WO1996007487A1 - Procede de synthese de materiaux aux proprietes electroniques, magnetiques et/ou optiques regulees - Google Patents

Procede de synthese de materiaux aux proprietes electroniques, magnetiques et/ou optiques regulees Download PDF

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WO1996007487A1
WO1996007487A1 PCT/GB1995/002124 GB9502124W WO9607487A1 WO 1996007487 A1 WO1996007487 A1 WO 1996007487A1 GB 9502124 W GB9502124 W GB 9502124W WO 9607487 A1 WO9607487 A1 WO 9607487A1
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particles
metal
solution
dispersion
semi
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PCT/GB1995/002124
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Donald Bethell
David Jorge Schiffrin
Mathias Brust
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The University Of Liverpool
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • B05D1/18—Processes for applying liquids or other fluent materials performed by dipping
    • B05D1/185—Processes for applying liquids or other fluent materials performed by dipping applying monomolecular layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y10/00—Nanotechnology for information processing, storage or transmission, e.g. quantum computing or single electron logic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y25/00—Nanomagnetism, e.g. magnetoimpedance, anisotropic magnetoresistance, giant magnetoresistance or tunneling magnetoresistance
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL 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
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K9/00—Tenebrescent materials, i.e. materials for which the range of wavelengths for energy absorption is changed as a result of excitation by some form of energy
    • C09K9/02—Organic tenebrescent materials
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/015—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on semiconductor elements having potential barriers, e.g. having a PN or PIN junction
    • G02F1/017—Structures with periodic or quasi periodic potential variation, e.g. superlattices, quantum wells
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/14—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates
    • H01F41/30—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates for applying nanostructures, e.g. by molecular beam epitaxy [MBE]
    • H01F41/301—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for applying magnetic films to substrates for applying nanostructures, e.g. by molecular beam epitaxy [MBE] for applying ultrathin or granular layers
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
    • H10K30/30—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising bulk heterojunctions, e.g. interpenetrating networks of donor and acceptor material domains
    • H10K30/35—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising bulk heterojunctions, e.g. interpenetrating networks of donor and acceptor material domains comprising inorganic nanostructures, e.g. CdSe nanoparticles
    • H10K30/352—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising bulk heterojunctions, e.g. interpenetrating networks of donor and acceptor material domains comprising inorganic nanostructures, e.g. CdSe nanoparticles the inorganic nanostructures being nanotubes or nanowires, e.g. CdTe nanotubes in P3HT polymer
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/701—Langmuir Blodgett films
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL 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
    • C03C2217/00—Coatings on glass
    • C03C2217/40—Coatings comprising at least one inhomogeneous layer
    • C03C2217/42—Coatings comprising at least one inhomogeneous layer consisting of particles only
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
    • H10K30/50—Photovoltaic [PV] devices
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/30—Coordination compounds
    • H10K85/331—Metal complexes comprising an iron-series metal, e.g. Fe, Co, Ni
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/60—Organic compounds having low molecular weight
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/60—Organic compounds having low molecular weight
    • H10K85/615—Polycyclic condensed aromatic hydrocarbons, e.g. anthracene
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/60—Organic compounds having low molecular weight
    • H10K85/649—Aromatic compounds comprising a hetero atom
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/549—Organic PV cells

Definitions

  • the present invention relates to solutions or
  • the method of the invention makes it possible to produce synthesised materials with controlled electronic, magnetic and/or optical properties on the nanometre scale.
  • a first aspect of the invention concerns the
  • a gas phase can only be utilized if the polyfunctional linker molecule is short and volatile. This is of importance in the production of thin films.
  • a second aspect of the invention provides methods for linking the small particles in a
  • small metal or semi-conductor particles e.g. colloids, whose typical diameter range is from 10-500 nm, and clusters, whose typical size range is from 0.5 to 10 nm (particles of size 0.5 to
  • Solutions or dispersions of metal particles are of course known. However the solutions or dispersions of the art are either too stable that they can not be reacted or are so reactive that the metal particles coalesce and finally precipitate out. Typical solutions or dispersions include
  • hydrosols and ligand stabilised colloids or clusters hydrosols and ligand stabilised colloids or clusters.
  • AuCl 4 - was transferred from aqueous solution to toluene using tetraoctylammonium bromide as a phase transfer reagent and reduced with aqueous sodium borohydride in the presence of a stabilising agent dodecanethiol
  • nanodimensions can be produced which is stable yet can be reacted with linker molecules to enable materials to be synthesised in a controlled manner by using an electron solvent donor i.e. a solvent capable of electron donation, for example aromatic compounds or ethers in the presence a phase transfer reagent.
  • an electron solvent donor i.e. a solvent capable of electron donation, for example aromatic compounds or ethers in the presence a phase transfer reagent.
  • the particles For example, for aromatic compounds the particles would interact with the ⁇ electron system and for ethers with the non bonded electrons.
  • aromatic solvent is used here to benzophenyl
  • heterocyclic compounds which can donate ⁇ electrons.
  • a solution or dispersion consisting essentially of metal particles of nanometre dimensions dissolved or dispersed in an electron donor solvent.
  • phase transfer reagent is selected according to the specification of the aqueous metal ion and for an anion is preferably a hydrophobic quaternary ammonium, phosphonium or arsonium ion.
  • the electron donor is an aromatic solvent for example toluene, although other solvents capable of donating ⁇ electrons such as, for example, benzene, anisole, methylnaphthalene, aniline, xylene and mixtures of the above with polycyclic aromatic compounds such as m-terphenyl, naphthalene and phenanthrene may be used.
  • aromatic solvent for example toluene
  • other solvents capable of donating ⁇ electrons such as, for example, benzene, anisole, methylnaphthalene, aniline, xylene and mixtures of the above with polycyclic aromatic compounds such as m-terphenyl, naphthalene and phenanthrene may be used.
  • hydrophobic quaternary ammonium, phosphonium or arsonium ions may, for example, be the tetraoctyl ammonium ion [N(C 8 H 17 ) 4 ] + .
  • substituted ammonium, phosphonium or arsonium ions could be used, preferably C 5 to C 10 alkyl substituted quaternary ions.
  • a method of producing a solution or dispersion of metal particles of nanometre dimensions comprising
  • linker molecules not only determine the potential energy barriers between particle centres but also control the symmetry of the structure of the resultant material. This enables the materials to be synthesised with properties which can be precisely controlled by the chemical nature of the linker molecules.
  • the new approach taken is to use polyfunctional linker molecules to link small particles of 0.5 to 500 nm or to attach them to a substrate to yield two- dimensional or three-dimensional structures.
  • a two step method of producing a bulk material which comprises
  • this is achieved by firstly preparing a solution or dispersion of metal particles, for example gold, in an aromatic solvent, for example toluene, in the presence of hydrophobic quartenary ammonium, phosphonium or arsonium ions, for example a tetraoctylammonium ion and subsequently reacting said solution or dispersion with a polyfunctional linker molecule, for example 1,9 nonanedithiol.
  • metal particles for example gold
  • an aromatic solvent for example toluene
  • hydrophobic quartenary ammonium, phosphonium or arsonium ions for example a tetraoctylammonium ion
  • this may be achieved by firstly preparing a solution or dispersion of semiconductor particles and subsequently reacting said solution or dispersion with a polyfunctional linker molecule, for example a silane.
  • a polyfunctional linker molecule for example a silane.
  • TiO 2 colloids can be prepared by controlled hydrolysis of titanium alkoxides in the water pools of reverse micellar systems.
  • indium/tin oxide a high temperature approach is followed, by the controlled hydrolysis of suitable indium and tin compounds in high temperature solvents, such as, for example m-terphenyl.
  • the polyfunctional linker molecule is dissolved or dispersed in the same solvent as the metal or semi conductor particle.
  • a one step method of producing a bulk material of particles of nanometre dimensions comprising preparing a solution or
  • this is achieved by preparing a solution or dispersion of metal particles, for example gold, in an organic electron donor solvent, for example diethyl ether in the presence of a linker molecule, for example 1,9 nonanedithiol.
  • an organic electron donor solvent for example diethyl ether
  • a linker molecule for example 1,9 nonanedithiol.
  • the linker molecule in this embodiment also acts as a stabilising ligand, preventing coalescence of particles. It is not therefore essential to include hydrophobic quartenary ammonium, phosphonium or arsonium ions.
  • this may be achieved by preparing a solution or dispersion of a semi-conductor material in the presence of a linker molecule, for example a silane.
  • a linker molecule for example a silane.
  • a method of producing a thin film structure from particles of nanometre dimensions comprising forming at least one layer of metal or semi conductor particles onto a substrate by treating the substrate with a
  • polyfunctional linker molecule so that a first reactive group of the polyfunctional linker molecule reacts with the substrate linking it thereto and subsequently treating the functionalised substrate with a solution of the metal or semi conductor particles so that a second reactive group of the polyfunctional linker molecule reacts with the metal or semi conductor particles linking it thereto.
  • the step of treating the substrate may be by treating it with a solution of linker molecules, so as to react the linker molecules, or by direct reaction such as for example by reacting the linker molecules in the gas phase.
  • the process can be repeated to build on top of the first layer of metal or semi-conductor particles a plurality of layers of the same or different metal or semi-conductor particles and/or linkers.
  • one or more further layers of metal or semi-conductor particles may be formed onto an already formed layer of metal or semi-conductor particles by treating the already formed layer of metal or semiconductor particles with the same or a different polyfunctional linker molecule so that the same or a different polyfunctional linker molecule reacts with the already formed layer of metal or semi-conductor particles linking the same or different polyfunctional linker molecule thereto to form a functionalised layer of metal or semi-conductor particles and subsequently treating the functionalised layer of metal or semiconductor particles with a solution of the same or different metal or semi-conductor particles to react the second reactive group of the same or different polyfunctional linker molecule with the same or different metal or semi-conductor particles.
  • the polyfunctional linker molecule is dissolved in the same solvent as the metal or semi conductor particles although this is not essential.
  • the substrate is treated by first subjecting it to the linker molecule. This is
  • linker molecule preferably done by immersing it in a solution of the linker molecule although for volatile linker molecules adsorption from the gas phase could be used.
  • the particles can be metal or semi conductor particles so long as they can be generated in solution or dispersion as colloids or clusters.
  • the preferred particles are the coin metals such as, for example, gold, silver and copper, the
  • the metal particles need not be elemental
  • the semiconductor particles include silicon, and arsenides, oxides and chalcogenides or any other materials which show semi-conductor properties and which can be made into particles of nanometre dimensions.
  • the preferred polyfunctional linker molecules comprise a hydrocarbon skeleton with at least two functional groups (which groups may be the same or different) capable of binding to other particles or a substrate.
  • They may be electronically neutral or carry a charge.
  • thiocarbonyl compounds such as thiourea and other thioamides and corresponding groups where heavier group VI elements such as selenium and tellurium replace sulphur;
  • the hydrocarbon skeleton can be a linear or branched aliphatic chain which may contain cyclic moieties, carbon multiple bonds and/or other TT- systems.
  • These additional i ⁇ -systems could be mono- or poly-cyclic aromatic hydrocarbon units including fullerenes (with or without electron donating or electron withdrawing substituents), heterocycles, quinones or metallocene units and embrace chromophoric and ionophoric groups and units capable of acting as redox centres.
  • X a functional group and where more than one X is denoted this may be the same or
  • n an integer preferably from 0 to 20
  • the carbon skeletons shown in I, II and III are illustrative of the type of structures and the number of carbon atoms in the chain could vary and is
  • a thin film structure comprising a substrate and at least one layer of particles of nanometre dimensions linked thereto by linker molecules.
  • the particles can be colloids or clusters of metals or semi conductors.
  • the linker molecule can be any organic molecule with at least two functional groups which groups will react with a substrate and a particle or with two particles. Where the particles are metal particles, such as for example, gold or silver or semi conductor
  • the preferred linkers will be polythiols including dithiols or the corresponding groups where heavier group VI elements such as selenium and tellurium replace sulphur.
  • the preferred linkers will include silanes as functional groups.
  • the resulting material can become part of a growing structure.
  • the growth rate or degree of attachment can be controlled by the type of linker molecule. It is also possible to attach other compounds to the linker molecules.
  • the electronic, magnetic and/or optical signals are the electronic, magnetic and/or optical signals.
  • a quantum dot, quantum wire or quantum well device comprising a material as hereinbefore described.
  • the invention will be further described by way of example only, by reference primarily to a system in which the small particles are gold and the linker molecule is a dithiol. Additionally some examples of applications using semi conductor particles as well as metal particles are given.
  • the ruby coloured dispersions contain particles, shown by TEM, to be in the range between 6 and 12 nm.
  • Example 2 A solution of 1,9 nonanedithiol in toluene as described in Example 2 (typically 10 ml, 0.2 mmol dm- 3 ) was added to a solution of small gold particles (100 ml, 250 - 500 mg gold dm -3 , size range 6 - 12 nm) prepared as described in Example 1.
  • the small gold particles precipitate over night quantitatively and form a bulk material as illustrated in Fig 1, which is a schematic representation of the growth of bulk material by self assembly from dissolved metal
  • a solution of small gold particles was prepared as described in Example 1 but in the presence of 1,9 nonanedithiol in the organic phase.
  • nonanedithiol was added to the reaction mixture immediately before the addition of the reducing agent (sodium borohydride). At least an equimolar amount of 1,9 nonanedithiol with respect to gold is required, but higher ratios are possible. A dark precipitate of the nanomaterial is formed within a few minutes after addition of the reducing agent.
  • the activation energy for electron hopping is ca. 5 times higher as temperature dependent
  • Fig. 2 is a schematic representation of the preparation of a layered structure. More particularly it shows the preparation of nanostructured materials by surface functionalization of the substrate followed by successive attachment of gold nanoparticles and bifunctional linker molecules, in this example, a dithiol, 2A illustrates glass silonization, 2B
  • Fig. 3 is a schematic representation of a multilayer nanostructure array forming quantum dots.
  • Small particles anchor to a substrate containing linker groups and subsequent growth of layers can then be achieved by alternatively derivatising the surface with for example dithiol and with gold particles.
  • the technique is described by way of an example.
  • Glass microscope slides were functionalised with (3-mercaptopropyl)trimethoxysilane.
  • the functionalised slides were immersed overnight in a solution of colloidal gold in toluene with a gold content of approximately 250 mg dm as described in Example 1.
  • the layer of gold particles formed overnight on the glass surface is visible with the naked eye as a slight pink tint.
  • the derivatised slides were washed
  • Fig. 5 shows a typical STM image of the material obtained with a Burleigh scanning tunnelling microscope. The image shows unambiguously that the individual particles do not coalesce to form bigger units as its is commonly observed for deposits of colloidal metals.
  • the present method involves the use of two solutions, one of nanoparticles and the other of polyfunctional linker molecules.
  • the fabrication process comprises simply the successive immersion of the sample on which the device is to be grown in solutions of the above separated by a simple washing step. The operation can be carried out in an open fume cupboard, without the need of sophisticated and high capital cost control equipment.
  • Nanostructured quantum dot, quantum wire and quantum well materials will be of great importance for the development of the new generation of
  • the present invention can be regarded as the prototype of a nanostructured array of quantum dots with adjustable electronic conductivity in the range typical for semi conductors.
  • oxidants such as chlorine or ozone.
  • a further example of the application of the techniques described herein is the preparation of materials, such as, for example, glass modified to benefit from the unique electrochromic effects which can be produced by applying thin film structures to substrates.
  • the thin film structures can be prepared by functionalising the glass with a mercaptosilane.
  • the functionalisation of surface OH groups with tri- methoxypropyl mercaptosilane leads to an -SH
  • the Au-terminated layer can then be derivatised with, for example, a dithiol leading again to an -SH terminated layer. Again, by immersion of the material in the colloidal gold solution, a new layer can be grown. The process can be repeated many times, leading to the growth of multilayers of a material formed by clusters joined in a 3-D array by multifunctional organic groups.
  • the optical and electrical properties of the material are dependent on the organic groups used for joining the metal clusters. For instance, the organic groups used for joining the metal clusters.
  • resistivity is greatly decreased in the order of C 16 , C 12 , C 9 and C 6 dithiols.
  • the use of a p-xylene-dithiol results in compounds of very low resistivity, showing the important influence of the potential energy barrier resulting from the presence of the organic linker between the clusters.
  • FIG. 2 schematic model of the type of structures which are probably formed is shown in Fig. 2.
  • electrochromic properties can be produced using the methods and solutions of the invention, the potential (and hence, charge) dependence on the optical
  • ER electroreflectance
  • the second aspect that is very important from the point of view of the practical applications of these novel materials is the order of magnitude of the effect. From AC impedance measurements it appears that the charge modulation is always localised in the metal layer in contact with the electrolyte solution. Thus, the overall change in reflectance with potential, which is of the order of 0.1%, is localised in a region with a thickness of the diameter of the particles used, which was approximately 8 nm in these
  • FIG. 10 shows the current-potential response of a solid state nanostructured device consisting of:
  • Fig. 11 is a diagrammatic illustration of the basic structures for the preparation of a solid state TiO 2 sensitised photovoltaic deivce.
  • VB-valence band; CB conduction band.
  • gold, semi conductor particles such as, for example, gold, semi conductor particles such as, for
  • TiO 2 indium tin oxide (ITO), and CdS can be
  • TiO 2 particles are self-assembled in a structure consisting of linkers incorporating electron transfer donor and acceptor groups, present on opposite sides of the layer of TiO 2 nanoparticles obtained by a step-wise process of the type schematically described with reference to metal particles in Fig. 2.
  • the performance can be tuned to the wavelength of the incident radiation.
  • IR reflectors with, for example ITO by controlling the size of the particles forming a film array.
  • IR reflectors are of fundamental importance for ensuring that the temperature of operation of PV modules is kept as low as possible.
  • ITO thin films are prepared by sputtering and the resulting

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Abstract

La présente invention se rapporte à un procédé de production d'une structure de couche mince à partir de particules aux dimensions nanométriques, ce procédé consistant à former au moins une couche de particules métalliques ou semi-conductrices sur un substrat par traitement du substrat avec une molécule de liaison polyfonctionnelle de sorte qu'un premier groupe réactif de la molécule de liaison polyfonctionnelle réagisse avec le substrat pour se lier à celui-ci, puis à traiter le substrat fonctionnalisé avec une solution de particules métalliques ou semiconductrices de sorte qu'un second groupe réactif de la molécule de liaison polyfonctionnelle réagisse avec les particules métalliques ou semi-conductrices pour se lier à celles-ci.
PCT/GB1995/002124 1994-09-10 1995-09-08 Procede de synthese de materiaux aux proprietes electroniques, magnetiques et/ou optiques regulees WO1996007487A1 (fr)

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