US20140030527A1 - Dissymmetric particles (janus particles), and method for synthesizing same by means of bipolar electrochemistry - Google Patents

Dissymmetric particles (janus particles), and method for synthesizing same by means of bipolar electrochemistry Download PDF

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Publication number
US20140030527A1
US20140030527A1 US13/996,783 US201113996783A US2014030527A1 US 20140030527 A1 US20140030527 A1 US 20140030527A1 US 201113996783 A US201113996783 A US 201113996783A US 2014030527 A1 US2014030527 A1 US 2014030527A1
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particles
substrates
electrodes
metal
electrolytic solution
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Gabriel Michel Pierre Loget
Alexander Kuhn
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Centre National de la Recherche Scientifique CNRS
Universite Sciences et Technologies Bordeaux 1
Institut Polytechnique de Bordeaux
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Universite Sciences et Technologies Bordeaux 1
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Assigned to CENTRE NATIONAL DE LA RECHERCHE SCIENTIFIQUE, INTSTITUT POLYTECHNIQUE DE BORDEAUX reassignment CENTRE NATIONAL DE LA RECHERCHE SCIENTIFIQUE ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: UNIVERSITE BORDEAUX 1
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D13/00—Electrophoretic coating characterised by the process
    • C25D13/12—Electrophoretic coating characterised by the process characterised by the article coated
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02—Making microcapsules or microballoons
    • B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/02—Electroplating of selected surface areas
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2991—Coated

Definitions

  • the present invention generally relates to dissymmetric particles, also called Janus particles of micron or submicron size, as well as a method of synthesis of such particles by bipolar electrochemistry.
  • Janus is a god with a head but with two opposite faces.
  • the term “Janus” qualifies any dissymmetric object, such as a spherical particle whereof the two hemispheres would be physically and/or chemically different.
  • Janus particles dissymmetric particles of micron or submicron size having two parts that are chemically different and/or have different polarities 1.2 . Due to these properties, these particles constitute a unique category of materials that have a growing interest to both the industry and the scientific community. In fact, such particles can be used in a large number of applications ranging from catalysis 3 fields to therapeutic treatments 4 . Until now, most of the techniques and methods used to generate such objects required to break the symmetry by introducing an interface 2,5,6,7 . However, this has the disadvantage of making the preparation of large quantities of particles rather difficult in as far as most techniques usually lead to equivalents of a monolayer of materials, since the particle modifications take place in a two-dimensional reaction space.
  • bipolar electrochemistry represents another attractive possibility of selectively modifying particles in a three-dimensional reaction medium.
  • This concept which was first described by Fleischmann et al. 11 in 1986, is based on the fact that when placing a conductive object in an electric field of high intensity between two electrodes, a polarization which is proportional to the electric field as well as to the characteristic dimensions of the object, appears. If the polarization is strong enough, the oxidation-reduction reactions can occur at the opposite ends of the object.
  • the potential difference V must be in first approximation at least equal to the difference between the formal potentials of the two oxidation-reduction pairs involved. For example, if one wishes to carry out dissymmetric functionalization with gold at the negatively charged ends by means of tetrachloroaurate, the following reaction must be carried out:
  • NHE being the normal hydrogen electrode serving as reference.
  • a purpose of embodiments of the present invention is to overcome all or part of the disadvantages of the prior art, by implementing a truly three-dimensional method exhibiting a high flexibility of use, which makes the formation of a broad range of Janus particles possible in terms of material, size, shape and nature of the modification.
  • the method developed by the applicants allows for the formation of Janus particles of micron or submicron size exhibiting an isotropic or anisotropic shape and whereof the modified part has a specific shape delimited by a precise outline.
  • embodiments of the present invention relate to Janus particles of micron or submicron size comprising an electrically conductive substrate exhibiting an at least chemically and/or physically modified part by deposit of a layer of electrochemically depositable material and an unmodified part.
  • these Janus particles are of isotropic shape, and the layer of electro-chemically depositable material has a specific shape delimited by a precise contour.
  • Janus particles may have one or several chemically and/or physically modified parts.
  • the Janus particles have two chemically and/or physically modified parts, which can be identical or different.
  • a particularly interesting configuration of the particles according to an embodiment of the invention can for example be the following: one of the parts is covered with a layer of a first electrochemically depositable material, and the other part is covered with a layer of a second electrochemically depositable material different from said first material.
  • a configuration two areas modified by covering with different materials
  • several alternatives are possible depending on the required application:
  • the first and second materials are electrically conductive materials
  • the first and second materials are insulating materials
  • the first material is an electrically conductive material and the second material is an insulating material.
  • electrically conductive materials that can be used within the framework of embodiments of the present invention, it can be particularly cited metals and semiconductors.
  • metals that can be used within the framework of embodiments of the present invention it can more particularly be cited gold, copper, zinc, silver, platinum and nickel.
  • the semiconductors that can be used within the framework of embodiments of the present invention, it can be more particularly cited ZnO, CdS, CdSe and Ti0 2 .
  • an insulating material that can be used within the framework of embodiments of the present invention, it may be particularly cited polymeric materials, organic molecules (particularly electrophoretic paint), silica-based sol-gel materials, metal oxides or metal salts.
  • polymeric material that can be used within the framework of embodiments of the present invention, one may particularly cite the polymers selected from the families of polypyrroles, polyanilines and polythiophenes.
  • the substrate of the Janus particles must necessarily be an electrically conductive substrate so that the polarization can take place when the substrate is placed in the electric field between two electrodes according to a method of the invention.
  • It may consist of a substrate in a conductive or semi-conductive material, for example beads of carbon or of a metal or a metal alloy.
  • Embodiments of the present invention also relate to an electrochemical method for the synthesis of Janus particles based on electrically conductive submicron or micron substrates, wherein it comprises the following steps:
  • the method according to embodiments of the invention is applicable to particulate substrates of isotropic shape (in particular beads), as well as to substrates of anisotropic shape (for example, nanotubes or disks).
  • the substrates are carbon or metal beads or nanotubes.
  • the separators are not permeable to the substrates and are placed in a same reactor of electrodeposition containing the electrolytic solution and the electrodes, by being arranged between said electrodes such as to define:
  • a cathodic compartment incorporating the electrode serving as cathode and adjacent to one of said separators, and
  • an anodic compartment incorporating the electrode serving as anode and adjacent to the other separator.
  • the separators while being non-permeable to substrates are still permeable to ions.
  • it can consist in membranes that are non-permeable to substrates as well to the source of electrodepositable material, or it can also consist in frit materials, which are impermeable to substrates, but let the material source through.
  • the electric field intensity will be of the order of 1 Kv/m to 1 MV/m, and its duration of application ranging between 10 seconds and 10 minutes, either continuously or intermittently and/or in an alternating manner.
  • the separators are in a sealing material.
  • it may consist in thin glass walls or in plastic material such as PLEXIGLAS®.
  • the intensity of the electric field will be of the order of 1 Kv/m to 1000 MV/m, and its application duration ranging between 10 seconds and several hours.
  • the source of electrochemically depositable material which is introduced into the cell can be selected from metal ions, metal salts (which form during the implementation of the method according to embodiments of the invention, first a hydroxide precipitating on the surface of the substrate to then be transformed into an oxide), the electro-polymerizable monomers, the organic electro-crystallizable salts, inorganic electro-crystallizable salts, organic electro-graftable molecules, electrophoretic paints and precursors of silica-based sol-gel materials.
  • electro-polymerizable monomers it may be particularly cited monomers derived from pyrrole, aniline and thiophene.
  • precursors of silica-based sol-gel materials it can also be cited precursors of alkoxysilane type which are selected from methyl trimethoxysilane (MTMS), tetraethoxysilane (TEOS), methyltriethoxylsilane (MTES) dimethyldiethoxysilane, and combinations thereof.
  • MTMS methyl trimethoxysilane
  • TEOS tetraethoxysilane
  • MTES methyltriethoxylsilane
  • metal ions By way of metal ions, it can be particularly cited metal ions of gold, copper, zinc, silver, platinum and nickel.
  • the shape of the layer of electrochemically depositable material is defined by acting on the concentration of the precursor filler and the electrodepositable material as well as on the applied electric field, as the shape of the layer depends on the competition between the direction of migration of the ions and the kinetics of electrodeposition, which substantially depends on the concentration of the precursor and the field applied.
  • the electrolytic solution implemented in the method according to the invention may be an aqueous solution or a non-aqueous solvent solution, for example toluene, acetonitrile, or combinations thereof.
  • the electrolytic solution has a viscosity that is sufficient to prevent or inhibit the particle from rotating.
  • the electrolyte solution is gelled.
  • the substrates are of anisotropic shape, it is not necessary to increase the viscosity, but the viscosity can be increased to ensure that the deposit has a specific shape.
  • embodiments of the present invention also relate to a device for implementing the method according to embodiments of the invention, wherein the device comprises an electrodeposition cell containing the electrolytic solution, said cell being bounded by separators into a sealed material outside which electrodes are arranged in a contiguous manner.
  • FIG. 1 represents a block diagram of the bipolar electrodeposition used to form Janus particles
  • FIG. 2 represents a block diagram of an example of electrodeposition cell for implementing the method according to a first embodiment
  • FIG. 3 represents a block diagram f an electrodeposition device for implementing the method according to a second embodiment
  • FIG. 4 schematically represents a Janus particle according to the invention, of isotropic shape (in this instance a bead), which has two modified areas.
  • FIGS. 5A to 5C correspond to three images of scanning electron microscopy (SEM) of three examples of Janus particles (carbon beads) according to embodiments of the invention of isotropic shape,
  • FIG. 6 shows:
  • FIG. 7 shows two images A and B of scanning electron microscopy (SEM) of substrates of submicron size and of isotropic shape, before (image A) and after bipolar electrodeposition (image B), the modified part corresponding to the small white dot;
  • SEM scanning electron microscopy
  • FIG. 8 shows four images (a, b, c, d) of optical microscopy in transmission of bi-functionalized copper/copper carbon tubes, by means of the method according to an embodiment of the invention by imposing voltage pulses;
  • FIG. 9 a shows an image of scanning electron microscopy (SEM) of a bi-functionalized copper/copper carbon tube by means of the process according to an embodiment of the invention
  • FIG. 9 b shows an image of scanning electron microscopy (SEM) of a bi-functionalized copper/polypyrrole carbon tube by means of the method according to the invention
  • FIG. 10 shows an image of scanning electron microscopy (SEM) of a single crystal localized deposit of a platinum salt (white part on FIG. 10 ) on a carbon bead by bipolar electrochemistry in accordance with the method according to an embodiment of the invention.
  • SEM scanning electron microscopy
  • FIGS. 2 to 9 are identical elements represented on FIGS. 2 to 9 are identified by identical numerical references.
  • FIG. 1 which is discussed in the description of the prior art, represents a block diagram of an example of a device for implementing the method according to a first embodiment of the invention. This figure particularly shows that sufficient polarization of a conductive particle makes it possible to break the symmetry.
  • FIGS. 2 and 3 represent block diagrams of an electrodeposition device for implementing the method according to embodiments of the invention, each corresponding to a different embodiment. These figures show that the electrodeposition device comprises an electrodeposition cell 3 , defined by two separators 31 , 32 , and is arranged between two electrodes 21 , 22 .
  • the operating principle for the two embodiments of the electrodeposition device comprises the following steps:
  • FIG. 3 more particularly represents an electrodeposition device 3 , which comprises an electrodeposition reactor 5 containing the electrolytic solution 40 , the electrodes 21 and 22 which are immersed into the electrolytic solution, and the separators 31 , 32 which consist of membranes or plates which are non-permeable to the substrates. These membranes 31 , 32 are arranged between the electrodes 21 , 22 such as to define:
  • FIG. 4 more particularly represents an electrodeposition device 3 wherein the separators 31 , 32 are in watertight material (glass or PLEXIGLAS®). They delimit the electrodeposition cell 3 containing the electrolytic solution 40 and outside which 3 the electrodes 21 , 22 are contiguously arranged.
  • the separators 31 , 32 are in watertight material (glass or PLEXIGLAS®). They delimit the electrodeposition cell 3 containing the electrolytic solution 40 and outside which 3 the electrodes 21 , 22 are contiguously arranged.
  • the substrates 1 used are either carbon tubes (images 6 A 1 , 6 A 2 and 6 A 3 ) or vitreous carbon beads (images 6 B 1 , 6 B 2 and 6 B 3 ),
  • the electrolytic solutions 40 are aqueous solutions which, as a source of electrodepositable material, contain the following metal salts:
  • the electrolytic solution 40 is a hydrogel agar.
  • FIGS. 8 a to 8 d the visible scale (black lines) is of 20 m.
  • FIGS. 8 a (with a pulse interval of 5 minutes) and 8 b (with a pulse interval of 10 s) correspond to a pulse of 12 s
  • FIGS. 8 c (with a pulse interval of 5 minutes) and 8 d (with a pulse interval of 10 s) correspond to a pulse of 30 s.
  • the obtained particles were also observed with a scanning electron microscope (SEM) ( FIG. 9 a ).

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Engineering & Computer Science (AREA)
  • Dispersion Chemistry (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
US13/996,783 2010-12-22 2011-12-15 Dissymmetric particles (janus particles), and method for synthesizing same by means of bipolar electrochemistry Abandoned US20140030527A1 (en)

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FR1061031 2010-12-22
FR1061031A FR2969508B1 (fr) 2010-12-22 2010-12-22 Particules dissymetriques (particules de janus) et leur procede de synthese par electrochimie bipolaire.
PCT/FR2011/053001 WO2012085399A1 (fr) 2010-12-22 2011-12-15 Particules dissymetriques (particules de janus) et leur procede de synthese par electrochimie bipolaire

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CN103846067A (zh) * 2014-03-19 2014-06-11 中国科学技术大学 一种粒径和形貌均可控的磁性异性Janus微球及其制备方法和所用的微流体控制装置
CN103846068A (zh) * 2014-03-19 2014-06-11 中国科学技术大学 一种粒径和形貌可控的单分散极性异性Janus微球及其制备方法和所用的微流体控制装置
CN103920434A (zh) * 2014-04-21 2014-07-16 中国科学技术大学 一种粒径与形貌可控的具有电荷与光学异性特征的炭黑/聚四氟乙烯Janus微球及其制备方法
CN105420761A (zh) * 2015-11-05 2016-03-23 上海应用技术学院 一种在氧化铝模板上自还原制备多种金属Janus颗粒的方法
WO2018014052A1 (en) * 2016-07-11 2018-01-18 Csir Composite activated carbon and conductive polymer adsorption media
CN107987279A (zh) * 2017-11-29 2018-05-04 湘潭大学 利用离子液体双极性电化学合成花瓣状金属有机框架物ZIF-8的Janus微球的方法
CN108822302A (zh) * 2018-06-20 2018-11-16 同济大学 一种Janus纳米颗粒及其制备方法与应用
US10221288B1 (en) 2017-08-08 2019-03-05 International Business Machines Corporation Matrix bonding abrasion resistant CNTs (MBARCs) and employing same in fiber reinforced polymer composites
US10670964B2 (en) 2017-11-21 2020-06-02 International Business Machines Corporation Ruggedized solder mask material
US10745821B2 (en) 2010-12-22 2020-08-18 Universite de Bordeaux Dissymetric particles (Janus particles) and their method of synthesis by bipolar electrochemistry
CN111663167A (zh) * 2020-06-16 2020-09-15 合肥工业大学 一种基于bpe技术的金属线制备方法

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CN105414541B (zh) * 2015-11-26 2017-07-28 哈尔滨工业大学 一种双金属Janus结构纳米粒子的制备方法
CN108530582B (zh) * 2017-03-03 2019-08-09 中国科学院化学研究所 多组分的Janus复合纳米材料及其制备方法
CN112805083B (zh) * 2018-08-02 2024-01-05 南洋理工大学 通过两相界面组装的janus颗粒制备
CN110449150B (zh) * 2019-07-04 2020-11-06 中山大学 一种内嵌纳米金属的中空炭管阵列催化剂及其制备方法和应用
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Cited By (13)

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US10745821B2 (en) 2010-12-22 2020-08-18 Universite de Bordeaux Dissymetric particles (Janus particles) and their method of synthesis by bipolar electrochemistry
CN103846068A (zh) * 2014-03-19 2014-06-11 中国科学技术大学 一种粒径和形貌可控的单分散极性异性Janus微球及其制备方法和所用的微流体控制装置
CN103846067A (zh) * 2014-03-19 2014-06-11 中国科学技术大学 一种粒径和形貌均可控的磁性异性Janus微球及其制备方法和所用的微流体控制装置
CN103920434A (zh) * 2014-04-21 2014-07-16 中国科学技术大学 一种粒径与形貌可控的具有电荷与光学异性特征的炭黑/聚四氟乙烯Janus微球及其制备方法
CN105420761A (zh) * 2015-11-05 2016-03-23 上海应用技术学院 一种在氧化铝模板上自还原制备多种金属Janus颗粒的方法
WO2018014052A1 (en) * 2016-07-11 2018-01-18 Csir Composite activated carbon and conductive polymer adsorption media
US10221288B1 (en) 2017-08-08 2019-03-05 International Business Machines Corporation Matrix bonding abrasion resistant CNTs (MBARCs) and employing same in fiber reinforced polymer composites
US10739679B2 (en) 2017-11-21 2020-08-11 International Business Machines Corporation Ruggedized solder mask material
US10670964B2 (en) 2017-11-21 2020-06-02 International Business Machines Corporation Ruggedized solder mask material
CN107987279A (zh) * 2017-11-29 2018-05-04 湘潭大学 利用离子液体双极性电化学合成花瓣状金属有机框架物ZIF-8的Janus微球的方法
CN108822302A (zh) * 2018-06-20 2018-11-16 同济大学 一种Janus纳米颗粒及其制备方法与应用
CN108822302B (zh) * 2018-06-20 2020-08-14 同济大学 一种Janus纳米颗粒及其制备方法与应用
CN111663167A (zh) * 2020-06-16 2020-09-15 合肥工业大学 一种基于bpe技术的金属线制备方法

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FR2969508A1 (fr) 2012-06-29
EP2663394B1 (fr) 2020-02-05
JP6063390B2 (ja) 2017-01-18
CA2822779C (fr) 2020-06-30
WO2012085399A1 (fr) 2012-06-28
US20170130356A1 (en) 2017-05-11
US10745821B2 (en) 2020-08-18
EP2663394A1 (fr) 2013-11-20

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