WO2009098655A2 - Pellicules antibactériennes obtenues par pulvérisation, et procédé permettant de conférer des propriétés antibactériennes à un substrat - Google Patents

Pellicules antibactériennes obtenues par pulvérisation, et procédé permettant de conférer des propriétés antibactériennes à un substrat Download PDF

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Publication number
WO2009098655A2
WO2009098655A2 PCT/IB2009/050476 IB2009050476W WO2009098655A2 WO 2009098655 A2 WO2009098655 A2 WO 2009098655A2 IB 2009050476 W IB2009050476 W IB 2009050476W WO 2009098655 A2 WO2009098655 A2 WO 2009098655A2
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WO
WIPO (PCT)
Prior art keywords
antibacterial
substrate
silver
antibacterial properties
sputtering
Prior art date
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Ceased
Application number
PCT/IB2009/050476
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English (en)
Other versions
WO2009098655A3 (fr
Inventor
Monica Ferraris
Diego Chiaretta
Michael Fokine
Marta Miola
Enrica Verne'
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Politecnico di Torino
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Politecnico di Torino
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.)
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Publication date
Application filed by Politecnico di Torino filed Critical Politecnico di Torino
Publication of WO2009098655A2 publication Critical patent/WO2009098655A2/fr
Publication of WO2009098655A3 publication Critical patent/WO2009098655A3/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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/10—Glass or silica
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment

Definitions

  • the present invention relates to a method for conferring antibacterial properties to a substrate, and to substrates provided with antibacterial coating.
  • antibacterial materials have been identified, among which natural and inorganic substances, such as tea extracts, chitosan, copper, zinc, and silver.
  • natural and inorganic substances such as tea extracts, chitosan, copper, zinc, and silver.
  • silver or silver ions are well known due to their powerful antibacterial activity.
  • JP 2005263767 discloses antibacterial films obtained using a composite aqueous solution comprising an alkaline silicate solution and an aqueous silicate solution containing crystalline particles of silicon dioxide and copper.
  • a composite aqueous solution comprising an alkaline silicate solution and an aqueous silicate solution containing crystalline particles of silicon dioxide and copper.
  • a number of articles relate to the formation of silica particles through the St ⁇ ber method, followed by a coating of silver/silver nanoparticles with the formation of an antibacterial composite; see reference texts [4, 5].
  • these composites are not mechanically stable, and require to be melted in order to produce thin films or coatings, following which it is difficult to control the silver/silver ion ratio. Again, the high temperatures involved make the use of these methods difficult to coat some polymers.
  • the reference text [6] discloses the formation of nanoparticles on the silica surface, thus obtaining structures which suffer from a reduced mechanical stability.
  • antibacterial coatings are described which are obtained by using conventional melting techniques of silver-doped glasses. These techniques require high temperature treatments of the whole substrate to be coated, therefore they have a reduced applicability.
  • the chemical vapour deposition has been used to deposit titanium dioxide films containing silver ions, (see reference texts [9, 10]), as well as inorganic films containing silver ions.
  • the drawback of the known techniques for the deposition of antibacterial films consists in that such techniques do not allow obtaining coatings provided with a suitable thermal and mechanical stability; furthermore, the time-related release of silver ions is efficient for a short period of time, following which the antibacterial properties decrease or cease.
  • Object of the present invention is to provide a method that allows obtaining a coating suitable to any substrates, provided with wear and aging mechanical and thermal resistance, while obtaining antibacterial properties which are active for an extended period of time.
  • a method to confer antibacterial properties to a substrate characterised in that it comprises the coating of said substrate with a film comprising a glass, ceramic, or glass-ceramic material, and a metal having antibacterial properties, by radio-frequency co-sputtering.
  • the radio-frequency co-sputtering technique (rf) employing a silica-based glass and a metal with antibacterial properties as targets, the preparation and deposition of silica- based thin films containing high concentrations of the metal and the metallic ion having antibacterial properties are made possible.
  • the technique allows obtaining a coating with mechanical and thermal resistance properties, and due to the stability of the silica films, the antibacterial ion release also has a time-stable behaviour.
  • the concentration of the antibacterial metal ions can be controlled in order to confer suitable antibacterial properties and, thus, also a suitable duration of the effectiveness time.
  • the co-sputtering technique using silver and silica as targets is described in detail in the reference text [9],
  • the main object of this publication was to obtain films containing metallic nanoparticles of silver in silica films for applications in the photonics and sensor systems field. Through such method, the application of an annealing thermal treatment stage is possible, during which the silver ions diffusion and the aggregation thereof is caused, in order to form metallic silver nanoparticles.
  • the method according to the invention may optionally contemplate a high temperature thermal treatment stage that, anyhow, may generally reduce the antibacterial effectiveness, if it is not carried out in the proper manner. Since the annealing causes the antibacterial agent formation in the metallic form, at the expense of the ionic form, the ionic form availability is consequently reduced. However, an appropriate annealing can be advantageous to the aim of modifying the release rate of the ions of the metal having antibacterial properties, and modifying the antibacterial properties and the effectiveness duration of the film.
  • Preferred thermal treatment conditions range between 400°C and 800 0 C, and for periods of time ranging between 30 and 90 minutes.
  • the metal having antibacterial properties can be selected particularly from copper, zinc, and silver, silver being the preferred metal.
  • the usable siliceous materials comprise glass, ceramic, and glass-ceramic materials, including materials having bioactive properties.
  • the method according to the invention can be applied to the antibacterial film formation on different materials, including polymers, glasses, ceramic materials, metals, and alloys.
  • the applications include any substrates, surfaces, or devices in relation to which it is advantageous to achieve antibacterial properties, while providing a coating surface which is mechanically and thermally stable for extended periods of time.
  • the rf-co-sputtering technique disclosed in the reference text [9] is used, without application of a thermal treatment.
  • Silica or silicon was used as a substrate.
  • a conventional sputtering chamber in an inert atmosphere was used, where the metal-glass target was obtained by gluing small silver plates (10 mm diameter) on a glass surface with a conductive silver-based glue.
  • the deposition parameters of the rf-sputtering method can be varied in order to optimize their influence on the silver concentration in the coating film.
  • a bacterial broth was prepared by melting a Staphylococcus aureus (ATCC 29213) freeze- dried disc in 5 ml Brain Heart medium, and it was incubated at 35 0 C overnight; then, 10 ⁇ l suspension were extracted, which were spread on a blood-agar plate to allow bacterial growth and CFU (Colonies Forming Units) formation.
  • Staphylococcus aureus ATCC 29213 freeze- dried disc in 5 ml Brain Heart medium, and it was incubated at 35 0 C overnight; then, 10 ⁇ l suspension were extracted, which were spread on a blood-agar plate to allow bacterial growth and CFU (Colonies Forming Units) formation.
  • Mc Farland 0.5 suspension (containing approximately 1 - 2x10 8 CFU/ml) was prepared by inoculating some colonies which were grown on the plate in physiologic solution.
  • the Mc Farland index is a measurement of the solution cloudiness (a cloudy solution has a higher bacterial content than a clear solution), and an optical assessment was carried out (Phoenix Spec BD Mc Farland).
  • an aliquot of the described suspension was evenly spread on a Mueller Hinton agar plate; the silver-containing samples were deposited on the agar surface and incubated at 35 0 C for 24 hours.
  • the antibacterial behaviour was assessed by observing the inhibition halo, that is, a zone where the bacteria had not grown, all around the samples after incubation.
  • the inhibition zone assessment tests demonstrate the effective antibacterial properties of the samples: silver ions coming from the glass surface produce a significant and reproducible halo of about 6mm all around the sample.
  • NCCLS M2-A9 Performance Standards for Antimicrobial Disk Susceptibility Tests, Approved Standard - Ninth Edition.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Surface Treatment Of Glass (AREA)
  • Laminated Bodies (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

Cette invention concerne un procédé permettant de conférer des propriétés antibactériennes à un substrat, caractérisé en ce qu'il comprend le recouvrement dudit substrat par une pellicule composée de verre, de céramique ou d'un matériau de verre-céramique, et un métal ayant des propriétés antibactériennes, par co-pulvérisation radiofréquence.
PCT/IB2009/050476 2008-02-08 2009-02-05 Pellicules antibactériennes obtenues par pulvérisation, et procédé permettant de conférer des propriétés antibactériennes à un substrat Ceased WO2009098655A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ITTO2008A000098 2008-02-08
ITTO20080098 ITTO20080098A1 (it) 2008-02-08 2008-02-08 Pellicole antibatteriche ottenute da sputtering e procedimento per conferire proprieta antibatteriche ad un substrato

Publications (2)

Publication Number Publication Date
WO2009098655A2 true WO2009098655A2 (fr) 2009-08-13
WO2009098655A3 WO2009098655A3 (fr) 2009-12-03

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PCT/IB2009/050476 Ceased WO2009098655A2 (fr) 2008-02-08 2009-02-05 Pellicules antibactériennes obtenues par pulvérisation, et procédé permettant de conférer des propriétés antibactériennes à un substrat

Country Status (2)

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IT (1) ITTO20080098A1 (fr)
WO (1) WO2009098655A2 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108570649A (zh) * 2018-04-26 2018-09-25 常州龙腾光热科技股份有限公司 一种区域表面等离子体增强超薄宽带复合吸收膜
GB202011249D0 (en) 2020-07-21 2020-09-02 Pilkington Group Ltd Antimicrobial substrate
WO2020183204A1 (fr) 2019-03-14 2020-09-17 Pilkington Technology Management Limited Revêtement antimicrobien
WO2022058734A1 (fr) 2020-09-16 2022-03-24 Pilkington Group Limited Revêtement antimicrobien et antiviral
WO2022090708A1 (fr) 2020-10-26 2022-05-05 Pilkington Group Limited Utilisation de substrats revêtus

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100425330C (zh) * 2005-03-31 2008-10-15 鸿富锦精密工业（深圳）有限公司 光催化增强装置
SG172722A1 (en) * 2006-06-21 2011-07-28 Agc Glass Europe Substrate with antimicrobial properties

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108570649A (zh) * 2018-04-26 2018-09-25 常州龙腾光热科技股份有限公司 一种区域表面等离子体增强超薄宽带复合吸收膜
WO2020183204A1 (fr) 2019-03-14 2020-09-17 Pilkington Technology Management Limited Revêtement antimicrobien
US12459857B2 (en) 2019-03-14 2025-11-04 Pilkington Technology Management Limited Antimicrobial coating
WO2021260370A1 (fr) 2020-06-23 2021-12-30 Pilkington Group Limited Substrat antimicrobien
GB202011249D0 (en) 2020-07-21 2020-09-02 Pilkington Group Ltd Antimicrobial substrate
WO2022058734A1 (fr) 2020-09-16 2022-03-24 Pilkington Group Limited Revêtement antimicrobien et antiviral
WO2022090708A1 (fr) 2020-10-26 2022-05-05 Pilkington Group Limited Utilisation de substrats revêtus

Also Published As

Publication number Publication date
WO2009098655A3 (fr) 2009-12-03
ITTO20080098A1 (it) 2009-08-09

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