DE DK DM DZ EC EE ES FI GB GD GE GH GM HR HU ID IL IN IS JP KE KG KP KR KZ LC LK LR LS LT LU LV MA MD MG MK MN MW MX MZ NO NZ PL PT RO RU SD SE SG SI SK SL TJ TM TR TT TZ UA UG US UZ VN YU ZA ZW

AL Designated countries for regional patents

Kind code of ref document: A1

Designated state(s): GH GM KE LS MW MZ SD SL SZ TZ UG ZM ZW AM AZ BY KG KZ MD RU TJ TM AT BE CH CY DE DK ES FI FR GB GR IE IT LU MC NL PT SE TR BF BJ CF CG CI CM GA GN GQ GW ML MR NE SN TD TG

DFPE Request for preliminary examination filed prior to expiration of 19th month from priority date (pct application filed before 20040101)
121 Ep: the epo has been informed by wipo that ep was designated in this application
WWE Wipo information: entry into national phase

Ref document number: 698/KOLNP/2003

Country of ref document: IN

WWE Wipo information: entry into national phase

Ref document number: 2001271098

Country of ref document: EP

WWE Wipo information: entry into national phase

Ref document number: 1020037007687

Country of ref document: KR

WWE Wipo information: entry into national phase

Ref document number: 2002551484

Country of ref document: JP

Ref document number: 2003/00935

Country of ref document: TR

WWE Wipo information: entry into national phase

Ref document number: 018209858

Country of ref document: CN

Ref document number: PV2003-1755

Country of ref document: CZ

WWP Wipo information: published in national office

Ref document number: 1020037007687

Country of ref document: KR

WWP Wipo information: published in national office

Ref document number: 2001271098

Country of ref document: EP

REG Reference to national code

Ref country code: DE

Ref legal event code: 8642

WWP Wipo information: published in national office

Ref document number: PV2003-1755

Country of ref document: CZ

WWR Wipo information: refused in national office

Ref document number: PV2003-1755

Country of ref document: CZ

WWW Wipo information: withdrawn in national office

Ref document number: 2001271098

Country of ref document: EP