EP2104751A1 - Procédé de préparation de points quantiques incorporés dans une matrice et points quantiques incorporés dans une matrice et préparés à l'aide du procédé - Google Patents

Procédé de préparation de points quantiques incorporés dans une matrice et points quantiques incorporés dans une matrice et préparés à l'aide du procédé

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Publication number
EP2104751A1
EP2104751A1 EP07856081A EP07856081A EP2104751A1 EP 2104751 A1 EP2104751 A1 EP 2104751A1 EP 07856081 A EP07856081 A EP 07856081A EP 07856081 A EP07856081 A EP 07856081A EP 2104751 A1 EP2104751 A1 EP 2104751A1
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EP
European Patent Office
Prior art keywords
quantum dots
precursor
matrix
reagent
substrate
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.)
Ceased
Application number
EP07856081A
Other languages
German (de)
English (en)
Inventor
David FUERTES MARRÓN
Sebastian Lehmann
Sascha Sadewasser
Martha Christina Lux-Steiner
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.)
Helmholtz Zentrum Berlin fuer Materialien und Energie GmbH
Original Assignee
Helmholtz Zentrum Berlin fuer Materialien und Energie GmbH
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Application filed by Helmholtz Zentrum Berlin fuer Materialien und Energie GmbH filed Critical Helmholtz Zentrum Berlin fuer Materialien und Energie GmbH
Publication of EP2104751A1 publication Critical patent/EP2104751A1/fr
Ceased legal-status Critical Current

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    • 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
    • C23C14/04—Coating on selected surface areas, e.g. using masks
    • C23C14/042—Coating on selected surface areas, e.g. using masks using masks
    • 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
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/02—Pretreatment of the material to be coated
    • 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
    • C23C14/0623—Sulfides, selenides or tellurides
    • 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
    • C23C14/46—Sputtering by ion beam produced by an external ion source
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02—Pretreatment of the material to be coated
    • C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
    • C23C16/0281—Deposition of sub-layers, e.g. to promote the adhesion of the main coating of metallic sub-layers
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/305—Sulfides, selenides, or tellurides
    • 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
    • C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/02—Pretreatment of the material to be coated
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F77/00—Constructional details of devices covered by this subclass
    • H10F77/10—Semiconductor bodies
    • H10F77/12—Active materials
    • H10F77/126—Active materials comprising only Group I-III-VI chalcopyrite materials, e.g. CuInSe2, CuGaSe2 or CuInGaSe2 [CIGS]
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F77/00—Constructional details of devices covered by this subclass
    • H10F77/10—Semiconductor bodies
    • H10F77/14—Shape of semiconductor bodies; Shapes, relative sizes or dispositions of semiconductor regions within semiconductor bodies
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
    • H10P14/20—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials
    • H10P14/203—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials using transformation of metal, e.g. oxidation or nitridation
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
    • H10P14/20—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials
    • H10P14/26—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials using liquid deposition
    • H10P14/265—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials using liquid deposition using solutions
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
    • H10P14/20—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials
    • H10P14/34—Deposited materials, e.g. layers
    • H10P14/3402—Deposited materials, e.g. layers characterised by the chemical composition
    • H10P14/3436—Deposited materials, e.g. layers characterised by the chemical composition being chalcogenide semiconductor materials not being oxides, e.g. ternary compounds
    • 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
    • Y02E10/541—CuInSe2 material PV cells
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Definitions

  • the invention relates to a method for producing quantum dots embedded in a matrix on a substrate and to quantum dots embedded in a matrix produced by the method.
  • quantum dots For objects with dimensions of only a few nanometers, so-called quantum or nanopoints or islands, the freedom of movement of the electrons is limited in all three spatial directions ("zero-dimensional system") The linear dimension in all three directions is thus less than the de Broglie wavelength of the charge carriers
  • quantum dots have a highly modified electronic structure from the corresponding bulk material, in particular the density of states is more like that for molecules
  • the size and the electronic structure can be influenced, because of the small electrical capacity of the quantum dots, the addition of another electron (“single-electron tunneling") to the already present in the quantum dot, a certain energy expenditure in the range of a few 10 meV to several 100 meV (“Coulomb blockade”).
  • Quantum dots are currently mainly used in nanoelectronics and nanoelectronics, for example photodetectors and semiconductor lasers, but also in solar cells.
  • Quantum dots are currently mainly used in nanoelectronics and nanoelectronics, for example photodetectors and semiconductor lasers, but also in solar cells.
  • the generation of binary, ternary or multinary compound semiconducting quantum structures in a semiconducting matrix is becoming increasingly important in the production of efficient solar cells.
  • the most widely used method of producing quantum dots is the Stranski-Krastanov epitaxial growth method, which relies on strain of the crystal lattice of the growing semiconductor on the overgrown substrate material. This lattice strain causes the growing layer does not grow uniformly, but form small, nanometer-sized islands, which represent the quantum dots.
  • This method allows some control of the quantum dot size and density while controlling the arrangement and positions is very limited.
  • Other quantum dot fabrication methods use the scanning probe microscopy methodology. These methods allow a very good control of the size and position of the quantum dots, but they are sequential methods in which each quantum dot must be individually tailored. Thus, such methods are only partially suitable for components with a large number of quantum dots.
  • the in-situ generation of quantum dots in a matrix is known, for example, from US 2004/0092125 A1.
  • a dielectric precursor is applied to a thin metal layer on a substrate and heated in stages, whereby the metal layer and the precursor are stacked in layers, so that quantum dots are formed from the precursor in the metal layer.
  • a production method of quantum dots is known in which GaAs quantum dots formed from Ga drops are coated with a buffer layer and a barrier layer as a passivation layer.
  • a similar procedure is from the KR 1020010054538 A known.
  • JP 2006080293 A discloses a method for the self-organized arrangement of InAs quantum dots on a GaAs layer, wherein the quantum dots are embedded in a GaAs matrix. Furthermore, it is known from US Pat. No. 5,229,320 to deposit quantum dots through a porous GaAs membrane on an AIGaAs substrate and subsequently to grow a matrix of AIGaAs for embedding. A method for producing a polymer with dispersed nanoparticles is known from DE 601 08 913 T2, wherein first a polymer precursor is deposited, then nanoparticles are distributed thereon as quantum dots and these are embedded by crosslinking of the polymer by heating in the matrix.
  • a polymer is added. This serves primarily to encase the dissolved precursor in the solvent and prevents agglomeration of the nanoparticles during the spray deposition.
  • the polymer deposits on the substrate, where it forms a matrix in which the quantum dots are embedded.
  • Such a polymer matrix of a transparent plastic has a specific refractive index for optical purposes and can with additional polymer layers of other refractive indices are layered. The polymer does not undergo a chemical reaction, it does not interact with the reagent.
  • Materials other than a polymer can not be used in the known method of forming the matrix because matrix formation is merely a secondary effect there and is formed as a simple precipitate on the substrate.
  • the main purpose of the polymer used is to prevent the agglomeration of the dissolved precursor particles and to have corresponding materials and properties.
  • US 2003/0129311 A1 discloses a similar process, in which, however, first a porous polymer template is formed. The pores of the polymer are then filled with a precursor solution, from which then the quantum dots are formed.
  • the object of the invention is to provide a method for generating quantum dots embedded in a matrix, with which it is possible selectively to produce any but polymer-free matrices without aggravating method limitations.
  • the choice of the matrix composition should be independent of the quantum dot properties, but also determine the material composition of the quantum dots, so that a concordant composition results between quantum dots and matrix.
  • Generation of the quantum dots should remain independent of the strong process limitations of epitaxial growth.
  • the process should be simple, inexpensive and robust and preferably also lead to products based on compound semiconductors, which can be used in particular in solar cell technology. The solution to this problem can be found in the method claim.
  • Advantageous developments of the invention are set forth in the subclaims and explained in more detail below in connection with the invention.
  • the invention provides a method for the production of quantum dots embedded in a matrix on a substrate, in which first quantum dots of a precursor (precursor) of at least one first metal or a metal compound are applied to the substrate.
  • the highly structured or nanostructured deposition determines the geometry and density of the quantum dots.
  • the electronic properties of the quantum dots are determined independently of the substrate, whereby a multiplicity of different substrates can be used, for example simple glass, metal-coated glass, monocrystalline wafers, polycrystalline layers, films. Coupling, for example, to prestressed lattice states in a crystalline substrate is eliminated.
  • the use of a precursor in the invention removes the link between ultimate feature size and self-assembly of the quantum dots during the process.
  • Various methods for applying the quantum dots are known per se and are mentioned below.
  • the reagent consists of at least one second metal and / or a chalcogen and contains all elements of the matrix to be formed, wherein the matrix has a composition exclusively of the elements of the reagent.
  • the chemical reaction between the precursor and the reagent is brought about by a simultaneous or subsequent temperature increase (annealing step) for contacting.
  • the contact between the reagent and the applied quantum dots results in a chemical reaction of the precursor to the desired final material composition of the quantum dots.
  • a matrix of the elements in the reagent with a corresponding stoichiometric ratio is formed.
  • the matrix deposits, so that the quantum dots are fully embedded in the in-situ formed matrix after carrying out the reaction with the reagent.
  • quantum dots can be prepared starting from elemental metals or metal compounds as a precursor by a gas phase reaction with multinary or elemental chalcogens.
  • the gas phase reaction step in the method according to the invention preferably serves to grow the matrix from a binary, ternary or multinary compound semiconductor, into which the quantum dots are also formed in a compound semiconductor ( with one or more metal components opposite the matrix).
  • the gas phase reaction step on the one hand take place so that the precursor is reacted directly to the final product, for example by increased process temperature, or on the other hand so that this reaction takes place in a subsequent, separate annealing step.
  • the dimensions of the precursor structure, the precursor elements used and the elements of the gas phase reaction used determine the structural, electronic and optical properties of the end product.
  • Various methods are available for the preparation of the precursor as well as for the gas phase reaction.
  • a multiplicity of methods are available which are then converted by means of the following gas-phase-based method step into preferably semiconducting structures, such as, for example, evaporation, sputtering, lithographic processes, focussed ion beam, Methods based on scanning probe microscopy, electrochemical deposition and the wet-chemical methods ILGAR and SILAR.
  • gas-phase-based method step into preferably semiconducting structures, such as, for example, evaporation, sputtering, lithographic processes, focussed ion beam, Methods based on scanning probe microscopy, electrochemical deposition and the wet-chemical methods ILGAR and SILAR.
  • From the closest to the invention DE 694 11 945 T2 a method for applying a dissolved precursor is known, which can also be used in the invention, but with the proviso that the precursor used is also soluble.
  • the method is then advantageously characterized in a development by a liquid-phase precursor which is dissolved in a vaporizable solvent
  • the solvent may be evaporated before, during, or after initiation of the chemical reaction between the precursor and the reagent such that a wet or dry chemical reaction results in the end product of the quantum dots.
  • a solid phase precursor in addition to the dissolved application of the precursor but can also be used advantageously a solid phase precursor. Using special but quite simple methods, it is then applied to the substrate in a high to nanostructured form.
  • a solid-phase precursor in the form of nanoparticles can be applied to the substrate by simple scattering. Targeted application of the nanoparticles, for example with micromanipulatoren, is also possible.
  • a similar variety of processes are available for the gas phase reaction of the desired elements in the reagent with the metallic precursors.
  • Semiconducting elements are preferably used in the method according to the invention.
  • the desired end product which usually contains at least one metal and / or a chalcogen
  • various combinations of elemental, binary, ternary or multinary metallic precursors are available which can be combined with appropriate elemental, binary, ternary or multinary chalcogenides in the reagent can be reacted.
  • binary, ternary or multinary compound semiconductors for the quantum structure and the matrix are preferably generated. In this case, elements from groups I to VI are preferably used.
  • the deposition of a diffusion barrier or passivation layer onto the applied quantum dots can be provided as an additional method step in the previously described method for the production of quantum dots embedded in a matrix, which allows the lateral outdiffusion of the precursor particles. Prevents elements from the quantum dots.
  • the method according to the invention thus produces quantum dots embedded in a matrix, which are characterized by a concordant composition between quantum dots and matrix in a simple manner, which is not restricted by structures or materials.
  • the quantum dots are an additive composition of the Elements of precursor and reagent and the matrix has a composition consisting solely of the elements of the reagent.
  • the concordant composition can preferably be based advantageously on the basis of binary, ternary and / or multinary semiconductor compounds. embodiments
  • Embodiments of the method for producing quantum dots embedded in a matrix on a substrate according to the invention and the product which can be produced therewith are explained in more detail below with reference to synthesis examples and a schematic figure for a further understanding of the invention.
  • the figure shows the individual process steps of the method according to the invention.
  • the method is exemplary for the growth of quantum dots QD from ternary or multinary compound semiconductors of the chalcopyrite family (Na 1 Cu 1 Ag) (Al 1 Ga 1 In 1 TI) (S 1 Se 1 Te) 2 or generally l-III-VI 2 Compounds and for simple binary compounds of the type 1-Vl 1 1 2 -Vl 1 Hl-Vl 1 Hl 2 -Vl 3 etc., such as CuS, Cu 2 S, Ga 2 Se 3 , GaSe, described and may be similar Also be transferred to compounds containing IN-V 1 H-VI and group IV elements.
  • the precursor PC in the case of ternary and multinary compounds consists of Group I, Group III or MII-type alloys deposited on a substrate SU by a suitable method (see above), and then during a subsequent annealing step be exposed to the gas atmosphere of the reagent RG.
  • the reagent RG contains one or more chalcogens and the metals which are not present in the precursor PC and which are still desired in the finished quantum dot QD.
  • the dry precursor PC is applied to the substrate SU in the form of nanometer-sized islands, that is to say in highly structured form.
  • the final size of the quantum dots QD of the binary, ternary or multinary compound may generally differ from the size of the precursor islands and depends on the diffusion process of the various elements involved in the conditions during the gas phase reaction step. As a function In this case, the final structure of these reaction conditions can show a smaller or larger dimension than the originally applied precursor islands.
  • Precursor PC metallic points with lateral and vertical dimensions in the nanometer range are first deposited on a substrate SU made of glass (non-conductive) or molybdenum-coated glass (conductive).
  • the deposition of this precursor PC takes place by means of evaporation using a suitable mask for nanostructuring of the metal deposition.
  • it may also be by physical vapor deposition, molecular beam epitaxy, chemical transport methods (chemical vapor deposition, metal-organic vapor deposition, etc.) or chemical or electrochemical processes (SILAR, ILGAR, electrodeposition, chemical bath deposition, etc.).
  • the substrate SU with the metal precursors PC is then subjected to an annealing step which allows the reaction with the gaseous reagent RG, which in this case contains Ga and Se.
  • the gaseous components react with the Cu, forming the ternary compound CuGaSe 2 in the form of nanometer-sized quantum dots.
  • the process parameters are chosen such that these ternary quantum dots form within a matrix MA of a binary compound (Ga 2 Se 3 ), which precipitates simultaneously with the reaction to the ternary quantum dots (see the figure).
  • the matrix MA deposits first on the substrate SU and then on the converted quantum dots QD, so that the quantum dots QD are finally embedded in the matrix MA.
  • the Process kinetics that determine the size and shape of the resulting nanometer sized structures can be controlled via process parameters including, but not limited to, process temperature, gas phase saturation conditions at the appropriate substrate temperature, and process time.
  • the precursor PC consists of a metallic alloy of Cu and Ga in the desired composition, which is prepared by previously described methods and then subjected to an annealing step with In 1 Se and S as reagent RG in the gas phase.
  • the reaction kinetics is controlled as described above.
  • Cu (In, Ga) (Se 1 S) quantum dots QD are formed in an ln 2 (Se, S) 3 matrix MA.
  • the precursor PC consists either of islands of Group I or Group III elements or of alloys of Group I or Group III elements or of alloys or islands of Type I-III, which are then subjected to the annealing step in the presence of not contained in the precursor PC, still needed metals and the desired chalcogen are subjected, this being carried out by chemical vapor transport.
  • metal halides, organometallic compounds and chalcogen halides are used, as in a common chemical or metal-organic gas phase process.
  • a matrix MA of metals which are not yet contained in the precursor PC and still require the required chalcogen forms on the substrate SU at the same time.
  • Halides are binary compounds of a halogen atom and an element or radical that is less electronegative than the halogen. With the salt-forming halogens F, Cl, Br, I correspondingly fluorides, chlorides, bromides and iodides are formed. In combination with metals or chalcogens as partners, metal or chalcogen halides are formed accordingly. Metal halides are used in particular in lighting technology.
  • the organometallic compounds are compounds in which an organic radical or an organic compound is bonded directly to a metal atom.
  • all of the metal halides, organometallic compounds and chalcogen halides known to those skilled in the art for use in a conventional chemical or metal-organic gas phase process can be employed in the invention.
  • the precursor PC consists of metals as described above, with a certain proportion of a few percent or more of magnetic elements, for example Mn or Fe, being added to these metals.
  • the annealing step then takes place again as described above.
  • There is no change in the composition of the matrix MA compared with what has been described above.
  • the magnetization occurs only in the area of the quantum dots QD.
  • Process pressure from UHV (1CT 6 mbar and less) in evaporation-based systems (PVD, MBE), low pressures (10 "1 to 10 2 mbar) in chemically-based systems, ambient pressure at electrode position, and higher.
  • Process temperature depends on the type of metallic precursor used. From ⁇ 300 ° C for Cu-Al-Na based precursor PC and higher; from room temperature for In-Ga based precursors and higher. Upper temperature limits are set by the type of substrate used SU: ⁇ 600 ° C for standard glass, more than 1000 0 C for metal foils, under 250 to 300 0 C for plastic substrates. The chemical reaction for elements such as Cu, In and Se is exothermic, so here the room temperature is sufficient as a process temperature.
  • Process time Dependent on the deposition and the process technology.
  • the deposition of the precursor PC can take place within a few seconds.
  • the simultaneous or subsequent heating process can take between a few seconds and hours (without heating-cooling cycles) (depending on the desired material composition of the quantum dots QD and layer thickness of the matrix MA).

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  • General Physics & Mathematics (AREA)
  • Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
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Abstract

L'invention concerne un précurseur métallique qui est dissous dans une solution contenant un polymère devant être déposé sur un substrat par répartition de la pulvérisation des gouttelettes. Une réaction en phase gazeuse consécutive avec un réactif contenant des chalcogènes produit des points quantiques dans une matrice polymère. Pour produire des matrices quelconques toutefois sans polymères, le procédé selon l'invention permet, après avoir fourni des points quantiques (QD) à partir d'un précurseur (PC), la mise en contact consécutive des points quantiques (QD) fournis et du substrat (SU) non recouvert avec un réactif en phase gazeuse (RG) qui contient tous les constituants de la matrice (MA) que l'on doit obtenir. On effectue une réaction chimique entre le précurseur (PC) et le réactif (RG) par une hausse de température qui se produit en même temps ou après la mise en contact. On peut ainsi produire une composition concordante entre les points quantiques (QD) et la matrice (MA), les points quantiques (QD) présentant une composition d'additifs à partir des éléments du précurseur (PC) et du réactif (RG) et la matrice (MA) présentant une composition exclusivement à partir des éléments du réactif (RG). Grâce à un choix des éléments adapté, on peut produire des composés semi-conducteurs binaires, ternaires ou multinaires que l'on retrouve dans des applications nano-optiques, nanoélectroniques mais aussi dans les cellules photovoltaïques.
EP07856081A 2006-12-16 2007-12-11 Procédé de préparation de points quantiques incorporés dans une matrice et points quantiques incorporés dans une matrice et préparés à l'aide du procédé Ceased EP2104751A1 (fr)

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DE102006060366A DE102006060366B8 (de) 2006-12-16 2006-12-16 Verfahren zur Herstellung von von einer Matrix abgedeckten Quantenpunkten
PCT/DE2007/002230 WO2008074298A1 (fr) 2006-12-16 2007-12-11 Procédé de préparation de points quantiques incorporés dans une matrice et points quantiques incorporés dans une matrice et préparés à l'aide du procédé

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US9490414B2 (en) 2011-08-31 2016-11-08 L. Pierre de Rochemont Fully integrated thermoelectric devices and their application to aerospace de-icing systems
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US9159872B2 (en) 2011-11-09 2015-10-13 Pacific Light Technologies Corp. Semiconductor structure having nanocrystalline core and nanocrystalline shell
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DE102006060366B4 (de) 2012-08-16
JP2010513032A (ja) 2010-04-30
DE102006060366A1 (de) 2008-06-19
US20100108986A1 (en) 2010-05-06
US8334154B2 (en) 2012-12-18
WO2008074298A1 (fr) 2008-06-26

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