WO2015177327A1 - Del infrarouge - Google Patents

Del infrarouge Download PDF

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Publication number
WO2015177327A1
WO2015177327A1 PCT/EP2015/061351 EP2015061351W WO2015177327A1 WO 2015177327 A1 WO2015177327 A1 WO 2015177327A1 EP 2015061351 W EP2015061351 W EP 2015061351W WO 2015177327 A1 WO2015177327 A1 WO 2015177327A1
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WO
WIPO (PCT)
Prior art keywords
light
phosphor
emitting device
range
metal
Prior art date
Application number
PCT/EP2015/061351
Other languages
German (de)
English (en)
Inventor
Beata MALYASA
Thomas JÜSTEL
Dominik Uhlich
Ines Becker
Helga Bettentrup
Original Assignee
Tailorlux 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 Tailorlux Gmbh filed Critical Tailorlux Gmbh
Priority to CN201580037820.0A priority Critical patent/CN106661447A/zh
Publication of WO2015177327A1 publication Critical patent/WO2015177327A1/fr

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Classifications

    • 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
    • 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
    • C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
    • C09K11/68—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals containing chromium, molybdenum or tungsten
    • C09K11/685—Aluminates; Silicates
    • 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
    • C09K11/7708—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
    • C09K11/7712—Borates

Definitions

  • the invention relates to a light emitting device and the use of the light emitting device.
  • infrared LEDs which so far have a line emission in the infrared range.
  • US 201 0/0320480 A1 describes an ionic converter material for I R LEDs.
  • WO 2012/1 59556 A1 describes a powdered ionic LED material.
  • WO 201 3/169364 A1 describes the microbiological production of ionic spinel.
  • the object of the present invention is to provide a technology with which efficient light sources with broadband emission in the infrared range can be made available.
  • the object underlying the invention is achieved by a light-emitting device which has a broadband infrared light emission comprising a light emitting part and a phosphor capable of absorbing a part of the light emitted from the light emitting part and emitting light of a wavelength different from that of the absorbed light, wherein a) the phosphor in the host lattice has at least one metal or semiconductor element which is not chromium, b) 0, 1 to 10 mol% of the atoms of the at least one metal or semiconductor element of the luminescent substance are replaced by chromium, and c) the luminescent substance is a semiconductor substance selected from borate, aluminate, gallate, germanate, vanadate, oxynitride, sulfide, silicate, sulfate, phosphate, molybdate, tungstate, oxide or mixtures thereof.
  • the light-emitting device is an LED (light-emitting diode).
  • the light-emitting device is provided as described in EP 0 936 682, unless features are described differently in the present description.
  • the phosphor preferably contains at least 75 mol% of the metal atoms Al (aluminum).
  • the phosphor is preferably a borate or aluminate.
  • 0.5 to 3 mol% of the atoms of the at least one metal or semiconductor element of the phosphor are replaced by chromium, particularly preferably exclusively Al atoms by chromium.
  • Chromium is preferably present in the oxidation state 3+. This is well suited since it exhibits high PL quantum yields as an activator ion, for example in aluminates or gallates, and furthermore has an energy level diagram as [Ar] 3d 3 -lon, which on the one hand favors emission transitions in the NI R range and on the other hand Position of these transitions by the crystal field strength D q and the Racah parameter B (covalent character) makes it easy to adjust.
  • a broadband emission in the NI R range for example, 4 T2g - 4 A2g
  • Cr 3+ phosphors are needed, in which the Cr 3+ is in a place with a weak crystal field, for example, a tetrahedral space.
  • Fig. 21 shows a Tanabe-Sugano diagram of a d 3 system (for example, Cr 3+ [Ar] 3d 3 ).
  • the operating temperature of the phosphor is preferably in a range of 1 0 ° C to 400 ° C.
  • the phosphor preferably has the formula
  • M 1 is an alkaline earth metal, transition metal or lanthanide
  • M 2 is an alkaline earth metal
  • M 3 is Al, Ga, In, Ge, or Sc
  • A is an anion
  • m is a number in the range of 1 to 2
  • n is a number in the range of 0 to 1
  • o is a number in the range of 0.9 to 0.999
  • p is a number in Range from 0.001 to 1
  • q is a number in the range of 2 to 1 5
  • r is a number in the range of 3 to 20.
  • the anion preferably has a charge of -2.
  • the anion is preferably selected from borate or oxygen.
  • M 1 is preferably selected from Gd, Y, Lu, Ca, Sr, La or Ba.
  • M 2 is preferably Mg.
  • the number n can then be 1, for example.
  • the phosphor is preferably selected from the group YAl3 (B03) 4, LaAl 3 (B0 3 ) 4, GdAl 3 (B0 3 ) 4, LuAl 3 (B0 3 ) 4 , YGa 3 (B0 3 ) 4 , LaGa 3 (B0 3 ) 4 , GdGa 3 (B0 3 ) 4, LuGa 3 (B0 3 ) 4, Yln 3 (B0 3 ) 4, Laln 3 (B0 3 ) 4, Gdln 3 (B0 3 ) 4, Luln 3 (B0 3 ) 4, YSc 3 (B0 3 ) 4, LaSc 3 (B0 3 ) 4, GdSc 3 (B0 3 ) 4, LuSc 3 (B0 3 ) 4, SrAh 2 0i 9, CaAli20i9, BaAli20i 9, LaMgAln Oi g, Zn 3 Ga2Ge40i4, La 3 GasGeOi4, La5G
  • the phosphor is preferably excited by radiation in the range from 250 to 750 nm, in particular in the range between 400 and 650 nm.
  • the phosphor is preferably located within a luminescence conversion screen (eg, powder layer, ceramic, glass-ceramic, monocrystal, or powder-polymer composite) of the light-emitting device.
  • This luminescence conversion screen may be part of an LED.
  • the phosphor is intended, for example, to convert the spectrum of the light-emitting part (with an emission of, for example, 300-500 nm) into a broadband NI R spectrum.
  • the phosphor is preferably in particulate form.
  • the median d50 of the particle size is preferably in a range of 1 to 20 ⁇ , most preferably in a range of 5 to 8 ⁇ .
  • the particle size can be measured by means of laser scattering. If the diameter is lower, the conversion efficiency can collapse.
  • the phosphor preferably has a high stability with respect to high radiation powers.
  • the radiant power ⁇ in watts is described by DI N 5031 -1 as the quotient of the radiant energy Q and the time t: dQ
  • the determination of these parameters can be done via a power meter.
  • the phosphor has a stability to high radiation powers in so far as that the decrease in the brightness of the phosphor after 1 000 operating hours does not decrease more than 20% of the output power in the endurance test. This stability measurement can be carried out, for example, according to the known methods at 85 ° C. under 85% atmospheric humidity under continuous load with 1 W radiation power (see also LH Cho, G.
  • the phosphor preferably has a chemical resistance, in particular also to water and CO2.
  • the resistance of the converter materials, as well as a complete ready-made LED are, for example, long-term tested by stability tests at 80 ° C and 80% humidity and this influence is evaluated over the duration of the test. Preferably after two days immersion in 5 wt.% Hydrochloric acid no decrease in the radiant power.
  • the phosphor preferably has a high absorption in the emission maximum of the light-emitting part.
  • the reflectance of the phosphor is preferably in a range of 75% to 5%, preferably in a range of 30% to 5%, in the wavelength range of the light emission of the excitation element.
  • the reflection of powders is characterized for example by the diffuse scattering of the particles, so that the reflection within an integrating sphere has to be measured for the determination, so that angle-dependent effects are excluded.
  • the excitation and emission modulator are tuned synchronously and the spectrum of the sample is divided by the spectrum of the white standard (BaS04) (see Luminescence properties of Eu3 + doped tungstates, thesis by Helga Bettentrup, University of Osnabrück, Steinfurt, October 2009).
  • a + T + R 1 with the absorption A, the transmission T and the reflection R.
  • the phosphor preferably has a quantum yield in a range of 30 to 100%, preferably 80% to 100%.
  • the quantum yield is determined according to DI N 5031 -9, under luminescence quantum yield ⁇ ⁇ with
  • At least one further phosphor is present, which is different from the first phosphor.
  • This at least one further phosphor is preferably an aluminate, garnet, silicate, nitride or oxynitride.
  • This at least one further phosphor preferably emits light in a range from 400 to 1800 nm. More preferably at least two further phosphors are present.
  • Figure 23 shows an emission spectrum of a phosphor converted LED made with a yellow garnet phosphor, a red nitride phosphor, and a claimed NI R phosphor.
  • the host lattice of the phosphor is preferably covalent.
  • the covalent character or else nephelauxetic effect can be described, for example, by an electronegativity difference.
  • the electronegativity difference in the host lattice of the phosphor ⁇ is in a range of 0 to 1.5. This can be determined by conventional methods (see L. Pauling, The Nature of the Chemical Bond and the Structure of Molecules and Crystals: An Introduction to Modern Structural Chemistry, Cornell University Press, 1960).
  • the outlying d electrons in the metal atom of the material of the phosphor such as Al are preferably delocalized. This means that the energy difference between the most energetic outboard d orbital and the lowest energy d orbital is preferably between 10,000 to 30,000 cm -1 . This energy difference can be determined by evaluating the fluorescence spectra.
  • the crystal field splitting of the material of the phosphor is preferably low.
  • the crystal field splitting is at most 2 D q derived from the Tanabe-Sugano diagram for d 3 ions ( Figure 21). This is also described in standard textbooks (see JE Huheey, R. Keiter, R. Keiter, Inorganic Chemistry, Principles of Structure and Reactivity, De Gruyter, Berlin, Boston, 2003) and can be demonstrated by calculation but also by practical experiments.
  • the Stokes' shift of the specific material of the phosphor is preferably high.
  • the energy difference between the maximum of the excitation and emission band is referred to for example as Stokes' sche shift.
  • This Stokes' sche shift can be determined by conventional methods.
  • a host lattice with spinel structure or garnet structure may be disadvantageous in certain circumstances, since these have a weak covalent character depending on their composition.
  • Spinel compounds are usually of low covalent character and are more ionic. As a result, spinel structures generally produce line emissions instead of the desired broadband emissions. Spinel compounds are therefore not preferred as the phosphor.
  • the metal or semiconductor element is preferably a metal element.
  • the metal element is replaced by chromium.
  • the at least one metal or semiconductor element is a Group 1 3 element.
  • the at least one metal or semiconductor element has tetrahedral coordination in the host lattice.
  • this is at least one metal or semiconductor element - for example M 3 - Al, Ga, In, Tl, Ge, Zn, Sn or Si and most preferably Al.
  • At least one further metal is present in addition to the at least one metal or semiconductor element and in particular the group 1 3 element.
  • This further metal is preferably selected from alkaline earth metals, transition metals, lanthanides.
  • Particularly suitable elements are those which are stable as redox ions in the oxidation states +2 and +3.
  • the further metal is preferably selected from Mg, Ca, Sr, Ba, Y, Gd, La, Lu or mixtures thereof. From the other metal so for example, two different metals may be present.
  • a further metal Ba and additionally Mg may be present. bandwidth
  • the phosphor preferably emits light having a conversion rate of emitted to absorbed photons of at least 10%.
  • the energy distribution of the emission spectrum must preferably match the application, which is a band width of the emission of at least 10 nm, preferably 50 nm to 100 nm or even greater.
  • the phosphor preferably emits light over a wavelength range having a width of at least 50 nm in a range between 750 nm and 1800 nm, preferably in the range 850 to 1000 nm.
  • the phosphor preferably emits light having an intensity of at least 10% relative to the maximum emission over the entire range of at least 750 nm to 800 nm under otherwise identical conditions.
  • the light emission of the phosphor is given by a relaxation from an excited state with a spin multiplicity 2S + 1 of 4.
  • the phosphor preferably emits between 650 and 1800 nm.
  • the phosphor preferably has a low thermal quenching. This was for example by V. Bachmann et.al. on the basis of (Ca, Sr, Ba) Si202N2: Eu 2+ extensively studied (see verse Bachmann, C. Ronda, O. Oeckler, W. Schnick, A. Meijerink, Colorpoint tuning for (Sr, Ca, Ba. ) Si202N2: Eu2 + for White Light LEDs, Chemistry of Materials (2009) 316-325.).
  • the quantification of the thermal quenching takes place, for example, by the temperature-dependent recording of emission spectra, which, however, also by the consideration of the absolute intensity in the emission maximum can be represented by considering the emission integrals.
  • TQ1 / 2 or also TQ50 describes the intensity at which only 50% of the intensity after warming up of 0 K is present. The sooner the thermal quenching starts, the worse it is for use as a converter material in LED applications, since here the operating temperatures are between 100 and 200 ° C in chip proximity.
  • TQ 50 is preferably at least 400 ° C for the phosphor of the present invention.
  • the object underlying the invention is achieved by a broadband radiator in the near infrared range, which has a light-emitting device according to the invention.
  • the object underlying the invention is achieved by a heat cabin having a broadband radiator according to the invention.
  • the object underlying the invention is achieved by the use of the device according to the invention for the non-invasive determination of blood constituents, analytical purposes, heat therapy, improved wound healing, pain therapy, food monitoring, heat cabins, safety detectors, motion detectors, and detectors in ATMs.
  • X-ray powder diffractograms were measured by conventional methods, measured in reflection on a Rigaku type MiniFlex II powder diffractometer with Bragg-Brentano geometry.
  • the X-ray source was a copper X-ray tube with ⁇ -radiation of wavelength 0, 1 5413 nm with a Tube voltage of 30 kV and a tube current of 10 mA used. All diffractograms were measured in the angular range 2 ⁇ 10 to 80 ° in 0.02 ° increments.
  • Emission spectra were measured by conventional methods as described, for example, by JR Lakowicz in Principles of Fluorescence Spectroscopy (see JR Lakowicz, Principles of Fluorescence Spectroscopy, Edition: 3rd ed., 2006 Corr. 5th printing 2010, Springer, New York, 2010). , The reported emission spectra were recorded on a fluorescence spectrometer from Edinburgh Instruments FLS 920 in a powder sample holder with mirror optics. The spectra were excited at the absorption maximum and measured in the wavelength range from 450 to 1000 nm in 1 nm increments.
  • Excitation spectra were measured by conventional methods as described by J.R. Lakowicz (see J. R. Lakowicz, Principles of Fluorescence Spectroscopy, ed., 3rd Ed., 2006, Corr., 5th printing, 2010, Springer, New York, 2010). All excitation spectra were recorded with a fluorescence spectrometer from Edinburgh Instruments type FLS 920 in the wavelength range between 250 and 650 nm in 1 nm increments. As detection wavelength, the emission maximum of the examined samples was selected.
  • the light-emitting device according to the invention was produced by customary methods and methods, as described, for example, in the exemplary embodiments and the description of EP 0 936 682.
  • the educts were thoroughly mixed in an agate mortar and then transferred to a corundum crucible. In a first calcination step, the mixture was dehydrated for 2 h at 500 ° C. Then it was again crushed and the mixture calcined for 4 h at 1200 ° C, forming the target phase. Show it:
  • Fig. 1 X-ray powder diffraction of Y (Alo.9sCro.02) 3 (603) 4 for Cu
  • Kalpha radiation Fig. 2 Emission spectrum of Y (Alo.98Cro.02) 3 (803) 4 at 425 nm excitation
  • Fig. 3 Excitation spectrum of Y (Alo.98Cro.o2) 3 (BO3) 4 for 720 nm
  • Emission Fig. 4 Reflectance spectrum of Y (Alo.98Cro.o2) 3 (BO3) 4 versus BaSÜ4 as
  • Fig. 4a quench curve of Y (Alo.99Cro.oi) 3 (BO3) 4
  • the educts were thoroughly mixed in an agate mortar and then transferred to a corundum crucible. In a first calcination step, the mixture was dehydrated for 2 h at 500 ° C. Then it was again crushed and the mixture calcined for 4 h at 1200 ° C, forming the target phase. Show it :
  • Fig. 5 X-ray powder diffractogram of Gd (Alo.9sCro.02) 3 (603) 4 for Cu
  • Fig. 6 Emission spectrum of Gd (Alo.9sCro.02) 3 (603) 4 at 420 nm
  • Fig. 7 Excitation spectrum of Gd (Alo.9sCro.02) 3 (603) 4 for 720 nm
  • Emission Fig. 8 Reflectance spectrum of Gd (Alo.9sCro.02) 3 (603) 4 against BaSÜ4 as white standard c) Ba g Alio Oi 7 : Cr (0.1-10%)
  • the educts were thoroughly mixed in an agate mortar and then transferred to a corundum crucible. The mixture was then calcined for 5 hours at 1250 ° C to form the target phase. Show it:
  • Fig. 9 X-ray powder diffractogram of BaMg (Alo.99Cro.oi) ioOi7 for
  • Fig.12 Reflectance spectrum of BaMg (Alo.99Cro.oi) ioOi7 versus BaSÜ4 as white standard
  • the educts were thoroughly mixed in an agate mortar and then transferred to a corundum crucible. Then, the mixture was calcined at 1400 ° C for 5 hours to form the target phase. Show it:
  • Fig. 13 X-ray powder diffractogram of LaMg (Alo.98Cro.o2) Oi9 for
  • the educts were thoroughly mixed in an agate mortar and then transferred to a corundum crucible. Then, the mixture was calcined at 1400 ° C for 5 hours to form the target phase. Show it:
  • Fig. 17 X-ray powder diffractogram of Sr (Alo.9sCro.02) 12019 for Cu
  • FIG. 18 Emission spectrum of Sr (Alo.9sCro.02) 12019 at 420 nm excitation

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Luminescent Compositions (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Power Engineering (AREA)
  • Led Device Packages (AREA)

Abstract

La présente invention concerne un dispositif électroluminescent, ainsi que l'utilisation dudit dispositif électroluminescent.
PCT/EP2015/061351 2014-05-23 2015-05-22 Del infrarouge WO2015177327A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201580037820.0A CN106661447A (zh) 2014-05-23 2015-05-22 红外线led

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102014107321.5A DE102014107321B4 (de) 2014-05-23 2014-05-23 Infrarot LED
DE102014107321.5 2014-05-23

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Publication Number Publication Date
WO2015177327A1 true WO2015177327A1 (fr) 2015-11-26

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CN (1) CN106661447A (fr)
DE (1) DE102014107321B4 (fr)
WO (1) WO2015177327A1 (fr)

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JP7575658B2 (ja) 2020-08-31 2024-10-30 日亜化学工業株式会社 アルカリ土類アルミン酸塩蛍光体、発光装置及びアルカリ土類アルミン酸塩蛍光体の製造方法

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US10971658B2 (en) * 2017-09-28 2021-04-06 Lumileds Llc Infrared emitting device
DE102018213377A1 (de) * 2018-08-09 2020-02-13 Robert Bosch Gmbh Spektrometer und Verfahren zur Kalibrierung des Spektrometers
CN110358537A (zh) * 2019-07-11 2019-10-22 东南大学 一种用于led植物生长灯的深红色荧光粉及其制备方法

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US20030222268A1 (en) * 2002-05-31 2003-12-04 Yocom Perry Niel Light sources having a continuous broad emission wavelength and phosphor compositions useful therefor
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WO2011095530A1 (fr) * 2010-02-04 2011-08-11 Technische Universität Graz Matériau luminescent comprenant du borate double d'yttrium et d'aluminium dopé avec du chrome(iii)

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US20030222268A1 (en) * 2002-05-31 2003-12-04 Yocom Perry Niel Light sources having a continuous broad emission wavelength and phosphor compositions useful therefor
US20100307055A1 (en) * 2007-10-23 2010-12-09 Jack Silver Protection of plastics
WO2011095530A1 (fr) * 2010-02-04 2011-08-11 Technische Universität Graz Matériau luminescent comprenant du borate double d'yttrium et d'aluminium dopé avec du chrome(iii)

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Publication number Priority date Publication date Assignee Title
JP7575658B2 (ja) 2020-08-31 2024-10-30 日亜化学工業株式会社 アルカリ土類アルミン酸塩蛍光体、発光装置及びアルカリ土類アルミン酸塩蛍光体の製造方法

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