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EP4559596A1 - Procédé laser de fabrication de nanoparticules magnétoplasmoniques - Google Patents

Procédé laser de fabrication de nanoparticules magnétoplasmoniques Download PDF

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Publication number
EP4559596A1
EP4559596A1 EP23212167.3A EP23212167A EP4559596A1 EP 4559596 A1 EP4559596 A1 EP 4559596A1 EP 23212167 A EP23212167 A EP 23212167A EP 4559596 A1 EP4559596 A1 EP 4559596A1
Authority
EP
European Patent Office
Prior art keywords
thin metal
metal film
metal
sample
thin
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.)
Pending
Application number
EP23212167.3A
Other languages
German (de)
English (en)
Inventor
Evaldas Stankevicius
Vita Petrikaite
Gediminas Niaura
Valdas Sablinskas
Justinas Ceponkus
Ieva Matulaitiene
Romualdas Trusovas
Lina Mikoliunaite
Martynas Talaikis
Agne Zdaniauskiene
Sonata Adomaviciute-Grabusove
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.)
Vilniaus Universitetas
Valstybinis Moksliniu Tyrimu Institutas Fiziniu ir Technologijos Mokslu Centras
Original Assignee
Vilniaus Universitetas
Valstybinis Moksliniu Tyrimu Institutas Fiziniu ir Technologijos Mokslu Centras
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 Vilniaus Universitetas, Valstybinis Moksliniu Tyrimu Institutas Fiziniu ir Technologijos Mokslu Centras filed Critical Vilniaus Universitetas
Priority to EP23212167.3A priority Critical patent/EP4559596A1/fr
Publication of EP4559596A1 publication Critical patent/EP4559596A1/fr
Pending legal-status Critical Current

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/14Making metallic powder or suspensions thereof using physical processes using electric discharge
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/17Metallic particles coated with metal
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/0466Alloys based on noble metals

Definitions

  • the invention relates to a method of producing magneto-plasmonic particles by laser irradiation.
  • Magneto-plasmonic nanoparticles can be generated using chemical synthesis, microemulsion synthesis, sonochemical synthesis, physical vapor deposition and hybridization of pre-synthesized nanoparticles.
  • Main disadvantages of known methods are toxicity of the chemical precursors, time-consuming of the process, low efficiency of large-scale production, high cost and impurity of production, expensive vacuum required equipment, etc.
  • Our proposed laser-based method solves these problems: the laser-based process does not use toxic chemical precursors. High efficiency and purity of the production can be ensured using non-vacuum equipment with inexpensive laser systems.
  • magneto-plasmonic particles with laser irradiation often lacks flexibility by precisely controlling the formed nanoparticle composition, which may vary depending on the specific application.
  • US patent application No. US11/092,717 (publication No. US2006/0057384A1 ) describes how to coat gold nanoparticles with a magnetic shell using laser ablation. Gold and iron colloidal nanoparticles are mixed and then irradiated with a laser beam. Main disadvantage is that process comprises multiple steps for obtaining magneto plasmonic nanoparticles.
  • US patent No. US7,029,514 describes synthesis of core-shell nanoparticles using a chemical synthesis of nanoparticles from metal salts.
  • Main disadvantage is that process comprises using chemical synthesis comprising use of chemical substances such as salts, resulting in bimetal nanoparticles with additives and necessity for additional cleaning process of the nanoparticle.
  • the present invention is dedicated to overcoming of the above shortcomings and for producing further advantages over prior art.
  • the invention relates to a method for producing magneto-plasmonic particles by laser ablation.
  • the method uses two metallic samples each being a distinct metal sample one from another and simultaneously placed opposite each other in a liquid medium.
  • First metallic sample which is a thin metal film, has magnetic or plasmonic properties, and the other metallic sample accordingly has plasmonic or magnetic properties.
  • both metallic samples are thin metal films, they are deposited on ultra-thin glass substrates as coating.
  • the first metallic sample is a thin metal film
  • the second sample is bulk metal.
  • the metallic samples are arranged in front of each other at a certain distance in the liquid medium.
  • plasma is induced in the thin metallic coatings.
  • bulk metal is used as the second metallic sample, plasma is induced on the surface layer of the bulk metal sample.
  • the produced magneto-plasmonic nanoparticles depend on distance between the coatings, thickness of the used coatings, focusing conditions of the laser beam, and energy and duration of the laser pulses.
  • the produced magneto-plasmonic nanoparticles can be used in cancer diagnosis and treatment by using surface-enhanced Raman spectroscopy and other methods.
  • first (106) and second (108, 108') metal targets differ in type of metal.
  • Each of the two thin metal films (106, 108) are deposited on a glass substrate (105, 109) and placed opposite each other in a liquid medium (104).
  • First thin metal film (106) has magnetic properties, i.e. a magnetic response to magnetic fields
  • the second thin metal film (108) has plasmonic properties, i.e. surface plasmon resonance, enhancement of electromagnetic field.
  • the first thin metal film (106) can have plasmonic properties and the second thin metal film (108) accordingly will have magnetic properties.
  • Distance between the thin metal films (106, 108) is controlled by varying thicknesses of spacers (107).
  • the arranged substrates (105, 109) coated with metallic thin films (106, 108) are irradiated by a laser beam (102) focused using a lens (101) through a glass window in a cuvette (103).
  • the composition of the generated nanoparticles is controlled by varying thicknesses of the thin metal film (106, 108), spacing between them, the laser beam (102) focusing conditions, laser beam (102) pulse energy, duration and scanning speed. All these parameters influence the temperature and dynamics of plasma from both targets (106, 108), leading to the different degree of plasma mixing and the formation of different kind of hybrid nanoparticles.
  • the top target, first thin metal film (106), is positioned so the substrate (105) faces the laser beam (102).
  • the laser beam (102) passes the transparent substrate (105) and ablation of the first thin metal film (106) occurs.
  • the laser beam (102) passes gap between the first thin metal film (106) and the second thin metal film (108) and starts ablation of the second thin metal film (108).
  • the targets (106, 108) can be interchanged by placing the magnetic thin metal film on top as the first thin metal film (106) and the plasmonic thin metal film at the bottom as the second thin metal film (108) and vice versa.
  • the first thin metal film (106) and the second thin metal film (108) may be interchanged at any point during the ablation process, for example in the middle of the ablation process.
  • Both thin films (106, 108) are placed in a liquid medium, such as water, acetone, isopropanol, etc. Both thin metal films (106, 108) are placed facing each other perpendicular to the laser beam (102) at a distance, for example of 1 to 500 ⁇ m, which can be adjusted using spacers (107) or a precise translation stage.
  • the ablation process is performed by scanning a laser beam (102) or moving the whole setup with a stationary laser beam (102).
  • one thin metal film (106) on a transparent glass substrate (105) and a bulk metal sample are placed opposite each other in a liquid medium (104).
  • First thin metal film (106) has magnetic properties, i.e.
  • the bulk metal sample (108') has plasmonic properties, i.e. surface plasmon resonance, enhancement of electromagnetic field.
  • the first thin metal film (106) can have plasmonic properties and the bulk metal sample (108') accordingly will have magnetic properties.
  • Distance between the thin metal film (106) and the bulk metal sample (108') is controlled by varying thicknesses of spacers (107).
  • the arranged substrate (105) coated with thin metal film (106) and surface layer of the bulk metal sample (108') are irradiated by a laser beam (102) focused using a lens (101) through a glass window in a cuvette (103).
  • the composition of the generated nanoparticles is controlled by varying thicknesses of the thin metal film (106), spacing between thin metal film (106) and the bulk metal sample (108'), the laser beam (102) focusing conditions, the laser beam (102) pulse energy, duration and scanning speed. All these parameters influence the temperature and dynamics of plasma from both targets (106, 108'), leading to the different degree of plasma mixing and the formation of different kinds of hybrid nanoparticles.
  • the first thin metal film (106) on an ultrathin transparent substrate (105) and bulk metal sample (108') are used as laser beam (102) targets, as shown in Fig. 2 , the top target, the first thin metal film (106), is positioned so the substrate (105) faces the laser beam (102).
  • the laser beam (102) passes the transparent substrate (105) ablation of the first thin metal film (106) occurs. Afterwards, the laser beam (102) passes the gap between the first thin metal film (106) and the bulk metal sample (108') and starts ablating the second target which is the bulk metal sample (108').
  • the bottom target must be bulk and the top target only a thin metal film (106) on an ultrathin transparent substrate (105).
  • Both the first thin metal film (106) and the bulk metal sample (108') are placed in a liquid medium, such as water, acetone, isopropanol, etc. Both (106, 108') are placed facing each other perpendicular to the laser beam (102) at a distance, for example of 1 to 500 ⁇ m, which can be adjusted using spacers (107) or a precise translation stage.
  • a liquid medium such as water, acetone, isopropanol, etc.
  • Both (106, 108') are placed facing each other perpendicular to the laser beam (102) at a distance, for example of 1 to 500 ⁇ m, which can be adjusted using spacers (107) or a precise translation stage.
  • plasma is induced in the thin metallic films (106, 108) or the thin metallic film (106) and the bulk metal sample (108') when the target (106, 108') are exposed to the laser beam (102).
  • the targets (106, 108, 108') emit plasma at temperatures ranging from 1000 to 10000 K and expand during the process.
  • plasma in both cases from both targets (106, 108, 108') interacts together, the shockwave is created that travels through the plasma and mixes the ablated material from both targets (106, 108, 108').
  • Plasma cooling leads to the recombination of ions and electrons to form hybrid nanoparticles, which exhibit magneto-plasmonic properties in a solution.
  • the obtained hybrid magneto-plasmonic nanoparticles can be applied in medicine, for example, in cancer diagnosis and treatment by using surface enhanced Raman spectroscopy and other methods.
  • the ablation targets thin metallic films (106, 108) of thickness from 1 nm to 1 ⁇ m deposited on ultrathin, up to 150 ⁇ m, transparent substrate for applied laser radiation material substrate (105, 109) or targets a thin metal film (106) of thickness from 1 nm to 1 ⁇ m deposited on ultrathin, up to 150 ⁇ m, transparent substrate and the bulk metal target (108').
  • Each thin film (106, 108) comprises of one metal or a few different metals. For example, gold and silver films are deposited on separate areas of one substrate or mixed using periodic patterns through the surface for depositing on one substrate.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
EP23212167.3A 2023-11-27 2023-11-27 Procédé laser de fabrication de nanoparticules magnétoplasmoniques Pending EP4559596A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP23212167.3A EP4559596A1 (fr) 2023-11-27 2023-11-27 Procédé laser de fabrication de nanoparticules magnétoplasmoniques

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP23212167.3A EP4559596A1 (fr) 2023-11-27 2023-11-27 Procédé laser de fabrication de nanoparticules magnétoplasmoniques

Publications (1)

Publication Number Publication Date
EP4559596A1 true EP4559596A1 (fr) 2025-05-28

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060057384A1 (en) 2004-04-01 2006-03-16 Benoit Simard Methods for the fabrication of gold-covered magnetic nanoparticles
US7029514B1 (en) 2003-03-17 2006-04-18 University Of Rochester Core-shell magnetic nanoparticles and nanocomposite materials formed therefrom
US20140322138A1 (en) 2013-04-29 2014-10-30 Yuki Ichikawa Method of reliable particle size control for preparing aqueous suspension of precious metal nanoparticles and the precious metal nanoparticle suspension prepared by the method thereof
US9271706B2 (en) 2008-08-12 2016-03-01 Covidien Lp Medical device for wound closure and method of use
US20190334180A1 (en) 2016-04-19 2019-10-31 Dibyendu Mukherjee Compositions, systems and methods for producing nanoalloys and/or nanocomposites using tandem laser ablation synthesis in solution-galvanic replacement reaction
WO2023198617A2 (fr) * 2022-04-11 2023-10-19 Basf Se Nanoparticules de métal de transition en alliage multimétallique et leurs procédés de production

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7029514B1 (en) 2003-03-17 2006-04-18 University Of Rochester Core-shell magnetic nanoparticles and nanocomposite materials formed therefrom
US20060057384A1 (en) 2004-04-01 2006-03-16 Benoit Simard Methods for the fabrication of gold-covered magnetic nanoparticles
US9271706B2 (en) 2008-08-12 2016-03-01 Covidien Lp Medical device for wound closure and method of use
US20140322138A1 (en) 2013-04-29 2014-10-30 Yuki Ichikawa Method of reliable particle size control for preparing aqueous suspension of precious metal nanoparticles and the precious metal nanoparticle suspension prepared by the method thereof
US20190334180A1 (en) 2016-04-19 2019-10-31 Dibyendu Mukherjee Compositions, systems and methods for producing nanoalloys and/or nanocomposites using tandem laser ablation synthesis in solution-galvanic replacement reaction
WO2023198617A2 (fr) * 2022-04-11 2023-10-19 Basf Se Nanoparticules de métal de transition en alliage multimétallique et leurs procédés de production

Non-Patent Citations (6)

* Cited by examiner, † Cited by third party
Title
AMENDOLA VINCENZO ET AL: "Formation of alloy nanoparticles by laser ablation of Au/Fe multilayer films in liquid environment", JOURNAL OF COLLOID AND INTERFACE SCIENCE, ACADEMIC PRESS,INC, US, vol. 489, 13 October 2016 (2016-10-13), pages 18 - 27, XP029857354, ISSN: 0021-9797, DOI: 10.1016/J.JCIS.2016.10.023 *
C. GELLINIF.L. DEEPAKM. MUNIZ-MIRANDAS. CAPORALIF. MUNIZ-MIRANDAA. PEDONEC. INNOCENTIC. SANGREGORIO: "Magneto-plasmonic colloidal nanoparticles obtained by laser ablation of nickel and silver targets in water", J. PHYS. CHEM. C, vol. 121, 2017, pages 3597 - 3606
M. MUNIZ-MIRANDAF. MUNIZ-MIRANDAE. GIORGETTI: "Spectroscopic and microscopic analyses of Fe3O4/Au nanoparticles obtained by laser ablation in water", NANOMATERIALS, vol. 10, 2020, pages 132
SABLINSKAS VALDAS ET AL: "Magneto-plasmonic nanoparticles for SERS", PROCEEDINGS OF THE SPIE, SPIE, US, vol. 11797, 6 August 2021 (2021-08-06), pages 117972B - 117972B, XP060145100, ISSN: 0277-786X, ISBN: 978-1-5106-5738-0, DOI: 10.1117/12.2597199 *
SUBHAN ABDUL ET AL: "Pulsed Laser Synthesis of Bi-Metallic Nanoparticles for Biomedical Applications: A Review", 2022 ADVANCES IN SCIENCE AND ENGINEERING TECHNOLOGY INTERNATIONAL CONFERENCES (ASET), IEEE, 21 February 2022 (2022-02-21), pages 1 - 7, XP034103639, DOI: 10.1109/ASET53988.2022.9735057 *
V. AMENDOLAS. SCARAMUZZAF. CARRAROE. CATTARUZZA: "Formation of alloy nanoparticles by laser ablation of Au/Fe multilayer films in liquid environment", J. COLLOID INTERFACE SCI, vol. 489, 2017, pages 18 - 27, XP029857354, DOI: 10.1016/j.jcis.2016.10.023

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