EP2049617A1 - Led-konversionsleuchtstoffe in form von keramischen körpern - Google Patents

Led-konversionsleuchtstoffe in form von keramischen körpern

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Publication number
EP2049617A1
EP2049617A1 EP07765071A EP07765071A EP2049617A1 EP 2049617 A1 EP2049617 A1 EP 2049617A1 EP 07765071 A EP07765071 A EP 07765071A EP 07765071 A EP07765071 A EP 07765071A EP 2049617 A1 EP2049617 A1 EP 2049617A1
Authority
EP
European Patent Office
Prior art keywords
phosphor
ceramic
phosphor body
sio
ceramic phosphor
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Withdrawn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
EP07765071A
Other languages
German (de)
English (en)
French (fr)
Inventor
Holger Winkler
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 EP2049617A1 publication Critical patent/EP2049617A1/de
Withdrawn legal-status Critical Current

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    • 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
    • C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
    • C09K11/7774—Aluminates
    • 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
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    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
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Definitions

  • the invention relates to a ceramic phosphor body, its preparation by wet-chemical methods and its use as an LED conversion luminescent material.
  • a blue or near UV emitting electroluminescent chip of In (Al) GaN (or in the future also possibly on the basis of ZnO) is coated with a conversion luminescent from the Chip is excitable and emits certain wavelengths.
  • This combination of chip and phosphor is enclosed with a cast or injection molded epoxy, PMMA or other resin housing to protect the combination against environmental impact, rendering the housing material transparent in the visible and in the given conditions (T to 200 C C and high Radiation density and - load by chip and phosphor) should be stable and unchanging.
  • the phosphors are used as micropowder with a broad, production-related size distribution and morphology: After dispersing the phosphors in a matrix of silicones or resins, these are dropped onto the chip or into a reflector cone surrounding the chip or incorporated into the housing mass, wherein the coating takes place with the housing material (packaging, which also includes the electrical contacting of the chip belongs).
  • the phosphor is not plannable, reproducible and homogeneously distributed on / over the chip. The consequence of this is the inhomogeneous emission cone observable in today's LEDs, ie at different angles the LED emits different light. Whereby this behavior is not reproducible to differences between the LEDs of a batch leads, whereby all LEDs are examined and sorted individually (time-consuming binning procedures).
  • DE 199 63 805 describes an LED which is surrounded by a silicone housing or ceramic part, wherein phosphor powder can be embedded in the cover as a foreign component.
  • WO 02/057198 describes the preparation of transparent ceramics such as YAG: Nd, which may be doped with neodymium here. Such ceramics are used as solid-state lasers.
  • DE 103 49 038 describes a luminescence conversion body produced by solid-state diffusion methods based on a polycrystalline ceramic body of YAG, which is brought together with a solution of a dopant. By means of a temperature treatment, the dopant (activator) diffuses into the ceramic body, forming the phosphor.
  • the coating of the ceramic body of YAG with a cerium nitrate solution is carried out by complex, repeated dip-coating (immersion method, CSD).
  • the diameter of the crystallites is 1 to 100 microns, preferably 10 to 50 microns.
  • ceramic luminescence conversion body Disadvantage of such produced via solid-state diffusion method ceramic luminescence conversion body is that on the one hand on the atomic level homogeneous particle compositions are possible because in particular the doping ions are distributed irregularly, resulting in concentration hotspots to the so-called. Concentration quenching (see Shionoya, Phosphor Handbook, 1998, CRC Press). This reduces the conversion efficiency of the phosphor.
  • so-called mixing and firing processes can only produce micron-sized powders which do not have a uniform morphology and a broad particle size distribution. Large particles have greatly reduced sintering activity over smaller sub-micron particles. The ceramic formation is made difficult and further limited by an inhomogeneous morphology and / or broad particle size distribution.
  • the ceramic luminescence conversion body is not directly on the LED chip, but a few millimeters away, no imaging optics can be used.
  • the primary radiation of the LED chip and the secondary radiation of the phosphor thus take place at widely spaced locations.
  • imaging optics such as e.g. are required for car headlights, no homogeneous light, but there are two light sources are shown.
  • Another disadvantage of the above-mentioned ceramic luminescence conversion body is the use of an organic adhesive (e.g., acrylates, styrene, etc.). These are damaged by the high radiation density of the LED chip and the high temperature and lead by graying to the reduction of the light output of the LED.
  • the object of the present invention is therefore to develop a ceramic phosphor body which does not have one or more of the abovementioned disadvantages.
  • the present object can be achieved in that the phosphor is prepared wet-chemically with subsequent isostatic pressing and in the form of a homogeneous, thin and non-porous plate directly on the surface of the chip - A -
  • the present invention thus provides a ceramic phosphor body obtainable by mixing at least two educts with at least one dopant by wet-chemical methods and subsequent thermal treatment to phosphor precursor particles, preferably with a mean diameter of 50 nm to 5 microns, and isostatic pressing.
  • Scattering effects are negligible on the surface of the phosphor body according to the invention, which preferably has the shape of a small plate, because a so-called.
  • Another advantage of the phosphor body according to the invention is that no complex dispersion of the phosphors in epoxies, silicones or resins is necessary.
  • These prior art dispersions include i.a. polymerizable substances and are not storable because of these and other ingredients.
  • the LED manufacturer is able to store ready-to-use phosphors in the form of platelets; Moreover, the application of the phosphor ceramic is compatible with the other process steps of the LED production, while this in the - O ⁇
  • the phosphor bodies according to the invention can also, if not to the highest efficiencies, i. Lumenefficiencies of white LED value is placed, can also be applied directly over a finished, blue or UV LED. This makes it possible to influence the light temperature and the color tone of the light by simply replacing the phosphor plate. This can be done in the simplest way by replacing the chemically identical phosphor substance in the form of differently thick platelets.
  • the following compounds can be selected as the material for the ceramic phosphor bodies, with one or more doping elements being listed in the following notation to the left of the colon and the host compound to the right of the colon. When chemical elements are separated and bracketed by commas, they can optionally be used. Depending on the desired luminescence property of the phosphor body, one or more of the compounds selected can be used:
  • BaAl 2 O 4 Eu 2+ , BaAl 2 S 4 : Eu 2+ , BaB 8 O, 3 : Eu 2+ , BaF 2 , BaFBrEu 2+ , BaFCI: Eu 2+ , BaFChEu 2+ , Pb 2+ , BaGa 2 S 4 : Ce 3+ , BaGa 2 S 4 ) Eu 2+ , Ba 2 Li 2 Si 2 O 7 : Eu 2+ , Ba 2 Li 2 Si 2 O 7 : Sn 2+ , Ba 2 Li 2 Si 2 O.
  • the ceramic phosphor body consists of at least one of the following phosphor materials: (Y, Gd, Lu, Sc, Sm, Tb) 3 (Al, Ga) 5 O 12 ) Ce, (Ca, Sr 1 Ba) 2 SiO 4 ) Eu 1 YSiO 2 N) Ce 1 Y 2 Si 3 O 3 N 4 ) Ce 1 Gd 2 Si 3 O 3 N 4 ) Ce 1 (Y 1 Gd, Tb, Lu) 3 Al 5-x Si x O 12- x N x : Ce, BaMgAl 10 O 17 ) Eu, SrAl 2 O 4 ) Eu, Sr 4 Al 14 O 25 ) Eu, (Ca 1 Sr 1 Ba) Si 2 N 2 O 2 ) Eu, SrSiAl 2 O 3 N 2 ) Eu , (Ca 1 Sr 1 Ba) 2 Si 5 N 8 ) Eu, CaAISiN 3 ) Eu 1 Molybdate, tungstates, vanadates, Group III nitrides,
  • the ceramic phosphor body can be produced industrially, for example, as platelets in thicknesses of a few 100 nm up to about 500 ⁇ m.
  • the platelet extent (length x width) depends on the arrangement.
  • the size of the wafer according to the chip size from about 100 .mu.m * 100 microns to several mm 2 ) with a certain excess of about 10% - 30% of the chip surface with a suitable chip arrangement (eg Flip Chip arrangement) or to choose accordingly. If the phosphor plate is placed over a finished LED, the emerging cone of light is completely covered by the plate.
  • the side surfaces of the ceramic phosphor body can be mirrored with a light or noble metal, preferably aluminum or silver.
  • the mirroring causes no light to emerge laterally from the phosphor body. Lateral exiting light can reduce the luminous flux to be coupled out of the LED.
  • the mirroring of the ceramic phosphor body is carried out in a process step after the isostatic pressing to bars or plates, which may be done before the mirroring a tailor of the rods or plates in the required size.
  • the side surfaces are for this purpose e.g. wetted with a solution of silver nitrate and glucose and then exposed at elevated temperature to an ammonia atmosphere.
  • a silver coating on the side surfaces Alternatively, electroless metallization processes are also suitable, see, for example, Hollemann-Wiberg, Lehrbuch der Anorganischen Chemie, Walter de Gruyter Verlag or Ulimann's Encyclopedia of Chemical Technology.
  • the side facing the chip In order to increase the coupling of the electroluminescent blue or UV light of the LED chip into the ceramic, the side facing the chip must have the smallest possible surface area.
  • the ceramic phosphor over - -
  • Phosphor particles Particles have a large surface area and scatter back a high proportion of the incident light. This is absorbed by the LED chip and the existing components. This reduces the achievable light emission of the LED.
  • the ceramic phosphor body can be applied directly to the chip or the substrate, in particular in the case of a flip-chip arrangement. If the ceramic phosphor body is less or not much more than a wavelength of light away from the light source, near-field phenomena may be effective: the energy input from the light source to the ceramic may be intensified by a process similar to the so-called Forster transfer process.
  • the LED chip facing surface of the phosphor body according to the invention can be provided with a coating which acts anti-reflective with respect to the emitted from the LED chip primary radiation.
  • This coating can also consist of photonic crystals.
  • the phosphor body according to the invention can be fixed with a water glass solution on the substrate of an LED chip.
  • the ceramic phosphor body has a structured (eg pyramidal) surface on the side opposite an LED chip (see FIG. 2).
  • a structured (eg pyramidal) surface on the side opposite an LED chip (see FIG. 2).
  • the structured surface on the phosphor body is produced in that in the isostatic pressing, the pressing tool has a structured pressing plate and thereby embossed a structure in the surface. Structured surfaces are desired when thin phosphor bodies or platelets are to be produced.
  • the pressing conditions are known to the person skilled in the art (see J. Kriegsmann, Technische keramische Werkstoffe, Chapter 4, Deutscher dienst, 1998). It is important that 2/3 to 5/6 of the melting temperature of the material to be pressed are used as pressing temperatures.
  • the ceramic phosphor body according to the invention has a rough surface (see FIG. 2) on the side opposite an LED chip, the nanoparticles of SiO 2 , TiO 2 , Al 2 O 3 , ZnO 2 , ZrO 2 and / or Y 2 ⁇ 3 or combinations of these materials.
  • a rough surface has a roughness of up to several 100 nm.
  • the coated surface has the advantage that total reflection can be reduced or prevented and the light can be better decoupled from the phosphor body according to the invention.
  • the phosphor body according to the invention has a refractive index-adapted layer on the surface facing away from the chip, which facilitates the decoupling of the primary radiation and / or the radiation emitted by the phosphor body.
  • the ceramic phosphor body on the side facing an LED chip has a polished surface in accordance with DIN EN ISO 4287 (Rugotest, polished surface have the roughness class N3-N1). This has the advantage that the surface is reduced, whereby less light is scattered back.
  • this polished surface can also be provided with a coating that is transparent to the primary radiation, but reflects the secondary radiation. Then the secondary radiation can only be emitted upwards.
  • the starting materials for the preparation of the ceramic phosphor body consist of the base material (for example salt solutions of yttrium, aluminum, gadolinium) and at least one dopant (for example cerium).
  • Suitable starting materials are 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 , which are dissolved and / or suspended in inorganic and / or organic liquids. Preference is given to using mixed nitrate solutions which contain the corresponding elements in the required stoichiometric ratio.
  • a further subject matter of the present invention is a process for the production of a ceramic phosphor body with the following process steps: a) Production of a phosphor by mixing at least two educts and at least one dopant by wet-chemical methods and subsequent thermal treatment of the resulting phosphor precursors b) Isostatic pressing of the phosphor precursors into a ceramic phosphor body
  • the wet-chemical preparation generally has the advantage that the resulting materials have a higher uniformity with regard to the stoichiometric composition, the particle size and the morphology of the particles from which the ceramic phosphor body according to the invention is produced.
  • aqueous precursor of the phosphors consisting e.g. from a mixture of yttrium nitrate, aluminum nitrate, cerium nitrate and gadolinium nitrate solution
  • phosphor precursors consisting e.g. from a mixture of yttrium nitrate, aluminum nitrate, cerium nitrate and gadolinium nitrate solution
  • spray pyrolysis also called spray pyrolysis
  • aqueous or organic salt solutions educts
  • the abovementioned nitrate solutions of the corresponding phosphorus are mixed with an NH 4 HCO 3 solution, whereby the phosphor precursor is formed.
  • the abovementioned nitrate solutions of the corresponding phosphor educts are mixed at room temperature with a precipitation reagent consisting of citric acid and ethylene glycol and then heated. Increasing the viscosity causes phosphor precursor formation.
  • Spray pyrolysis belongs to the aerosol processes which are characterized by spraying solutions, suspensions or dispersions into a reaction chamber (reactor) which has been heated in different ways, as well as the formation and separation of solid particles.
  • a reaction chamber reactor
  • the thermal decomposition of the starting materials eg., Salts
  • new materials eg., Oxides, mixed oxides
  • the particle sizes were determined on the basis of SEM images by determining the particle diameters manually from the digitized SEM images.
  • the phosphor precursors are compressed isostatically (at pressures between 1000 and 10000 bar, preferably 2000 bar in an inert, reducing or oxidizing atmosphere or under vacuum) and thereby brought into the appropriate platelet shape.
  • the phosphor precursors are mixed before the isostatic pressing with a 0.1 to 1 wt% sintering aid such as silica or magnesium oxide nanopowder.
  • an additional thermal treatment can be carried out by the pressing at 2/3 to 3 A of its melting temperature in the chamber furnace possibly in reducing or oxidizing reaction gas atmospheres (O 2 , CO, H 2 , HVN 2 , etc), in air or in vacuo is treated.
  • Another object of the present invention is a lighting unit with at least one primary light source whose emission maximum is in the range 240 to 510 nm, wherein the primary radiation is partially or completely converted into longer-wave radiation by the ceramic phosphor body according to the invention.
  • this lighting unit is emitting white
  • the light source is a luminescent compound based on ZnO, TCO (transparent conducting oxide), ZnSe or SiC or else an organic light-emitting layer.
  • Another object of the present invention is the use of the ceramic phosphor body according to the invention for the conversion of blue or in the near UV emission in visible white radiation.
  • the ceramic phosphor body can be used as a conversion phosphor for visible primary radiation for generating white light.
  • the ceramic phosphor body absorbs a certain portion of the visible primary radiation (in the case of non-visible primary radiation, this is to be absorbed altogether) and the remaining portion of the primary radiation is transmitted in the direction of the surface, which the primary light source is opposite.
  • the ceramic phosphor body for the radiation emitted by it is as transparent as possible with respect to the decoupling on the surface emitting the primary radiation emitting material. It is also preferred if the ceramic phosphor body has a ceramic density between 80 and almost 100%.
  • the ceramic phosphor body is characterized by a sufficiently high translucency for the secondary radiation. This means that this radiation can pass through the ceramic body.
  • the ceramic phosphor body preferably has a transmission of more than 60% for the secondary radiation of a specific wavelength.
  • the ceramic phosphor body can be used as conversion phosphor for UV primary radiation for generating white light.
  • the ceramic phosphor body absorbs the entire primary radiation and if the ceramic phosphor body is as transparent as possible for the radiation emitted by it.
  • Example 1 Production of finely powdered (Yo. 98 Ce 0 .o 2 ) 3 Al 5 0 12 via co-precipitation with subsequent pressing and sintering to the phosphor plate
  • the precipitate is allowed to age for about 1 h and then filtered off with suction through a filter. Subsequently, the product is washed several times with deionized water.
  • the precipitate is transferred to the crystallizer and dried in a drying oven at 150 0 C. Finally, the dried precipitate is placed in the smaller corundum crucible, placed in the larger corundum crucible, which contains a few grams of granular activated carbon, and then sealed with the crucible lid. The sealed crucible is placed in the chamber furnace and then calcined at 1000 0 C for 4 h.
  • the fine phosphor powder which consists of the exact chemical stoichiometry with respect to the required cations with the lowest possible impurities (especially heavy metals in each case less than 50 ppm) preferably primary sub-micron primary grain is then in a press at 1000 - 10,000, preferably 2000 bar precompressed in the appropriate platelet form at a temperature of up to 5/6 of its melting temperature. Subsequently, an additional treatment of the compact takes place at 2/3 to 5/6 of its melting temperature in the chamber furnace in Formiergasatmospotrore.
  • Example 2 Preparation of a precursor (precursor particles) of the phosphor (Y 0 0 0 .98Ce 2h AI 5 O 2 via co-precipitation.
  • the pH must be kept at 8-9 by adding ammonia. After about 30 - 40
  • the entire solution should be added, forming a flaky, white precipitate.
  • the precipitate is allowed to age for about 1 h.
  • Example 3 Preparation of a precursor of the phosphor Y2.54iGd 0 , 45oCeo, oo9Al 5 Oi2 via co-precipitation
  • Example 4 Preparation of a precursor (precursor particle) of the phosphor Y2,88Ceo, i2AUOi2 via the pecchini process
  • Example 5 Preparation of a precursor (precursor particle) of the phosphor about the pecchini process
  • Example 7 Preparation of a precursor (precursor particle) of the phosphor Y2.54iGdo, 45oCeo, oo9Al 5 Oi2 by means of combustion method using urea
  • Example 8 Pressing the phosphor particles to a Leuchtstokkkeramik
  • Regarding the required cations with minimal impurities esp. Heavy metals each less than 50 ppm
  • consists of preferably sub-micron large primary grain is then precompressed in a press at 1000 - 10,000, preferably 2000 bar brought into the appropriate platelet form at a temperature of up to 5/6 of its melting temperature.
  • an additional treatment of the compact takes place at 2/3 to 5/6 of its melting temperature in the chamber furnace in Formiergasatmospotrore.
  • Example 9 Compression to a ceramic with the aid of sintering additives and subsequent silvering
  • the precursor particles described in the abovementioned Examples 1 to 7 are hot pressed isostatically using 0.1 to 1% sintering aid (MgO, SiO 2 nanoparticles), first in air, then in a reducing atmosphere of forming gas.
  • 0.1 to 1% sintering aid MgO, SiO 2 nanoparticles
  • the mirroring is carried out as follows:
  • the ceramic phosphor body resulting in the form of rods or platelets after isostatic pressing is wetted on the side surfaces with a solution of 5% AgNO 3 and 10% glucose. At an elevated temperature, the wetted material is exposed to an ammonia atmosphere. This forms a silver coating on the side surfaces.
  • FIG. 2 pyramidal structures 2 can be embossed onto the one surface of the thin ceramic plate by structured pressure plates (top). Without structured pressure plates (lower illustration), nanoparticles of SiO 2 , TiO 2 , ZnO 2 , ZrO 2 , Al 2 O 3 , Y 2 O 3 etc. or mixtures thereof can be applied subsequently on one side (rough side 3) of the ceramic ,
  • FIG. 3 ceramic conversion luminescent body 5 applied to the LED chip 6
  • FIG. 4 SEM photograph of a YAG: Ce fine powder prepared according to Example 1

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KR20090054978A (ko) 2009-06-01
TW200815564A (en) 2008-04-01
CA2660385A1 (en) 2008-02-14
US20100187976A1 (en) 2010-07-29
CN101501160A (zh) 2009-08-05

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