WO2006034561A1 - Convertisseur de lumiere a petite ouverture hautement efficace - Google Patents

Convertisseur de lumiere a petite ouverture hautement efficace Download PDF

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Publication number
WO2006034561A1
WO2006034561A1 PCT/BY2004/000023 BY2004000023W WO2006034561A1 WO 2006034561 A1 WO2006034561 A1 WO 2006034561A1 BY 2004000023 W BY2004000023 W BY 2004000023W WO 2006034561 A1 WO2006034561 A1 WO 2006034561A1
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Prior art keywords
nanocrystals
optical
chosen
film
xerogel
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PCT/BY2004/000023
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English (en)
Inventor
Sergey V. Gaponenko
Ulrike Woggon
Mikhail V. Artemyev
Leonid I. Gurinovich
Nikolay V. Gaponenko
Igor S. Molchan
Andrey A. Lutich
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The State Scientific Institution 'institute Of Molecular And Atomic Physics Of The National Academy Of Science Of Belarus'
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Priority to PCT/BY2004/000023 priority Critical patent/WO2006034561A1/fr
Priority to EA200700629A priority patent/EA010503B1/ru
Publication of WO2006034561A1 publication Critical patent/WO2006034561A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/02—Details
    • H01L31/0232—Optical elements or arrangements associated with the device
    • H01L31/02322—Optical elements or arrangements associated with the device comprising luminescent members, e.g. fluorescent sheets upon the device
    • 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
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/002—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of materials engineered to provide properties not available in nature, e.g. metamaterials
    • G02B1/005—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of materials engineered to provide properties not available in nature, e.g. metamaterials made of photonic crystals or photonic band gap materials

Definitions

  • the present invention relates to optical devices, and more particularly to optical devices comprising semiconductor quantum-size structures, which exhibit spatial electronic confinement, and dielectric photonic crystals, which exhibit spatial photonic confinement in the optical range of the electromagnetic spectrum.
  • the present invention can be used in optoelectronic devices employed as light detectors, emitters, and converters.
  • light conversion devices are based on employing new phosphors and/or new means of excitation thereof.
  • certain benefits of a device in one aspect are accompanied by considerable drawbacks in another aspect.
  • organic dyes introduce a number of unavoidable problems such as photochemical instability, invariability of spectral properties, low optical density, sensitivity to outdoor influence, etc.
  • organic-based phosphors do not possess sufficient compatibility with silicon-based photodetectors. the latter being most widely used type of photodevices.
  • optical spectral converter comprises a film of transparent unidirectionally arrayed material (a two-dimensional photonic structure), wherein the cavities are filled with wavelength- converting substance.
  • the wavelength-converting substance has the form of xerogel containing nanosize nanostr ⁇ ctures (nanocrystals or nanoclusters), which exhibit strong quantum-size effects.
  • the xerogel can be chosen from the family Of Al 2 O 3 , In 2 O 3 , TiO 2 , SiO 2 gels.
  • Nanocrystals can be chosen from the series of H-VI, I-VII, IH-V semiconductor compounds, preferably CdS, CdSe, ZnS, ZnSe, or a combination thereof forming a core-shell structure, e.g., CdSe/ZnS.
  • the nanocrystals are doped by metal ions, which can be chosen from among Mn 2+ , Eu 3+ , Tb 3+ , Sm 3+ , e.g., ZnSe:Mn 2+ /ZnS.
  • the film of transparent unidirectionally arrayed material can be one of the following photonic crystal types: porous membrane; mesotube monolayer; artificial opal.
  • the said photonic crystal is fabricated from the substance chosen from among the oxides SiO 2 , Al 2 O 3 , TiO 2 .
  • an optical-range photosensitive device with a thin-film wavelength converter comprises a film of transparent unidirectionally arrayed material (a two-dimensional photonic structure), wherein the cavities are filled with wavelength-converting substance.
  • the wavelength- converting substance has the form of xerogel containing nanosize nanostructures (nanocrystals or nanoclusters), which exhibit strong quantum-size effects.
  • the xerogel can be chosen from the family Of Al 2 O 3 , In 2 O 3 , TiO 2 , SiO 2 gels.
  • Nanocrystals can be chosen from the series of H-VI, I-VII, III-V semiconductor compounds, preferably CdS, CdSe, ZnS, ZnSe, or a combination thereof forming a core-shell structure, e.g., CdSe/ZnS.
  • the nanocrystals are doped by metal ions, which can be chosen from among Mn 2+ , Eu 3+ , Tb 3+ , Sm 3+ , e.g., ZnSe:Mn 2+ /ZnS.
  • the film of transparent unidirectionally arrayed material can be one of the following photonic crystal types: porous membrane; mesotube monolayer; artificial opal.
  • the said photonic crystal is fabricated from the substance chosen from among the oxides SiO 2 , Al 2 O 3 ,, TiO 2 .
  • Said optical photosensitive device comprises a said optical converter and a conventional optical detector, preferably a photodiode or phototransistor, in which case the whole device is fabricated on a silicon substrate.
  • the said optical detector may be a photoresistor, a solar cell, or a charge-coupled device (CCD) detector.
  • CCD charge-coupled device
  • a method of increasing the sensitivity of a photodetector in short wavelength range blue to ultraviolet spectral range.
  • the method consists in depositing an additional thin-film optical coating (conversion coating) onto a photosensitive area of the photodetector.
  • Said coating comprises a film of transparent unidirectionally arrayed material (a two-dimensional photonic structure), wherein the cavities are filled with wavelength-converting substance.
  • the wavelength- converting substance has the form of xerogel chosen from among Al 2 O 3 , In 2 O 3 , TiO 2 , SiO 2 gels and containing nanosize nanocrystals chosen from the series of H-VI, I-VII, IH-V semiconductor compounds, preferably CdS, CdSe, ZnS, ZnSe, or a combination thereof forming a core-shell structure (e.g., CdSe/ZnS), and doped by metal ions chosen from among Mn 2" , Eu 3+ , Tb 3+ , Sm 3+ (e.g., ZnSe:Mn 2+ /ZnS).
  • xerogel chosen from among Al 2 O 3 , In 2 O 3 , TiO 2 , SiO 2 gels and containing nanosize nanocrystals chosen from the series of H-VI, I-VII, IH-V semiconductor compounds, preferably CdS, CdSe, ZnS, ZnSe,
  • the film of transparent unidirectionally arrayed material can be one of the following photonic crystal types: porous membrane; mesotube monolayer; artificial opal.
  • Said optical photodetector can be a commercial semiconductor device of any type, such as a photodiode, a phototransistor, a photoresistor, a CCD detector, or a solar cell.
  • the commercial photodetector can be silicon-based.
  • FIG. 1 is a schematic illustration of various types of nanostructures: microporous silicon ( ⁇ ), mesotubes (b), synthetic opals (c), and the same said structures with pores filled with a gel (d. e,f) containing semiconductor quantum-sized nanocrystals.
  • FIG. 2 is a plot of the angular scattering diagram relative to the direction of the pores for a thin film of porous alumina for a light ray incident at different angles ⁇ .
  • FIG. 3 is a plot of the absorption and photoluminescence (PL) spectra of semiconductor quantum-sized ZnSe:Mn/ZnS nanocrystals in a thin polymer film, measured at room temperature.
  • PL absorption and photoluminescence
  • FIG. 4 is a plot of the luminescence indicatrix of a thin film of mesoporous alumina containing in its pores quantum-sized Mn-doped CdS nanocrystals ( ⁇ ), together with the luminescence indicatrix of the same nanocrystals inside a polymer film on a smooth silicon substrate (b).
  • FIG. 5 is a view of the spectral converter for conversion of radiation from blue and UV spectral range into longer-wavelength spectral range, according to the present invention.
  • FIG. 6 is a view of a highly efficient indicator panel with narrow output angular diagram, according to the present invention.
  • FIG. 7 is a view of a photodetector with increased photosensitivity in the near-UV spectral range.
  • sol-gel method of luminescent film fabrication A specific feature of the sol-gel method is the possibility of luminescent film formation made of xerogels in various mesoporous matrices [[5]
  • porous anodic alumina which consist of hexagonally packed self-organized cells with vertically arranged mesopores in the middle of the cells [[6] G.E.Thompson and G.C.Wood. Nature, V. 290 (1981 ) 230—
  • the luminescence of nanocrystals in the films formed in mesoporous matrices of anodic alumina and porous silicon is of significant interest due to high photochemical stability and better quantum yield compared to traditional films, which are rare earth-doped and formed with the sol-gel method on monocrystalline or porous silicon [[9] A.M.Dorofeev, N.V.Gaponenko, V.P.Bondarenko, E.E.Bachilo, N.M.Kazuchits, A.A.Leshok, G.N.Troyanova, N.N.Vorozov, V.E.Borisenko, H.Gnaser, W.Bock, P.Becker and H.Oechsner.
  • samples of porous anodic alumina can exhibit properties of a tvvo- dimensional photonic crystal [[13] H.Masuda, M.Ohya, H.Ason, M.Nakao, M.Montomi, and
  • porous anodic alumina gives rise to a synthesis technique of film structures providing control over spontaneous emission of phosphors located inside the pores as was observed with some samples of synthetic opals saturated with luminescent dyes [[16] E.P.Petrov, V.N.Bogomolov, I.I.Kalosha, and
  • W W 0 [I - (I - R) exp(-k!')), where WQ is the intensity of incident external radiation, R the reflectance at air/matrix boundary, k the absorptance, / * the effective "mean free path" of the photons.
  • the choice of semiconductor nanocrystals exhibiting quantum-size effects as an optically active material for luminescence center formation is determined by the presence of a number of unique optical properties related to spatial electron confinement.
  • the spatial confinement modifies the energy spectrum for the electrons and the probabilities of transition from one state to another. This leads to the optical manifestation of quantum-size effects.
  • the absorption and luminescence spectra, as well as the lifetime of the excited state is determined by the spatial configuration and size of quantum-sized structures rather than by the chemical composition thereof.
  • the characteristic size of such structures in the direction of confinement is of the order of one to several tens of nanometers, so the structures are called nanostructures.
  • photonic crystals that are of interest to device engineering
  • Three types of such photonic structures have been realized practically, as depicted in FIG. 1 : microporous membrane (a), mesotubes (b), and synthetic opal (c).
  • a thin film structured according to one of said types of photonic crystals is thus capable of redistributing the flow of light with any cross-section in a predetermined direction (as seen in FIG. 2).
  • Porous structures can have their pores filled with various compositions, for instance, with products of sol-gel synthesis (sols, gels, or xerogels) in order to adjust the mode structure by means of changing the medium/pore refractive index contrast.
  • H-VI semiconductors which serve as a base for fabrication of quantum-sized nanoparticles with controlled optical characteristics. Owing to strong spatial confinement of charge carriers in such nanocrystals, their absorption and luminescent spectra depend on the particle size rather than on its material, which allows to vary their optical properties.
  • the absorptance being high in the short-wavelength range ( ⁇ >10 4 ), semiconductor nanocrystals are efficient phosphors in the visible wavelength range.
  • the idea of the efficiency increase of light-emitting or light-converting devices according to the present invention is to concentrate the flow of light of the spontaneous emission from a source in one predetermined direction corresponding to a main photonic mode by placing the luminescent centers inside the cavities (pores) of a photonic crystal, the luminescence being excited at wavelength from other (more particularly, shorter-wave) spectral range.
  • vertically aligned mesoscopic pores in the anodic alumina film are filled with xerogel according to the sol-gel technology, said xerogel containing quantum-sized ZnSe:Mn + /ZnS nanocrystals doped with manganese ions, by means of multiple centrifugation of the corresponding sols and subsequent thermal treatment.
  • a structure possessing a highly directional output angular diagram and providing at least double increase in intensity at the direction normal to the sample surface is thus formed.
  • a line of optical devices can be designed, including displays, concentrators, converters, photodetectors, etc., which possess enhanced optical properties in a wide spectral range.
  • a porous film of material according to the construction design (silicon, alumina, glass, etc.) is manufactured. with the required porosity period according to the chosen working wavelength range.
  • the technology is chosen according to the relevant technical and cost requirements (chemical etching, anodic treatment, epitaxial growth, colloidal synthesis, etc.).
  • the manufactured film can be deposited on a working surface or remain on technological optically transparent substrates (such as glass, quartz, sapphire, etc.).
  • Mesoporous films located on transparent substrates can be utilized as a standalone device such as an optical concentrator.
  • quantum- sized nanocrystals are synthesized of any type of semiconductor compounds (II-VI, IH-V, I- VII; IV - Si, Ge, etc.) with or without shell, doped with Mn 2+ ions (or ions of other elements, e.g., rare earth ions Eu 3+ , Tb 3+ , Sm 3+ , etc.).
  • Said nanocrystals are nanoparticles with the such average size as to achieve a quantum-size short-wavelength shift of the edge of absorption band sufficient to separate the said absorption band from the luminescence band.
  • nanocrystals are passivated and dried to a powdery form.
  • nanocrystals are injected into sol-precursors of the xerogels based on titanium oxides TiOz, aluminum oxides Al 2 O 3 , indium oxides In 2 O 3 , silicon oxides SiO 2 , etc., having a high transmittance in the ultraviolet range.
  • Previously synthesized nanocrystals placed inside transparent xerogel matrices can be utilized as a standalone device, e.g., as a spectral converter of optical radiation or a UV-sensitizing coating for silicon-based and other photodetectors.
  • the previously manufactures mesoporous films are saturated with previously obtained xerogel containing previously synthesized nanocrystals by means of centrifugation (dipping, capillary wetting, etc.) in one or several cycles until the whole volume of the film pores is filled.
  • An external planar layer of gel is then formed to provide an optical gate for output radiation.
  • the mesoporous film can be mounted on an additional substrate made of any optically transparent material, such as an anodic alumina film on quartz or sapphire substrates.
  • the universal nature and a wide range of optical properties of output radiation of the present invention make it possible to create a complete line of highly directional display panels of various colors from near-monochromatic to white operating with a single illumination source and suitable for mass production.
  • the spectral optical converter constructed according to the first aspect of the present invention and schematically depicted in FIG. 5 comprises a film 1 of transparent uniformly arrayed mesoporous material, more particularly anodic alumina, saturated with a microporous xerogel, more particularly that based on indium oxide, containing emission centers 2, more particularly quantum-sized II-VI semiconductor nanocrystals doped with metal ions, more particularly manganese ions, and additionally comprising a substrate 3 made of quartz or glass and encased in a setting 4.
  • the mesoporous anodic alumina film can be fabricated through the next way.
  • the starting substrates represented glass, quartz or sapphire wafers, one surface of which contained adhesive Ta sublayer (20 A) and Al layer (5... 15 ⁇ m) formed by magnetron sputtering.
  • Fabrication of porous anodic alumina was realized by electrochemical anodizing of Al layer in 1.2 M phosphoric acid (PA) or 0.3 M oxalic acid (OA) solutions by a two-step method (see [[25] A.P.Li, F.Muller, U.Gosele. Polycrystalline and monocrystalline pore arrays with large interpore distance in anodic alumina, Electrochem. Solid-State Lett., V. 3, No. 3 5 (2000) 131 — 134] for the details).
  • Anodizing was performed at a temperature maintained at 20 0 C at a constant voltage 120 V (PA) or 40 V (OA), the resulting current was registered by an amperemeter.
  • the first anodizing was performed as long as a few minutes elapsed in steady-state regime.
  • the formed layer of anodic alumina was removed in an aqueous solution of 6 wt. % phosphoric acid and 1.8 wt. % chromic acid at a temperature 80...90 0 C.
  • the second anodizing was carried out in the same conditions.
  • the moment of finish of anodizing of Al layer was checked by decreasing the current in comparison to steady-state regime. At that moment, the voltage was lowered down to 100 V (PA) or 35 V (OA) to anodize Ta sublayer.
  • Anodizing of Ta sublayer was carried out until the current was decreased down to value of 0.05 of that of at steady-state regime.
  • porous anodic alumina was prepared by chemical etching of porous anodic alumina in 50 vol. % phosphoric acid (PA) for 1 h or in 10 vol. % phosphoric acid (OA) for 1 h, the temperature was kept at 25 0 C.
  • the preparation of porous anodic alumina was finished by rinsing in distilled water for 30 min and drying in air at 200 0 C for 10 min.
  • the resulting structure parameters of porous anodic alumina was as follows: pore diameters of 150 (PA) or
  • OA interpore distances 300 (PA) or 100 nm (OA).
  • the samples Prior to infiltration of porous anodic alumina with sols, the samples were dried at a temperature 200 0 C for 20 min to remove physically adsorbed water. Deposition of sol was performed by spin-on route at 2700...3000 rpm for 30 sec followed by drying in air at 200 0 C for 20 min.
  • the nanocrystals can be made as follows (see [[26] Jae Hun Chung, Chil Seong Ah, and Du- Jeon Jang. Formation and Distinctive Decay Times of Surface- and Lattice-Bound Mn "+ Impurity Luminescence in ZnS Nanoparticles. J. Phys. Chem. B, 105 (2001) 4128-4132] for the details).
  • Source materials Na 2 S 9H 2 O, Zn(NO 3 ) 2 -6H 2 O, and Mn(NO 3 )r6H 2 O were used as purchased from the Aldrich Chemical (Milwaukee, WI).
  • Aldrich Chemical Mowaukee, WI
  • ZnS-passivated ZnS nanoparticles (doped and passivated sample) were prepared by adding 2.5 mL of 40-mM Zn(NO 3 ) 2 -6H 2 O aqueous solution and 2.5 mL of 40-mM Na 2 S-W 2 O aqueous solution to 10 mL of the 2% Mn 2+ -doped sample at pH 10.3.
  • the average diameters of free and doped nanoparticles were estimated to be about 6 nm by using a transmission electron microscope (JEOL, JEM2000).
  • the saturation of the mesoporous film with xerogel containing nanocrystals can be carry out by means of multiple centrifugation of the corresponding sols and subsequent thermal t trrpea ⁇ ttmmpenntt.
  • the optical display panel constructed according to the second aspect of the present invention is schematically depicted in FIG. 6.
  • the said panel comprises a film 1 of transparent uniformly arrayed macroporous material, more particularly alumina, manufactured according to the example in the First Embodiment, saturated with a xerogel, more particularly that based on titanium oxide, containing emission centers 2, more particularly quantum-sized nanocrystals, and additionally comprising a substrate 3 made of a transparent material, more particularly quartz, glass, or sapphire.
  • the optical photosensitive device constructed according to the third aspect of the present invention and schematically depicted in FIG. 7 comprises a photodetector 5, more particularly a semiconductor photodiode having a photosensitive area 6 and an optical converter located over said photosensitive area 6, said converter manufactured according to the example in the First Embodiment and comprising a film 1 of transparent uniformly arrayed macroporous material, saturated with a xerogel, more particularly that based on aluminum oxide, containing emission centers 2, more particularly quantum-sized nanocrystals of the core-shell type, said core doped with metal ions, more particularly manganese ions, and additionally comprising electrical contacts 4 and a substrate 3 made of quartz.
  • a photodetector 5 more particularly a semiconductor photodiode having a photosensitive area 6 and an optical converter located over said photosensitive area 6, said converter manufactured according to the example in the First Embodiment and comprising a film 1 of transparent uniformly arrayed macroporous material, saturated with a xerogel, more particularly

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Abstract

L'invention concerne la conception d'un nouveau type de dispositifs construits sur la base des mécanismes de base connus relatifs à l'excitation par photoluminescence dans des nanocristaux à semi-conducteurs de taille quantique ainsi à des facteurs qui améliorent l'efficacité de l'émission grâce à une densité modifiée des états photoniques et des processus de transfert d'énergie dans des systèmes à nanocristaux dopés. L'idée a été réalisée sous la forme de structures photoniques de type 'xérogel microporeux / nanocristaux dopés / alumine anodique mésoporeuse', qui confère aux films ainsi obtenus des propriétés modifiées en termes de luminescence et de spectres d'absorption.
PCT/BY2004/000023 2004-09-27 2004-09-27 Convertisseur de lumiere a petite ouverture hautement efficace WO2006034561A1 (fr)

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PCT/BY2004/000023 WO2006034561A1 (fr) 2004-09-27 2004-09-27 Convertisseur de lumiere a petite ouverture hautement efficace
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