WO2012167804A1 - Procédé pour revêtir un substrat avec des nanoparticules d'argent - Google Patents

Procédé pour revêtir un substrat avec des nanoparticules d'argent Download PDF

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Publication number
WO2012167804A1
WO2012167804A1 PCT/EP2011/002806 EP2011002806W WO2012167804A1 WO 2012167804 A1 WO2012167804 A1 WO 2012167804A1 EP 2011002806 W EP2011002806 W EP 2011002806W WO 2012167804 A1 WO2012167804 A1 WO 2012167804A1
Authority
WO
WIPO (PCT)
Prior art keywords
substrate
silver
coating
silver nanoparticles
nitrobenzene
Prior art date
Application number
PCT/EP2011/002806
Other languages
English (en)
Inventor
Mohammed Rafiq Hussain Siddiqui
Abdulrahman AL-WARTHAN
Syed Farooq ADIL
Original Assignee
King Saud University
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 King Saud University filed Critical King Saud University
Priority to EP11729057.7A priority Critical patent/EP2718478B1/fr
Priority to PCT/EP2011/002806 priority patent/WO2012167804A1/fr
Publication of WO2012167804A1 publication Critical patent/WO2012167804A1/fr

Links

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
    • 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
    • C23C18/08—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 metallic material

Definitions

  • the present invention relates to a method for coating a substrate with silver nanoparticles.
  • Silver coatings on a substrate are well known in the art.
  • Tollens ' reaction i.e. the test for aldehydes resulting in the formation of a silver mirror due to reduction of silver ions
  • respective further coatings are also known from US 5, 186,984, 3,978,271, 5,346,651, 4,894,290 and 4,652,465.
  • US2007/0018140 Al discloses a method of producing metal nanoparticles, said method comprising (a) producing a metal alkanoate by reacting a metal precursor with an alkanoate of an alkali metal, alkali earth metal, or ammonium in an aqueous solution; (b) filtrating and drying the metal alkanoate; and (c) heat-treating the alkanoate of (b).
  • a method for coating a substrate with silver nanoparticles comprising the steps: contacting the substrate with a solution of silver Cg-Cig alkanoate, preferably oleate, in nitrobenzene, and refluxing the solution of silver Cg-Cis alkanoate in nitrobenzene at 215-25CPC, preferably 22CPC, for 1-5 hours, preferably 3 hours.
  • the method additionally comprises the steps: removing the solution after refluxing from the substrate, washing the substrate, and drying the substrate.
  • washing is done at least once with acetone and/or hexane.
  • the silver nanoparticles have a size of about 10-50 nm, and/or wherein the coating has a thickness of about 5-40 nm.
  • the substrate is glass.
  • More preferred silver alkanoate is added to nitrobenzene if the nitrobenzene is already refluxing.
  • the invention also provides a substrate coated with silver nanoparticles obtained by a method according to the invention.
  • the inventive method allows easy coating of a substrate, preferably a glass substrate, with a silver coating.
  • the inventive method is simple, facile, straight forward and easy to execute, both at small and larger scales. It can be also applied on an industrial level.
  • the method employed according to the present invention utilizes a silver alkanoate, especially a silver oleate as a source of silver.
  • the silver oleate can be also considered as a capping agent.
  • the inventive method involves the solvent to be heated, preferably followed by the addition of the silver salt while stirring.
  • a substrate for example glass plates (slides) can be placed into the solution prior to the addition of a silver salt.
  • the reaction is carried out under reflux of the solvent for a period of time, preferably about 3 hours, and is then allowed to cool.
  • the substrate can be removed from the reaction, can be optionally washed and dried, and the substrate is found to be coated with silver.
  • the coated substrate can be characterized using various analytical techniques such as AFM (Atomic Force Microscopy), SEM (Scanning Electron Microscopy) and TEM (Transmission Electron Microscopy).
  • AFM Atomic Force Microscopy
  • SEM Scanning Electron Microscopy
  • TEM Transmission Electron Microscopy
  • the silver particles are preferably in the range of 10 bis 50 nm. It has been also found that the coating on the substrate has preferably a thickness of about 5-40 nm.
  • the coated substrate obtained by the method of the present invention can be, for example, used as silver mirror without any backing support necessary, as anti reflective coating, for example for buildings, cars and glasses, as biofilms, as casing of electronic equipments, in electronic circuit boards, or in biology and medicine for antibacterial, antiviral and anticancer activity.
  • the inventive method is based on a solvothermal process utilizing a single step process that can be used for coating substrates, such as glass surfaces, for use of reflective purposes and as mirror without the presence of any backing material.
  • figure 1 shows a ! H HMR spectrum of silver oleate prepared according to example 1 ;
  • figures 2 and 3 show SEM images of silver nanoparticles as prepared according to example 2; and
  • figures 4 and 5 show AFM images of silver nanoparticles coated on glass according to example 3.
  • Preparation of silver oleate 10 grams of silver nitrate is introduced in a beaker and dissolved in a minimum quantity of water. 5 grams of sodium oleate is introduced in another beaker and dissolved in a minimum quantity of water, with heating and stirring, using a hot plate stirrer. After complete dissolution of sodium oleate, the solution is allowed to cool down to room temperature. Then, the silver nitrate solution is added to the oleate solution, slowly while being stirred, and the silver oleate is formed as a solid. The precipitate obtained is filtered and dried in an oven to give a white powder. This powder has been characterized and confirms the formation of silver oleate.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Chemically Coating (AREA)

Abstract

La présente invention concerne un procédé pour revêtir un substrat avec des nanoparticules d'argent comprenant les étapes de mise en contact du substrat avec une solution d'alcanoate en C8-C18 d'argent, de préférence un oléate, dans du nitrobenzène, et le chauffage à reflux de la solution d'alcanoate en C8-C18 d'argent dans du nitrobenzène à 215 à 250 °C, de préférence 220 °C, pendant 1 à 5 heures, de préférence 3 heures.
PCT/EP2011/002806 2011-06-08 2011-06-08 Procédé pour revêtir un substrat avec des nanoparticules d'argent WO2012167804A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP11729057.7A EP2718478B1 (fr) 2011-06-08 2011-06-08 Procédé pour revêtir un substrat avec des nanoparticules d'argent
PCT/EP2011/002806 WO2012167804A1 (fr) 2011-06-08 2011-06-08 Procédé pour revêtir un substrat avec des nanoparticules d'argent

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/EP2011/002806 WO2012167804A1 (fr) 2011-06-08 2011-06-08 Procédé pour revêtir un substrat avec des nanoparticules d'argent

Publications (1)

Publication Number Publication Date
WO2012167804A1 true WO2012167804A1 (fr) 2012-12-13

Family

ID=44627805

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2011/002806 WO2012167804A1 (fr) 2011-06-08 2011-06-08 Procédé pour revêtir un substrat avec des nanoparticules d'argent

Country Status (2)

Country Link
EP (1) EP2718478B1 (fr)
WO (1) WO2012167804A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10422033B2 (en) 2017-02-22 2019-09-24 King Saud University Green method for coating a substrate with silver nanoparticles

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3345199A (en) * 1963-08-16 1967-10-03 Engelhard Ind Inc Decorating composition and method for decorating therewith
US3978271A (en) 1975-04-15 1976-08-31 Ppg Industries, Inc. Thin metallic nickel-silver films by chemical replacement
US4652465A (en) 1984-05-14 1987-03-24 Nissan Chemical Industries Ltd. Process for the production of a silver coated copper powder and conductive coating composition
US4894290A (en) 1986-01-29 1990-01-16 Pilkington Brothers P.L.C. Coated glass
US5059242A (en) * 1990-04-27 1991-10-22 Firmstone Michael G Seed layer compositions containing organogold and organosilver compounds
US5186984A (en) 1990-06-28 1993-02-16 Monsanto Company Silver coatings
US5342973A (en) * 1986-02-24 1994-08-30 Scientific Design Company, Inc. Process for preparing silver salt solutions
US5346651A (en) 1993-08-31 1994-09-13 Cerdec Corporation Silver containing conductive coatings
US20070018140A1 (en) 2005-07-22 2007-01-25 Samsung Electro-Mechanics Co., Ltd. Metal nanoparticles and method for producing the same

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3345199A (en) * 1963-08-16 1967-10-03 Engelhard Ind Inc Decorating composition and method for decorating therewith
US3978271A (en) 1975-04-15 1976-08-31 Ppg Industries, Inc. Thin metallic nickel-silver films by chemical replacement
US4652465A (en) 1984-05-14 1987-03-24 Nissan Chemical Industries Ltd. Process for the production of a silver coated copper powder and conductive coating composition
US4894290A (en) 1986-01-29 1990-01-16 Pilkington Brothers P.L.C. Coated glass
US5342973A (en) * 1986-02-24 1994-08-30 Scientific Design Company, Inc. Process for preparing silver salt solutions
US5059242A (en) * 1990-04-27 1991-10-22 Firmstone Michael G Seed layer compositions containing organogold and organosilver compounds
US5186984A (en) 1990-06-28 1993-02-16 Monsanto Company Silver coatings
US5346651A (en) 1993-08-31 1994-09-13 Cerdec Corporation Silver containing conductive coatings
US20070018140A1 (en) 2005-07-22 2007-01-25 Samsung Electro-Mechanics Co., Ltd. Metal nanoparticles and method for producing the same

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10422033B2 (en) 2017-02-22 2019-09-24 King Saud University Green method for coating a substrate with silver nanoparticles

Also Published As

Publication number Publication date
EP2718478B1 (fr) 2016-03-23
EP2718478A1 (fr) 2014-04-16

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