EP2024466A1 - Procédé de fabrication d'une substance luminescente émettrice en ligne - Google Patents

Procédé de fabrication d'une substance luminescente émettrice en ligne

Info

Publication number
EP2024466A1
EP2024466A1 EP07724998A EP07724998A EP2024466A1 EP 2024466 A1 EP2024466 A1 EP 2024466A1 EP 07724998 A EP07724998 A EP 07724998A EP 07724998 A EP07724998 A EP 07724998A EP 2024466 A1 EP2024466 A1 EP 2024466A1
Authority
EP
European Patent Office
Prior art keywords
phosphor
mol
light source
lighting unit
light
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.)
Withdrawn
Application number
EP07724998A
Other languages
German (de)
English (en)
Inventor
Holger Winkler
Tim Vosgroene
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.)
Merck Patent GmbH
Original Assignee
Merck Patent GmbH
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 Merck Patent GmbH filed Critical Merck Patent GmbH
Publication of EP2024466A1 publication Critical patent/EP2024466A1/fr
Withdrawn legal-status Critical Current

Links

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
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7783—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals one of which being europium
    • C09K11/7794—Vanadates; Chromates; Molybdates; Tungstates
    • 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
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J61/00—Gas-discharge or vapour-discharge lamps
    • H01J61/02—Details
    • H01J61/38—Devices for influencing the colour or wavelength of the light
    • H01J61/42—Devices for influencing the colour or wavelength of the light by transforming the wavelength of the light by luminescence
    • H01J61/44—Devices characterised by the luminescent material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L2224/42—Wire connectors; Manufacturing methods related thereto
    • H01L2224/47—Structure, shape, material or disposition of the wire connectors after the connecting process
    • H01L2224/48—Structure, shape, material or disposition of the wire connectors after the connecting process of an individual wire connector
    • H01L2224/4805—Shape
    • H01L2224/4809—Loop shape
    • H01L2224/48091—Arched
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/80—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected
    • H01L2224/85—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected using a wire connector
    • H01L2224/85909—Post-treatment of the connector or wire bonding area
    • H01L2224/8592—Applying permanent coating, e.g. protective coating
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/10—Details of semiconductor or other solid state devices to be connected
    • H01L2924/11—Device type
    • H01L2924/12—Passive devices, e.g. 2 terminal devices
    • H01L2924/1204—Optical Diode
    • H01L2924/12044—OLED
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
    • H01L2933/0008—Processes
    • H01L2933/0033—Processes relating to semiconductor body packages
    • H01L2933/0041—Processes relating to semiconductor body packages relating to wavelength conversion elements
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/50—Wavelength conversion elements
    • H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
    • H01L33/502—Wavelength conversion materials
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
    • H10K59/30—Devices specially adapted for multicolour light emission
    • H10K59/38—Devices specially adapted for multicolour light emission comprising colour filters or colour changing media [CCM]

Definitions

  • the invention relates to new line emitter phosphors consisting of europium (lll) doped oxides, a process for their preparation, and white-emitting illumination units containing the line emitter phosphor according to the invention. Furthermore, the invention relates to the use of the line emitter phosphor as conversion phosphor for converting the blue or near UV emission into visible white radiation and their use as LED conversion phosphor for white LEDs or so-called color-on-demand applications.
  • the color-on-demand concept is the realization of light of a certain color point with a pcLED using one or more phosphors. This concept is e.g. used to create certain corporate designs, e.g. for illuminated company logos, brands etc.
  • White LEDs are very efficient light sources that consist of a blue electroluminescent chip of essentially InGaN and a phosphor applied over the chip. This is excited by the blue light and performs a wavelength conversion to longer wavelengths. Part of the blue light passes through the phosphor (transmission) and settles additively with the phosphor
  • the phosphors used are, in particular, systems such as garnets, in particular YAG: Ce (emission in the yellow range), and ortho-silicates (emission in the green-yellow to yellow-orange range).
  • Phosphor YOX (Y 2 O 3 : Eu 3+ ).
  • Eu 3+ -based red line-emitting phosphors are known for their very high efficiency and stability, however, these phosphors can not be used in blue LEDs, since an efficient excitation must occur in the UV range (wavelengths smaller than 300 nm) and blue LEDs in the Range from 440 to
  • the red portion in the emitted light of a LED equipped with these phosphors constantly decreases by hydrolysis processes, whereby the color point of the light emitted by the LED changes.
  • hydrolysis products have a corrosive effect and damage the environment of the phosphor, so that the life of the LED is relatively limited.
  • Banding emitter would be the use of red Eu- (lll) -doped line emitter phosphors, first described in the 1960s:
  • Gd 2 (WO 4 ) S Eu 3+
  • Y 2 (MoO 4 ) 3 Eu
  • GdPO 4 Eu
  • Phosphors have a low uniformity with respect to the stoichiometric composition (concentration gradient in particular of the activator Eu 3+ , which can lead to concentration quenching), the particle size and the morphology of the particles. A homogeneous and in particular reproducible coating with these particles on an LED chip is therefore not possible.
  • Object of the present invention is therefore to develop a method which does not have the aforementioned disadvantages. Because white LEDs only become existing lighting technologies
  • LEDs Light bulbs, halogen lamps, fluorescent lamps
  • areas such as Substitute room lighting, traffic and vehicle lighting if red phosphors are available for LEDs that are durable and efficient.
  • the present object can be achieved by reacting the corresponding reactants by wet chemistry and then subjected to a thermal treatment to the red line emitter phosphor.
  • the present invention thus provides a process for
  • M a M b ' M c " M d " EU e 3+ , Sr f 2+ , Ba 9 2+ , Pb h 2+ (I)
  • M is one or more of the elements Li, Na and / or K
  • M ' one or more of the trivalent rare earth metals La, Y and / or Gd,
  • M one or both of the anions MoO 4 2 " , WO 4 2" , M '" equal to a PO 4 3" -Anion, 0.001 ⁇ e ⁇ 20 mol%,
  • the wet-chemical preparation generally has the advantage that the resulting materials have a higher uniformity with respect to the stoichiometric composition, the particle size and the morphology of the particles. As a result, the particles allow a more homogeneous coating on the LED chip and allow very high internal quantum yields.
  • red line emitter phosphors for the preparation of the red line emitter phosphors as starting materials for the mixture of inorganic and / or organic substances such as nitrates, carbonates, bicarbonates, phosphates, carboxylates, alcoholates, acetates, oxalates, halides, sulfates, organometallic compounds,
  • Hydroxides and / or oxides of metals, semimetals, transition metals and / or rare earths are used, which are dissolved and / or suspended in inorganic and / or organic liquids.
  • Nitrates, halides and / or phosphates of the corresponding metals, semimetals, transition metals and / or rare earths are preferably used as starting materials.
  • the metals gadolinium, tungsten, europium, molybdenum, yttrium, phosphorus and / or sodium are preferably used as metals, semimetals, transition metals and / or rare earths.
  • the dissolved or suspended starting materials are heated with a surface-active agent, preferably a glycol, for several hours and the resulting intermediate product at room temperature with an organic precipitating reagent, preferably
  • ethylene glycol is used as the surface-active agent.
  • the dissolved or suspended educts are complexed with a polybasic carboxylic acid, preferably citric acid, and concentrated to dryness after addition of further educt solutions. After a thermal treatment at temperatures between 600 0 C and 1200 0 C results in the red line emitter phosphor as the final product.
  • the dissolved or suspended educts preferably chlorides and complex oxides, such as
  • Molybdate and / or tungstate possibly with the addition of phosphates, in the presence of a weak alkaline solution in the heat.
  • the precipitate is cleaned and dried and then subjected to a thermal treatment at temperatures between 600 and 1200 0 C for several hours, so that the end product of the red line emitter phosphor is formed.
  • the particle sizes were based on
  • SEM images were determined by determining the particle diameters manually from the digitized SEM images.
  • Another object of the invention is a phosphor of the formula I.
  • M a M b ' M c M d ⁇ Eu 8 3+ , Sr f 2+ , Ba 9 2+ , Pb h 2+ (I) where
  • M one or more of the elements Li, Na and / or K, M ' one or more of the trivalent rare earth metals La, Y and / or Gd,
  • M one or both of the anions MoO 4 2 " , WO 4 2" , M '" equal to a PO 4 3" -Anion, 0.001 ⁇ e ⁇ 20 mol%, 0 ⁇ f ⁇ 30 mol%,
  • Another object of the present invention is a phosphor of the
  • Another object of the present invention is a phosphor for converting the blue or near-UV emission of a light emitting element (e.g., semiconductor element such as InGaN or
  • AIInGaN in visible white radiation with high color rendering, wherein the phosphor consists of a mixture of garnet phosphors and the phosphor according to the invention of formula I, prepared by the wet-chemical process according to the invention.
  • the red line emitter has a narrow structured
  • Emission between 590 and 700 nm, more preferably between 600 and 660 nm.
  • garnet phosphors is understood to mean ternary crystalline compositions having a cubic garnet structure, such as YsAl 5 O 12 (YAG), which may be doped with cerium, for example.
  • YAG YsAl 5 O 12
  • Another object of the present invention is a phosphor for converting the blue or in the near UV emission of a light-emitting element (eg semiconductor element) into visible white radiation with high color rendering, wherein the phosphor from a
  • ortho-silicate phosphors means europium (II) -doped phosphors with an ortho-silicate matrix, in particular mixed alkaline earth metal ortho silicates.
  • the red line emitter phosphors according to the invention can generally be mixed with all common garnet and ortho-silicate phosphors which can be taken from the literature (for example William M. Yen et al., Inorganic Phosphors, CRC Press 2004).
  • Another object of the present invention is a lighting unit with at least one primary light source whose emission maximum in the range 190 to 350 nm and / or 365 to 430 nm and / or 430 to 480 nm and / or 520 to 560 nm, wherein the primary
  • Radiation is partially or completely converted into longer-wave radiation by a mixture of conversion phosphors and the inventive emitting europium (III) -activated oxide.
  • this lighting unit is emitting white.
  • the conversion phosphors include garnet phosphors, ortho-
  • Lighting unit emitting white.
  • the light source is a luminescent on ZnO, TCO (transparent conducting oxide), ZnSe or
  • SiC-based compound or even on an organic light-emitting layer based material.
  • the light source is a source which
  • Electroluminescence and / or photoluminescence shows.
  • the light source may also be a plasma or discharge source.
  • the phosphors according to the invention can either be dispersed in a resin (for example epoxy or silicone resin) or, with suitable size ratios, can be arranged directly on the primary light source or can be remote therefrom, depending on the application (the latter arrangement also excludes the "remote phosphor technology”).
  • a resin for example epoxy or silicone resin
  • the advantages of "remote phosphor technology” are known to the person skilled in the art and eg in the following publication: Japanese Journ. of Appl. Phys. VoI 44, no. 21 (2005). L649-L651.
  • Primary light source is realized by a photoconductive arrangement. This makes it possible that the primary light source is installed at a central location and this is optically coupled to the phosphor by means of light-conducting devices, such as light-transmitting fibers. In this way, the lighting requirements adapted lights can only be realized consisting of one or different phosphors, which can be arranged to form a luminescent screen, and a light guide, which is coupled to the primary light source realize. In this way, it is possible to place a strong primary light source at a convenient location for electrical installation and without further electrical wiring, but only by
  • Another object of the present invention is the use of the line emitter phosphor according to the invention for converting the blue or near UV emission into visible white radiation. Furthermore, the use of the phosphors according to the invention for converting the primary radiation into a specific color point according to the "color on demand" concept is preferred.
  • the red line emitter phosphor according to the invention emits almost exclusively a very intense red line in the wavelength range of 610-620 nm, which results from the 5 D 0 ⁇ 7 F 2 transition of the Eu 3 + results.
  • the batch was transferred to a muffle furnace and held at 600 for 5 hours
  • solution 1 2.120 g of lanthanum chloride hexahydrate and 1.467 g of europium chloride hexahydrate are dissolved in 100 ml of demineralized water [solution 1]. At the same time, a solution of 4.948 g of sodium tungstate dihydrate in 100 ml of deionized water is prepared [solution 2]. From solution 1, 100 ml are introduced, to this solution 2 is added dropwise (pH control should be in the range of
  • Fig. 1 Emission spectrum of the phosphor Nao .5 Gdo .3 Euo .2 WO 4
  • Fig. 2 Excitation spectrum of the phosphor Nao. 5 Gdo .3 Euo .2 WO 4
  • Fig.3 Emission spectrum of the phosphor (Gdo .6 Euo .4 ) 2 (WO 4 ) i .5 PO 4
  • Fig. 4 Excitation spectrum of the phosphor (Gdo .6 Euo .4 ) 2 (WO 4 ) i .5 PO 4
  • Fig. 5 shows the schematic diagram of a light-emitting diode with a phosphor-containing coating.
  • the component comprises a chip-type light-emitting diode (LED) 1 as a radiation source.
  • the light-emitting diode is mounted in a cup-shaped reflector, which is held by a Justagerahmen 2.
  • the chip 1 is connected via a flat cable 7 to a first contact 6 and directly to a second electrical contact 6 '.
  • a coating was applied, which is an inventive
  • Conversion luminescent substance contains.
  • the phosphors are used either separately or as a mixture. (List of part numbers: 1 light emitting diode, 2 reflectors, 3 resin, 4 conversion phosphors, 5 diffusers, 6 electrodes, 7 flat cables)
  • the phosphor is dispersed in a binder lens which simultaneously constitutes a secondary optical element and influences the light emission characteristic as a lens.
  • the phosphor is located in a thin layer of binder directly on the LED chip, and a secondary optical element made of a transparent material can be placed on top of it.
  • the conversion phosphor is dispersed in a binder, the mixture filling the cavity.
  • Lens; 4 semiconductor chip means.
  • This design has the advantage of being a flip-chip design whereby a greater portion of the light from the chip can be used for light purposes via the transparent substrate and a reflector on the floor. In addition, the heat dissipation is favored in this design.
  • the conversion phosphor is located on the back side of the LED chip, which has the advantage that the phosphor is cooled via the metallic connections.
  • Fig.15 shows an example of another application, as it is already known in principle from US-B 6,700,322.
  • the phosphor according to the invention is used together with an OLED.
  • the light source is an organic light-emitting diode 31, consisting of the actual organic film 30 and a transparent substrate 32.
  • the film 30 emits in particular blue primary light, generated for example by means of
  • PVK PBD: coumarin (PVK, abbreviation for poly (n-vinylcarbazole); PBD, abbreviation for 2- (4-biphenyl) -5- (4-tert-butylphenyl) -1, 3,4-oxadiazole) ).
  • the emission is partially converted into a yellow, secondarily emitted light by a cover layer formed from a layer 33 of the phosphor according to the invention. so that a white emission is achieved overall by color mixing of the primary and secondary emitted light.
  • the OLED consists essentially of at least one layer of a light-emitting polymer or of so-called small molecules between two electrodes, which consist of materials known per se, such as ITO (abbreviation for
  • Indium tin oxide as an anode and a highly reactive metal, such as Ba or Ca, as the cathode.Also often several layers between the electrodes are used, which either serve as a hole transport layer or serve in the field of small molecules as electron-transport layers Polymers are, for example, polyfluorene or polyspiro materials used.
  • Fig. 16 shows a low-pressure lamp 20 with a mercury-free
  • Gas filling 21 (schematized), which contains an indium filling and a buffer gas analogous to WO 2005/061659, wherein a layer 22 of the phosphors according to the invention is attached.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Luminescent Compositions (AREA)
  • Vessels And Coating Films For Discharge Lamps (AREA)

Abstract

L'invention concerne de nouvelles substances luminescentes émettrices en ligne, leur procédé de fabrication ainsi que des modules d'éclairage en lumière blanche comportant les substances luminescentes émettrices en ligne selon l'invention.
EP07724998A 2006-06-08 2007-05-09 Procédé de fabrication d'une substance luminescente émettrice en ligne Withdrawn EP2024466A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102006027026A DE102006027026A1 (de) 2006-06-08 2006-06-08 Verfahren zur Herstellung eines Linienemitter-Leuchtstoffes
PCT/EP2007/004075 WO2007140853A1 (fr) 2006-06-08 2007-05-09 Procédé de fabrication d'une substance luminescente émettrice en ligne

Publications (1)

Publication Number Publication Date
EP2024466A1 true EP2024466A1 (fr) 2009-02-18

Family

ID=38235250

Family Applications (1)

Application Number Title Priority Date Filing Date
EP07724998A Withdrawn EP2024466A1 (fr) 2006-06-08 2007-05-09 Procédé de fabrication d'une substance luminescente émettrice en ligne

Country Status (9)

Country Link
US (1) US20100171413A1 (fr)
EP (1) EP2024466A1 (fr)
JP (1) JP2009540022A (fr)
KR (1) KR20090026796A (fr)
CN (1) CN101460590A (fr)
CA (1) CA2654495A1 (fr)
DE (1) DE102006027026A1 (fr)
TW (1) TW200804565A (fr)
WO (1) WO2007140853A1 (fr)

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DE102007039260A1 (de) 2007-08-20 2009-02-26 Merck Patent Gmbh LCD-Hintergrundbeleuchtung mit LED-Leuchtstoffen
TWI385834B (zh) * 2009-02-06 2013-02-11 Yu Nung Shen Light emitting diode chip package and manufacturing method thereof
CN101619214B (zh) * 2009-07-31 2013-10-30 中国地质大学（武汉） 一种白钨矿物相红色荧光粉及其制备方法
US8541793B2 (en) * 2010-02-04 2013-09-24 Yu-Nung Shen Light emitting diode device and method for fabricating the same
CN103222026A (zh) 2011-07-04 2013-07-24 松下电器产业株式会社 等离子体显示面板
CN102604633B (zh) * 2012-02-07 2016-04-27 中国科学院福建物质结构研究所 一种四钨酸盐红色荧光粉及其制备方法
WO2013118199A1 (fr) * 2012-02-08 2013-08-15 パナソニック株式会社 Luminophore de type grenat d'yttrium-aluminium
CN104106150A (zh) * 2012-02-08 2014-10-15 松下电器产业株式会社 发光装置
WO2014203483A1 (fr) * 2013-06-21 2014-12-24 パナソニックＩｐマネジメント株式会社 Substance luminophore rouge et dispositif électroluminescent
DE102013109898A1 (de) * 2013-09-10 2015-03-12 Osram Oled Gmbh Organisches lichtemittierendes Bauelement, Verfahren zum Herstellen eines organischen lichtemittierenden Bauelements und Beleuchtungseinrichtung für ein Kraftfahrzeug
TWI575181B (zh) * 2014-09-26 2017-03-21 艾笛森光電股份有限公司 光線發射模組

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Also Published As

Publication number Publication date
JP2009540022A (ja) 2009-11-19
WO2007140853A1 (fr) 2007-12-13
TW200804565A (en) 2008-01-16
CA2654495A1 (fr) 2007-12-13
US20100171413A1 (en) 2010-07-08
DE102006027026A1 (de) 2007-12-13
KR20090026796A (ko) 2009-03-13
CN101460590A (zh) 2009-06-17

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