WO2010143225A1 - Poudre luminescente, son procédé de fabrication, élément luminescent dans lequel la poudre luminescente est utilisée, procédé pour la fabrication dudit élément luminescent et appareil pour la fabrication de poudre luminescente - Google Patents

Poudre luminescente, son procédé de fabrication, élément luminescent dans lequel la poudre luminescente est utilisée, procédé pour la fabrication dudit élément luminescent et appareil pour la fabrication de poudre luminescente Download PDF

Info

Publication number
WO2010143225A1
WO2010143225A1 PCT/JP2009/002596 JP2009002596W WO2010143225A1 WO 2010143225 A1 WO2010143225 A1 WO 2010143225A1 JP 2009002596 W JP2009002596 W JP 2009002596W WO 2010143225 A1 WO2010143225 A1 WO 2010143225A1
Authority
WO
WIPO (PCT)
Prior art keywords
supercritical fluid
light emitting
luminescent powder
crystal silicon
single crystal
Prior art date
Application number
PCT/JP2009/002596
Other languages
English (en)
Japanese (ja)
Inventor
齋藤健一
山村知玄
Original Assignee
国立大学法人広島大学
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 国立大学法人広島大学 filed Critical 国立大学法人広島大学
Priority to PCT/JP2009/002596 priority Critical patent/WO2010143225A1/fr
Publication of WO2010143225A1 publication Critical patent/WO2010143225A1/fr

Links

Images

Classifications

    • 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
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/59—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing silicon
    • C09K11/592—Chalcogenides
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/06—Silicon
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B33/00—Electroluminescent light sources
    • H05B33/10—Apparatus or processes specially adapted to the manufacture of electroluminescent light sources
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B33/00—Electroluminescent light sources
    • H05B33/12—Light sources with substantially two-dimensional radiating surfaces
    • H05B33/14—Light sources with substantially two-dimensional radiating surfaces characterised by the chemical or physical composition or the arrangement of the electroluminescent material, or by the simultaneous addition of the electroluminescent material in or onto the light source

Definitions

  • the present invention relates to a luminescent powder, a manufacturing method thereof, a light emitting element using the luminescent powder, a manufacturing method of the light emitting element, and a manufacturing apparatus of the luminescent powder.
  • Each of the light emitting layers A, B, and C is made of silicon oxide and nanosilicon contained in the silicon oxide.
  • the nanosilicon contained in the light emitting layers A, B, and C has different sizes. More specifically, the nanosilicon included in the light emitting layer A has a size of 1.5 to 2.0 nm, and the nanosilicon included in the light emitting layer B has a size of 2.0 to 2.5 nm.
  • the nanosilicon contained in the light emitting layer C has a size of 2.5 to 3.5 nm.
  • the silicon oxide film is manufactured by a high frequency sputtering method and a heat treatment. More specifically, the silicon oxide film includes an amorphous silicon oxide film a that is the source of the light emitting layer A, an amorphous silicon oxide film b that is the source of the light emitting layer B, and an amorphous silicon oxide film c that is the source of the light emitting layer C.
  • the silicon oxide film includes an amorphous silicon oxide film a that is the source of the light emitting layer A, an amorphous silicon oxide film b that is the source of the light emitting layer B, and an amorphous silicon oxide film c that is the source of the light emitting layer C.
  • the silicon oxide film is formed by sequentially laminating the amorphous silicon oxide films a, b, and c having different amounts of silicon atoms, and the light-emitting layers A and B containing nano-silicones having different sizes by heat-treating the laminated bodies. , C is manufactured.
  • Another object of the present invention is to provide a method for producing a luminescent powder capable of emitting white light.
  • Another object of the present invention is to provide an apparatus for producing a luminescent powder capable of emitting white light.
  • the luminescent powder includes a first step of holding single crystal silicon in a supercritical fluid made of carbon dioxide, and laser ablation in which nano-sized crystal silicon jumps out of the single crystal silicon into the supercritical fluid.
  • a method for producing a luminescent powder includes a first step of holding single crystal silicon in a supercritical fluid made of carbon dioxide, and a nanosize crystalline silicon from single crystal silicon to a supercritical fluid. A second step of irradiating the single crystal silicon with a laser beam having an intensity that causes laser ablation to jump out.
  • At least one of the first and second electrodes is composed of a plurality of electrode pieces.
  • the method for manufacturing a light emitting element includes a first step of manufacturing a plurality of light emitting powders, and a light emitting member made of a plurality of light emitting powders by collecting the plurality of light emitting powders.
  • the first step includes a first sub-step of holding single crystal silicon in a supercritical fluid made of carbon dioxide, and laser ablation in which nano-sized crystal silicon jumps out of the single crystal silicon into the supercritical fluid.
  • the luminescent powder can emit white light.
  • FIG. 1 It is sectional drawing of the luminescent powder by embodiment of this invention. It is the schematic which shows the structure of the manufacturing apparatus of the luminescent powder by embodiment of this invention. It is process drawing which shows the manufacturing method of the luminescent powder shown in FIG. It is a schematic diagram of the luminescent powder deposited on the substrate. It is an optical microscope image of the several luminescent powder arrange
  • FIG. Fig. 4 It is another fluorescence microscope image of the luminescent powder manufactured according to the process shown in FIG. Fig. 4 is a photoluminescence spectrum of a luminescent powder produced according to the process shown in Fig. 3. It is a figure which shows the pressure dependence of the integrated intensity
  • FIG. 1 is a cross-sectional view of a luminescent powder according to an embodiment of the present invention.
  • luminescent powder 10 according to an embodiment of the present invention includes crystalline silicon 1 and silicon oxide 2.
  • the silicon oxide 2 covers the crystalline silicon 1. Therefore, the luminescent powder 10 has a core / shell structure with the crystalline silicon 1 as a core.
  • the crystalline silicon 1 is made of single crystal silicon and has a spherical shape.
  • the crystalline silicon 1 has an average particle diameter of about 2 nm.
  • the silicon oxide 2 is made of silicon dioxide (SiO 2 ) and has an average thickness of about 2 nm. Therefore, the luminescent powder 10 has a spherical shape having a diameter of about 6 nm.
  • FIG. 2 is a schematic diagram showing a configuration of a luminescent powder manufacturing apparatus according to an embodiment of the present invention.
  • the luminescent powder manufacturing apparatus 100 includes a cylinder 20, pipes 21 and 23, a pump 22, a cooler 24, a reaction vessel 25, a laser device 26, a lens 27, and a heater. 28, a thermocouple 29, a temperature detector 30, and a controller 31.
  • the cylinder 20 has a pressure valve 201 and is a siphon type CO 2 cylinder.
  • the cylinder 20 stores gaseous carbon dioxide (CO 2 ).
  • the pipe 21 is an oil-free pipe and supplies CO 2 stored in the cylinder 20 to the pump 22 via the pressure valve 201.
  • the pressure valve 201 is sealed with a CO 2 swelling-resistant material (for example, ethylene propylene rubber, nitrile rubber, and chloropyrene rubber).
  • the pump 22 is manufactured by removing the lubricant. Then, the pump 22 supplies CO 2 supplied from the cylinder 20 via the pipe 21 into the reaction vessel 25 via the pipe 23. In this case, the pump 22 supplies a supercritical fluid composed of CO 2 via the CO 2 piping 23 so that the pressure generated in the reaction vessel 25 within the reaction vessel 25.
  • the lens 27 condenses the laser light emitted from the laser device 26 and irradiates the silicon lump 40 with the condensed laser light through the sapphire window 252. In this case, the lens 27 condenses the laser light so that the energy per pulse is changed from 19 mJ / pulse to 800 mJ / pulse.
  • the silicon lump 40 is made of, for example, a cube having a side length of 1 cm and has a (111) plane orientation.
  • the substrate 50 is made of, for example, carbon (C) or stainless steel. And the board
  • the heater 28 heats the reaction vessel 25 to a temperature at which CO 2 in the reaction vessel 25 becomes a supercritical fluid in accordance with control from the controller 31.
  • the thermocouple 29 detects an electromotive force due to the temperature of CO 2 in the reaction vessel 25 and outputs the detected electromotive force to the temperature detector 30.
  • the temperature detector 30 receives an electromotive force from the thermocouple 29, and detects the temperature T of CO 2 based on the received electromotive force. Then, the temperature detector 30 outputs the detected temperature T to the controller 31.
  • a high-pressure valve is also used in the path for supplying CO 2 from the cylinder 20 to the reaction vessel 25.
  • the high-pressure valve (diaphragm type) is connected to the oil-free valve. Become.
  • the pump 22 supplies CO 2 into the reaction vessel 25 so that the pressure in the reaction vessel 25 is in the range of 4.56 MPa to 14.8 MPa.
  • the heater 28 heats the reaction container 25 so that the temperature T of CO 2 in the reaction container 25 is in the range of 40 ° C. to 50 ° C.
  • the pressure in the reaction vessel 25 is in the range of 4.56 MPa to 14.8 MPa, and the temperature T of CO 2 in the reaction vessel 25 is not less than the critical temperature of 31 ° C., for example, in the range of 40 ° C. to 50 ° C. If it becomes, the CO 2 in the reaction vessel 25 becomes a supercritical fluid.
  • the gaseous CO 2 output from the pump 22 is cooled by the cooler 24 so as to become liquid CO 2.
  • liquid CO 2 is more gaseous CO 2.
  • the pressure of CO 2 in the reaction vessel 25 is easily set to a pressure of 4.56 MPa to 14.8 MPa by the pump 22 because it is easier to pressurize by the pump 22 than 2 . That is, it is for stably producing a supercritical fluid composed of CO 2 .
  • the pressure valve 201 supplies gaseous CO 2 from the cylinder 20 to the pump 22 via the pipe 21, and the pump 22 outputs CO 2 into the pipe 23.
  • the cooler 24 cools gaseous CO 2 to liquid CO 2 .
  • the pump 22 supplies the cooled liquid CO 2 to the reaction vessel 25 so as to have a pressure at which a supercritical fluid is generated in the reaction vessel 25 (step S2).
  • thermocouple 29 detects an electromotive force due to the temperature of CO 2 in the reaction vessel 25 and outputs the detected electromotive force to the temperature detector 30.
  • the temperature detector 30 detects the temperature T of CO 2 in the reaction vessel 25 based on the electromotive force received from the thermocouple 29 and outputs the detected temperature T to the controller 31.
  • the laser device 26 stops the laser beam irradiation (step S5).
  • nano products are grown in the reaction vessel 25 for the growth time determined by the pressure in the reaction vessel 25 (step S6). Due to this growth, crystalline silicon that has jumped into the supercritical fluid is cooled by supercritical CO 2 at the nanosecond to picosecond term scale immediately after laser light irradiation, and emits light while moving downward in the supercritical fluid. The luminescent powder 10 is deposited on the substrate 50. During these periods, the reaction vessel 25 is controlled by the controller 31 so as to have the same temperature.
  • the growth time is 4 to 10 minutes when the pressure in the reaction vessel 25 is 4.56 MPa, and 1 hour when the pressure in the reaction vessel 25 is 11.0 MPa. When the internal pressure is 14.8 MPa, it is 2 hours. These times were determined based on the calculated time for 100 nm particles to sink by 1 cm.
  • the growth time determined by the pressure of the supercritical fluid is generated by the CO 2 in the reaction vessel 25 and the laser ablation.
  • the crystalline silicon is cooled and the luminescent powder 10 is deposited on the substrate 50.
  • the laser device 26 condenses the laser light by the lens 27 and irradiates the silicon lump 40 with the laser light having an intensity of 800 mJ / pulse.
  • the laser device 26 is not limited to this, and the laser device 26 uses laser light having an intensity of 200 mJ / pulse or more, which is a critical intensity at which laser ablation occurs in which nano-sized crystalline silicon jumps out of the silicon mass 40 into the supercritical fluid. What is necessary is just to irradiate the silicon lump 40 via 27.
  • a plurality of luminescent powders 10 forming a network structure were collected and analyzed by EPMA (Electron Probe Micro Analyzer).
  • FIG. 6 is a diagram showing an analysis result by small-angle X-ray scattering. X-ray small angle scattering was measured using CuK ⁇ rays having a wavelength of 1.5 mm.
  • Curve k1 shows the analysis result by X-ray small angle scattering of the luminescent powder 10 manufactured by setting the pressure of the supercritical fluid made of CO 2 to 4.56 MPa. Furthermore, a curve k2 shows the analysis result by X-ray small angle scattering of the luminescent powder 10 manufactured by setting the pressure of the supercritical fluid made of CO 2 to 10.4 MPa. Furthermore, the curve k3 shows a typical spectrum of X-ray small angle scattering.
  • the luminescent powder 10 was composed of Si having a diameter of about 2 nm and SiO 2 having a thickness of about 2 nm. .
  • the luminescent powder 10 emits white light blue as a whole and emits white light in the region indicated by the arrow A.
  • FIG. 9 is another optical microscope image of a plurality of luminescent powders arranged on a stainless steel substrate.
  • the optical microscope image was taken under the same shooting conditions as those of the optical microscope image shown in FIG. Referring to FIG. 9, a product composed of a plurality of luminescent powders 10 is generated. And a product has a projection part.
  • FIG. 10 is another fluorescence microscopic image of the luminescent powder 10 manufactured according to the process shown in FIG.
  • the excitation wavelength of the luminescent powder 10 when a fluorescent microscope image is taken is 325 nm, and the intensity of the excitation light is 20 mW.
  • the fluorescence microscope image was image
  • FIG. 11 is a photoluminescence spectrum of the luminescent powder 10 produced according to the process shown in FIG. In FIG. 11, the horizontal axis represents wavelength (or energy), and the vertical axis represents intensity.
  • the excitation wavelength of the luminescent powder 10 when measuring photoluminescence is 325 nm, and the intensity of the excitation light is 2 mW.
  • a laser beam having a wavelength of 325 nm is irradiated onto the sample by epi-illumination (the intensity of the excitation light immediately before the sample is several tens of ⁇ W), and light emitted from the sample is collected by an ultraviolet-compatible objective lens.
  • the wavelength was dispersed by a single-type spectrometer, and the spectrum was measured by a CCD camera.
  • an instrument function is obtained based on an intensity-corrected light source compliant with the National Institute of Standards and Technology (NIST), and the spectral sensitivity characteristic is calibrated using the device function. The measurement was performed at normal temperature and normal pressure.
  • FIG. 12 is a diagram showing the pressure dependence of the integrated intensity of the emission spectrum.
  • the horizontal axis represents the pressure of the supercritical fluid at the time of manufacturing the luminescent powder 10
  • the vertical axis represents the integrated intensity.
  • Curve k9 shows the pressure dependence of the integrated intensity of the emission spectrum 40 minutes after producing the luminescent powder 10
  • curve k10 shows the emission spectrum two days after producing the luminescent powder 10.
  • the pressure dependence of the integrated intensity is shown
  • the curve k11 shows the pressure dependence of the integrated intensity of the emission spectrum two months after the luminescent powder 10 is manufactured.
  • the integrated intensity of the emission spectrum after 40 minutes from the production of the luminescent powder 10 is substantially constant with respect to the pressure of the supercritical fluid (see curve k9).
  • the luminous powder 10 after two months from the production of the luminous powder 10 has a maximum luminous intensity (integrated intensity) of about 100 times (see curves k9 and k11).
  • the emission intensity can be controlled by controlling the pressure of the supercritical fluid when the luminescent powder 10 is manufactured.
  • the emission intensity (integrated intensity) of the luminescent powder 10 becomes stronger as the elapsed time after the luminescent powder 10 is manufactured becomes longer (see curves k9 to k11).
  • steps S1 to S3 constitute a “first process” for holding single crystal silicon in a supercritical fluid made of carbon dioxide.
  • step S4 by irradiating the silicon lump 40 made of single crystal silicon with laser light having an intensity that causes laser ablation, the nano-sized crystalline silicon jumps out of the silicon lump 40 into the supercritical fluid.
  • Step S4 constitutes a “second step” of irradiating the single crystal silicon with a laser beam having an intensity that causes laser ablation in which nano-sized crystal silicon jumps out of the single crystal silicon into the supercritical fluid.
  • the crystalline silicon jumps out of the silicon lump 40 into the supercritical fluid by laser ablation, and the luminescent powder 10 is manufactured if the jumped crystalline silicon is cooled for an arbitrary time. Even if the sample is taken out before the time elapses, the luminescent powder 10 can be obtained. Therefore, the luminescent powder according to the embodiment of the present invention only needs to be manufactured by the first and second steps described above.
  • FIG. 13 is a cross-sectional view showing the configuration of the light emitting device according to the embodiment of the present invention.
  • a light emitting device 200 according to an embodiment of the present invention includes a transparent substrate 210, a transparent conductive film 220, a conductive polymer 230, a light emitting member 240, and an electrode 250.
  • the transparent substrate 210 is made of a film or glass.
  • the transparent conductive film 220 is made of any material for flexible displays such as ITO (Indium Tin Oxide), SnO 2 , ZnO, and organic EL (Electro Luminescence), and is formed around the transparent substrate 210.
  • the conductive polymer 230 is made of any one of polyacetylene, polyparaphenylene, polyaniline, polythiophene, and polyparaphenylene vinylene.
  • the conductive polymer 230 is disposed between the transparent conductive film 220 and the light emitting member 240 in contact with the transparent conductive film 220 and the light emitting member 240.
  • the light emitting member 240 is composed of a plurality of laminated light emitting powders 10.
  • the light emitting member 240 is disposed between the conductive polymer 230 and the electrode 250 in contact with the conductive polymer 230 and the electrode 250.
  • the light emitting element 200 emits white light when a voltage of 3.82 V is applied between the transparent conductive film 220 and the electrode 250, and a voltage of 3.3 V is generated between the transparent conductive film 220 and the electrode 250.
  • a voltage of 3.82 V is applied between the transparent conductive film 220 and the electrode 250
  • a voltage of 3.3 V is generated between the transparent conductive film 220 and the electrode 250.
  • FIG. 14 is a process diagram showing a method of manufacturing the light emitting device 200 shown in FIG. Referring to FIG. 14, when the manufacture of light emitting element 200 is started, a plurality of light emitting powders 10 are manufactured according to the process shown in FIG. 3 (step S11).
  • step S12 a plurality of luminescent powders 10 are collected and a light emitting member 240 made of the plurality of luminescent powders 10 is manufactured.
  • the light emitting member 240 is bonded to the transparent conductive film 220 by the conductive polymer 230 (step S13).
  • the electrode 250 is formed on the light emitting member 240 by any of sputtering, vapor deposition, and ink jet method (step S14). Thereby, the light emitting element 200 is completed.
  • FIG. 15 is a cross-sectional view showing the configuration of another light emitting device according to the embodiment of the present invention.
  • the light emitting device according to the embodiment of the present invention may be a light emitting device 200A shown in FIG.
  • the region of the light emitting member 240 in contact with the electrode piece 261 emits white light
  • the region of the light emitting member 240 in contact with the electrode piece 262 emits blue light
  • the region of the light emitting member 240 in contact with the electrode piece 263 is green.
  • the region of the light emitting member 240 that emits light and contacts the electrode piece 264 emits red light.
  • the light emitting element 200A is manufactured according to a process of adding a step of patterning the electrode 260 into electrode pieces 261 to 264 by photolithography after step S14 shown in FIG.
  • the electrode 250 may be made of a transparent conductive film such as ITO.
  • the light emitting element 200A may include an n-type or p-type silicon wafer having a carrier concentration of 10 20 cm ⁇ 3 or more, instead of the transparent substrate 210 and the transparent conductive film 220. In this case, the emitted light is emitted in the lateral direction of the light emitting element 200A.
  • the transparent conductive film 220 may be patterned in the same manner as the electrode 260.
  • at least one of the two electrodes disposed on both sides of the light emitting member 240 may be patterned into a plurality of electrode pieces.
  • the light emitting elements 200 and 200A described above are applied to lighting devices and display devices.
  • the luminescence lifetime of silicon nanomaterials is assumed to be on the order of microseconds (in some cases on the order of nanoseconds or picoseconds), considering its size. Therefore, by using the switching circuit, the light emission / flashing becomes quick and the electric follow-up property is good. As a result, the light emitting elements 200 and 200A are more suitable for a moving image display than a liquid crystal display device.
  • the luminescent powder 10 can be applied to an element for photoluminescence (PL).
  • PL photoluminescence
  • the conventional fluorescent lamp mercury is enclosed, and rare earth elements such as eurobium (Eu) and terbium (Tb) are excited by ultraviolet light of the enclosed mercury, and light of three primary colors is mixed to form a white fluorescent lamp. Therefore, when the above-described luminescent powder 10 is used in a fluorescent lamp, it can be used as a substitute for rare earth elements and a white fluorescent lamp can be realized by ultraviolet irradiation.
  • the luminescent powder 10 can also be applied to a plasma display.
  • the luminescent powder 10 is mixed with the ultraviolet transmissive polymer by mixing the luminescent powder 10 with the ultraviolet transmissive polymer together with the solvent, coating the solution on the inner wall of the glass, and then removing the solvent.
  • the structure is solidified on the glass surface.
  • the glass to be solidified may be any material as long as it is a transparent material, and the shape may be either a flat surface or a curved surface. Then, light is emitted from the inside by mercury discharge or rare gas discharge.
  • the reaction vessel 25 holds the silicon lump 40.
  • the reaction vessel 25 may hold a silicon wafer.
  • the silicon wafer is held in the reaction vessel 25 so that the surface thereof is substantially perpendicular to the laser beam.
  • the pump 22, the cooler 24, the heater 28, the thermocouple 29, the temperature detector 30 and the controller 31 generate a supercritical fluid made of CO 2 in the reaction vessel 25. Configure the “generator”.
  • the present invention is applied to a luminescent powder capable of emitting white light.
  • the present invention is also applied to a method for producing a luminescent powder capable of emitting white light.
  • the present invention is applied to a light emitting element using a luminescent powder capable of emitting white light.
  • the present invention is applied to a method for manufacturing a light-emitting element using a luminescent powder capable of emitting white light.
  • the present invention is applied to an apparatus for producing a luminescent powder capable of emitting white light.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Luminescent Compositions (AREA)

Abstract

Selon l'invention, de la poudre luminescente (10) est fabriquée à l'aide d'un premier procédé, dans lequel du silicium monocristallin est maintenu dans un fluide supercritique comportant du dioxyde de carbone, et d'un second procédé, dans lequel de la lumière laser, dont l'intensité donne lieu à une ablation par laser, des cristaux de silicium de dimension nanométrique étant dispersés à partir du silicium monocristallin dans le fluide supercritique, est dirigée sur le silicium monocristallin. Par conséquent, la poudre luminescente (10) comporte du silicium cristallin (1) de forme sphérique, de l'oxyde de silicium (2) recouvrant l'extérieur du silicium cristallin (1). Le diamètre du silicium cristallin (1) est d'environ 2 nm et l'épaisseur de l'oxyde de silicium (2) est d'environ 2 nm. Donc, la poudre luminescente (10) a une forme sphérique dont le diamètre est d'environ 6 nm.
PCT/JP2009/002596 2009-06-09 2009-06-09 Poudre luminescente, son procédé de fabrication, élément luminescent dans lequel la poudre luminescente est utilisée, procédé pour la fabrication dudit élément luminescent et appareil pour la fabrication de poudre luminescente WO2010143225A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/JP2009/002596 WO2010143225A1 (fr) 2009-06-09 2009-06-09 Poudre luminescente, son procédé de fabrication, élément luminescent dans lequel la poudre luminescente est utilisée, procédé pour la fabrication dudit élément luminescent et appareil pour la fabrication de poudre luminescente

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/JP2009/002596 WO2010143225A1 (fr) 2009-06-09 2009-06-09 Poudre luminescente, son procédé de fabrication, élément luminescent dans lequel la poudre luminescente est utilisée, procédé pour la fabrication dudit élément luminescent et appareil pour la fabrication de poudre luminescente

Publications (1)

Publication Number Publication Date
WO2010143225A1 true WO2010143225A1 (fr) 2010-12-16

Family

ID=43308499

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2009/002596 WO2010143225A1 (fr) 2009-06-09 2009-06-09 Poudre luminescente, son procédé de fabrication, élément luminescent dans lequel la poudre luminescente est utilisée, procédé pour la fabrication dudit élément luminescent et appareil pour la fabrication de poudre luminescente

Country Status (1)

Country Link
WO (1) WO2010143225A1 (fr)

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
K.SAITOW: "Gold Nanospheres and Nanonecklaces Generated by Laser Ablation in Supercritical Fluid", THE JOURNAL OF PHYSICAL CHEMISTRY C, vol. 112, 2008, pages 18340 - 18349 *
K.SAITOW: "Silicon Nanoclusters Selectively Generated by Laser Ablation in Supercritical Fluid", THE JOURNAL OF PHYSICAL CHEMISTRY B, vol. 109, 2005, pages 3731 - 3733 *
KEISUKE SATO: "Kashi Hakko Kino o Fuka shita Nano Silicon Ryushi no Seizoho to sono Oyo", ELECTRONIC MATERIALS AND PARTS, vol. 47, no. 11, 2008, pages 81 - 85 *
TOMOHARU YAMAMURA: "Cho Rinkai Ryutaichu deno Tankessho Silicon no Pulse Laser Shosha ni yori Sosei shita Midori.Aka Iro Hakko Silicon Nano Kessho", CSJ: THE CHEMICAL SOCIETY OF JAPAN KOEN YOKOSHU, vol. 88, no. 1, 2008, pages 429 *

Similar Documents

Publication Publication Date Title
US7132692B2 (en) Nanosilicon light-emitting element and manufacturing method thereof
CN104755584B (zh) 紫外光产生用靶、电子束激发紫外光源、以及紫外光产生用靶的制造方法
Guo et al. Aggregation-induced emission enhancement of carbon quantum dots and applications in light emitting devices
US20080191607A1 (en) Phosphor, Method For Producing Same, And Light-Emitting Device Using Same
KR20150079628A (ko) 자외광 발생용 타겟, 전자선 여기 자외광원 및 자외광 발생용 타겟의 제조 방법
Su et al. Understanding and manipulating luminescence in carbon nanodots
Ye et al. CsPbBr3 nanocrystals embedded glass enables highly stable and efficient light-emitting diodes
Wang et al. 2D XANES-XEOL mapping: observation of enhanced band gap emission from ZnO nanowire arrays
Basso et al. On the route towards a facile fluorescent nanodiamonds laser-synthesis
CN103502392B (zh) 紫外光产生用靶、电子射线激励紫外光源、以及紫外光产生用靶的制造方法
Zhao et al. Electrically driven plasmon mediated energy transfer between ZnO microwires and Au nanoparticles
El Jouad et al. Roughness effect on photoluminescence of cerium doped zinc oxide thin films
US8895947B2 (en) Ultraviolet light generating target, electron-beam-excited ultraviolet light source, and method for producing ultraviolet light generating target
Li et al. Electrical-pumping spasing action from cross-stacked microwires
WO2010143225A1 (fr) Poudre luminescente, son procédé de fabrication, élément luminescent dans lequel la poudre luminescente est utilisée, procédé pour la fabrication dudit élément luminescent et appareil pour la fabrication de poudre luminescente
Popovic et al. Continuous wave laser for tailoring the photoluminescence of silicon nanoparticles produced by laser ablation in liquid
JP5339683B2 (ja) 蛍光体膜の多元真空蒸着法を用いた製造方法
Pérez-Díaz et al. Study of silicon rich oxide light emitter capacitors using textured substrates by metal assisted chemical etching
CN104736661A (zh) 紫外光产生用靶、电子束激发紫外光源和紫外光产生用靶的制造方法
WO2010024447A2 (fr) Oxyde de magnésium contenant un centre coloré et film mince constitué d'un tel oxyde, milieu laser à longueur d'onde variable, dispositif laser, et dispositif source de lumière
LIEM et al. Facile synthesis of carbon quantum dots by plasma-liquid interaction method
Noor Microplasmas in ZnO Nano-forests under High Voltage Stress
Liu et al. Single photon emitters in hexagonal boron nitride fabricated by focused helium ion beam
Gelloz et al. Blue phosphorescence in oxidized nano-porous silicon
Khomchenko et al. Laser processing and characterization of ZnS–Cu thin films

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 09845752

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 09845752

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: JP