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WO2015002139A1 - Luminophore et dispositif électroluminescent - Google Patents

Luminophore et dispositif électroluminescent Download PDF

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Publication number
WO2015002139A1
WO2015002139A1 PCT/JP2014/067369 JP2014067369W WO2015002139A1 WO 2015002139 A1 WO2015002139 A1 WO 2015002139A1 JP 2014067369 W JP2014067369 W JP 2014067369W WO 2015002139 A1 WO2015002139 A1 WO 2015002139A1
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WIPO (PCT)
Prior art keywords
phosphor
light
emission
light emitting
crystal
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Ceased
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PCT/JP2014/067369
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English (en)
Japanese (ja)
Inventor
雄介 武田
亮治 稲葉
小林　学
岡田　拓也
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Denka Co Ltd
Original Assignee
Denki Kagaku Kogyo KK
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Priority to JP2015525204A priority Critical patent/JPWO2015002139A1/ja
Publication of WO2015002139A1 publication Critical patent/WO2015002139A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10H—INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
    • H10H20/00—Individual inorganic light-emitting semiconductor devices having potential barriers, e.g. light-emitting diodes [LED]
    • H10H20/80—Constructional details
    • H10H20/85—Packages
    • H10H20/851—Wavelength conversion means
    • H10H20/8511—Wavelength conversion means characterised by their material, e.g. binder
    • H10H20/8512—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
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
    • C09K11/77348—Silicon Aluminium Nitrides or Silicon Aluminium Oxynitrides
    • 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
    • C09K11/0883—Arsenides; Nitrides; Phosphides

Definitions

  • the present invention relates to a phosphor for an LED (Light Emitting Diode) or an LD (Laser Diode), and a light emitting device using the phosphor. More specifically, the present invention relates to a (Sr, Ca) AlSiN 3 -based nitride phosphor capable of realizing high-luminance red light emission, and a light-emitting device having excellent color rendering properties and luminous efficiency by using the phosphor.
  • a white LED for illumination As a white LED for illumination, a method of obtaining pseudo white light by combining a blue LED chip and a yellow phosphor is widely used.
  • this type of white LED enters the white region as its chromaticity coordinate value, there are few light emitting components such as the red region, so the appearance of the object illuminated by this white LED is illuminated with natural light. It is very different from how an object looks. That is, this white LED is inferior in color rendering, which is an indicator of the naturalness of how an object is viewed.
  • Patent Document 1 discloses a light emitting device that uses a YAG phosphor that emits yellow light, and a nitride and oxynitride phosphor that emits red light in order to supplement the red component of a white LED.
  • Patent Document 2 discloses Eu2 + -activated CaAlSiN 3 .
  • this document describes that a phosphor having an emission peak wavelength shifted to the short wavelength side can be obtained by substituting part of Ca with Sr.
  • this Eu 2+ activated (Sr, Ca) AlSiN 3 -based nitride phosphor has a shorter emission wavelength than the CaAlSiN 3 -based nitride phosphor and has a higher spectral component in the region with high visibility, it has a high brightness white color. It is effective as a red phosphor for LED.
  • the present inventors have intensively studied the composition range and synthesis conditions in the vicinity of Eu 2+ activated (Sr, Ca) AlSiN 3, and as a result, the crystal lattice of the (Sr, Ca) AlSiN 3 crystal phase. Can be narrowed down to the desired range, resulting in a decrease in the emission spectrum in the wavelength band beyond the human visible range, resulting in high-luminosity red with high visibility.
  • the present inventors have found that a red phosphor that emits light can be obtained.
  • the half width of the emission spectrum when excited with light having a wavelength of 455 nm is 72 nm or more.
  • the gist of the phosphor is 86 nm or less.
  • the phosphor of the present invention is a red light emitting phosphor having a peak wavelength ( ⁇ p) of an emission spectrum of 600 nm or more and 635 nm or less when excited with light having a peak in a wavelength range of 250 nm or more and 550 nm or less, particularly blue light of 455 nm.
  • ⁇ p peak wavelength
  • the full width at half maximum is limited to 72 nm to 86 nm.
  • the amount of emission spectrum in a region with low visibility is small, and high-luminance red light emission can be realized.
  • the light-emitting device of the present invention can emit high-luminance white having an excellent balance between color rendering properties and luminous efficiency by using this phosphor.
  • Phosphor according to the present invention have the general formula: M1 represented by a M2 b M3 c M4 d N e O f.
  • M1 is an activator added to the host crystal, that is, an element constituting the luminescent center ion of the phosphor, and is either one or both of Eu and Ce.
  • M1 can be selected according to the required emission wavelength, and is preferably Eu. If the amount of M1 added is too small, sufficient emission peak intensity cannot be obtained. If it is too large, concentration quenching tends to increase and the emission peak intensity tends to decrease, and as a result, a high-luminance phosphor cannot be obtained. . For this reason, the addition amount a of M1 is 0.00001 or more and 0.15 or less.
  • M2 is two or more elements selected from Mg, Ca, Sr, Ba, and Zn, which require Ca and Sr.
  • M3 is one or more elements selected from Al, Ga, In and Sc, and Al is preferable. If the content of M3 is too small, the target phosphor crystal cannot be obtained, and if it is too much, a heterogeneous phase is produced and the yield tends to decrease. For this reason, the content c of M3 is 0.5 or more and 1.5 or less.
  • N is nitrogen and O is oxygen.
  • the N content e is 2.5 or more and 3.0 or less, preferably 2.7 or more and 3.0 or less.
  • the O content f is 0 or more and 0.5 or less, preferably 0.3 or less.
  • the half-value width (FWHM (full width at half maximum)) of the phosphor according to the present invention is too narrow, the color rendering properties tend to decrease, and when it is too wide, the visibility tends to decrease. Therefore, the half width of the emission spectrum when excited with light having a wavelength of 455 nm is 72 nm to 86 nm. A more preferable lower limit of the half width is 75 nm, and a more preferable upper limit of the half width is 82 nm.
  • the main crystal phase preferably has the same structure as the (Sr, Ca) AlSiN 3 crystal phase. Whether or not the main crystal phase of the phosphor has the same structure as the (Sr, Ca) AlSiN 3 crystal can be confirmed by powder X-ray diffraction.
  • the crystal phase present in the phosphor is preferably the single crystal phase, but may contain a different phase as long as the phosphor characteristics are not greatly affected. Examples of the heterogeneous phase having a low influence on the fluorescence characteristics include (Ca, Sr) 2 Si 5 N 8 , ⁇ sialon, and AlN.
  • (Ca, Sr) 2 Si 5 N 8 includes a small amount of Al at the Si site and a small amount of O at the N site as a solid solution.
  • (Ca, Sr) 2 (Si, Al) 5 (N, O) 8 The amount of the different phase is preferably 10% or less in terms of the diffraction line intensity of the other crystal phase with respect to the strongest diffraction line intensity of the crystal phase when evaluated by the powder X-ray diffraction method.
  • the skeletal structure of (Sr, Ca) AlSiN 3 crystal is formed by bonding (Si, Al) —N 4 tetrahedrons, and Ca atoms and Sr atoms are located in the gaps.
  • a red phosphor is obtained.
  • the composition of the phosphor is kept electrically neutral by the overall parameters of Ca and Sr occupancy, Si / Al ratio, and N / O ratio.
  • the emission spectrum shape of a phosphor having a (Sr, Ca) AlSiN 3 crystal as the main crystal phase, that is, the half-value width (FWHM) of the emission peak is influenced by the crystal lattice around Eu 2+ that acts as the emission center.
  • the lattice constant a of the (Sr, Ca) AlSiN 3 crystal preferable for achieving the above half-value width is 9.7995 or more and 9.812 or less
  • the lattice constant b is 5.745
  • the lattice constant c is 5.150 or more and 5.165 or less. If these lattice constants are out of the above range, the emission spectrum is broadened and a red phosphor with low visual sensitivity tends to be formed, or the crystal lattice is distorted and crystal defects tend to occur, resulting in a decrease in emission characteristics.
  • the lattice constant of the crystal lattice varies depending on the Ca and Sr occupancy, Si / Al ratio, N / O ratio parameters, firing temperature, and the like of the above composition.
  • the ratio of the number of Sr atoms to the total number of atoms of Ca and Sr greatly affects the lattice constant of the crystal lattice.
  • the Sr occupation ratio (Sr / (Sr + Ca)) is preferably 0.85 or more and 0.95 or less, more preferably 0.88 or more and 0.94 or less. is there.
  • the peak wavelength ( ⁇ p) of the emission spectrum is too short, the light emission becomes yellowish, sufficient red light emission cannot be obtained, and the peak wavelength ( ⁇ p) of the emission spectrum is not obtained. If it is too long, it tends to emit red light with a dark red color and low visibility. For this reason, it is preferable that the peak wavelength of the emission spectrum when excited with light having a wavelength of 455 nm is 600 nm or more and 635 nm or less.
  • the peak wavelength can be adjusted, for example, by changing the Sr occupancy (Sr / (Sr + Ca)) or the like, and generally the peak wavelength tends to be shorter as the Sr content increases.
  • the phosphor of the present invention is preferably produced by a mixing step of mixing raw materials, a baking step of baking the raw materials after the mixing step, and a pulverizing step of pulverizing the sintered body after the baking step.
  • a mixing step of mixing raw materials a baking step of baking the raw materials after the mixing step
  • a pulverizing step of pulverizing the sintered body after the baking step it is preferable to add an acid treatment step and an annealing step. Impurities remaining on the surface in the acid treatment step can be vaporized and removed from the manufactured phosphor, and the surface layer of the phosphor can be densified in the annealing step.
  • the phosphor of the present invention has a half width limited to a specific range, and therefore can emit red light with high luminance with high luminance.
  • the light emitting device includes the above-described phosphor of the present invention and a light emitting element.
  • a light emitting element an ultraviolet LED, a blue LED, a phosphor lamp alone or a combination thereof can be used.
  • the light emitting element desirably emits light having a wavelength of 250 nm or more and 550 nm or less, and a blue LED light emitting element of 420 nm or more and 500 nm or less is particularly preferable.
  • a phosphor having another emission color can be used in combination.
  • Other phosphors of emission color include a blue emission phosphor, a green emission phosphor, a yellow emission phosphor, and an orange emission phosphor.
  • the phosphor that can be used in combination with the phosphor of the present invention is not particularly limited, and can be appropriately selected according to the luminance, color rendering, and the like required for the light emitting device. By mixing the phosphor of the present invention with phosphors of other emission colors, white having various color temperatures from daylight white to light bulb color can be realized. Examples of the light emitting device include a lighting device, a backlight device, an image display device, and a signal device.
  • the light-emitting device of the present invention can realize high-luminance white light by adopting the phosphor of the present invention and having an excellent balance between luminous efficiency and color rendering.
  • Table 1 shows composition ratios, firing temperatures, light emission characteristics, and lattice constants of the phosphors of Examples and Comparative Examples.
  • the phosphor of Example 1 is a mixing step of mixing raw materials, a baking step of baking the raw material after the mixing step, a pulverizing step of pulverizing the sintered body after the baking step, an acid treatment step, And it manufactured through the annealing process.
  • ⁇ Mixing process> ⁇ -type silicon nitride powder (NP-400 grade manufactured by Denki Kagaku Kogyo Co., Ltd., oxygen content 1.0% by mass) 25.84% by mass, aluminum nitride powder (F grade manufactured by Tokuyama Co., Ltd., oxygen content 0.6% by mass) %) 22.65% by mass and europium oxide powder (RU grade manufactured by Shin-Etsu Chemical Co., Ltd.) 0.78% by mass, and the raw material powder was dry-mixed for 10 minutes with a V-type mixer. In order to make the sizes of the raw materials uniform, among the mixed raw materials, those that passed through a nylon sieve having an opening of 250 ⁇ m were used in the following steps.
  • ⁇ Baking process> The raw material was set in an electric furnace together with the container and baked. Firing is performed using an electric furnace of a carbon heater, and after degassing to a vacuum, the temperature is raised at 5 ° C./min, and the gas is introduced from 500 ° C. at a flow rate of nitrogen gas of 5 liters / min. The heat treatment was performed at 1800 ° C. for 4 hours in a pressurized nitrogen atmosphere. After baking, the container was taken out and left to reach room temperature. The obtained fired body was a loosely agglomerated lump.
  • ⁇ Acid treatment process> The synthetic powder that passed through the sieve was subjected to an acid treatment in which the slurry concentration was added to 2.0 M hydrochloric acid so as to have a slurry concentration of 25% by mass and immersed for 1 hour. After the acid treatment, the hydrochloric acid slurry was stirred for 1 hour while stirring.
  • the boiled synthetic powder was cooled to room temperature and filtered to separate the acid treatment liquid from the synthetic powder.
  • the synthetic powder after the acid treatment liquid separation was left in a dryer set at a temperature in the range of 100 ° C. to 120 ° C. for 12 hours, and after the dried synthetic powder, it was classified into those that passed through a sieve having an opening of 150 ⁇ m. .
  • Phosphor has the general formula of Example 1: M1 a M2 represented by b M3 c M4 d N e O f, M1 is Eu, M2 is Sr and Ca, M3 is Al, M4 is Si, N is nitrogen, O Is oxygen, and each element content a to f and Sr occupancy (Sr / (Sr + Ca)) are the values shown in Table 1. Specifically, the phosphor is represented by Eu 0.008 (Sr, Ca) 0.992 Al 1.0 Si 1.0 N 3.0 , and a to f are 0.00001 ⁇ a ⁇ .
  • the half width of the emission spectrum was 78 nm, and the peak wavelength was 620 nm.
  • the full width at half maximum and the peak wavelength were measured using a spectrofluorometer (F-7000, manufactured by Hitachi High-Technologies Corporation) corrected with rhodamine B and a sub-standard light source.
  • F-7000 spectrofluorometer
  • a solid sample holder attached to the photometer was used, and a fluorescence spectrum at an excitation wavelength of 455 nm was obtained.
  • the phosphor of Example 1 was subjected to powder X-ray diffraction using CuK ⁇ rays using an X-ray diffractometer (D8 ADVANCE manufactured by Bruker AXS Co., Ltd.).
  • the obtained X-ray diffraction pattern was found to have a (Sr, Ca) AlSiN 3 crystal phase and a trace amount of AlN as a heterogeneous phase.
  • the relative luminance (%) was calculated from the product of the fluorescence spectrum and the standard visibility. Other examples and comparative examples described below were also measured under exactly the same conditions as in Example 1, and expressed as relative values with Example 1 as 100%. The acceptable value of relative luminance was 90% or more.
  • Example 2 Compared to the phosphor of Example 1, in Example 2, the Sr occupancy (Sr / (Sr + Ca)) was changed, and in Examples 3 and 4, the Sr occupancy (Sr / (Sr + Ca)) and the firing temperature were changed. changed.
  • Example 5 Compared with the phosphor of Example 1, in Example 5, the values of the contents a to d of the M1 to M4 elements were changed, and in Example 6, the values of the contents a to d of the M1 to M4 elements and the occupation of Sr The rate (Sr / (Sr + Ca)) was changed. In Example 7, the value of the N content e was changed, and in Example 8, the values of the M1, M2 and O contents a, b, and f were changed.
  • Comparative Examples 1 to 3 In Comparative Examples 1 to 3, as shown in Table 1, the values of the contents a to f of the respective elements are the same as in the phosphor of Example 1, but the Sr occupancy (Sr / (Sr + Ca) ) Or the firing temperature was changed.
  • the half-value width of the emission spectrum is limited to 72 nm to 86 nm, so that high-intensity red light emission is achieved. was gotten.
  • the phosphors of Comparative Examples 1 to 3 had a full width at half maximum exceeding the above range, and the relative luminance was extremely low.
  • the half-value width is in a range where the lattice constant a is from 9.795 to 9.812, in which the lattice constant b is from 5.745 to 5.755, and the lattice constant c is 5.150. It has been confirmed that this is achieved when it is in the range of 5.165 or less.
  • the lattice constant a was less than 9.795, the half width was outside the above range.
  • Example 9 Using a phosphor group consisting of the phosphor of Example 1, a green light emitting phosphor, and a blue light emitting phosphor, and a blue light emitting LED chip as a light emitting element, a general shell-type white light emitting device is manufactured. Manufactured. This light-emitting device had higher brightness than the comparative light-emitting device using the phosphor of Comparative Example 1 instead of the phosphor of Example 1. By using this light-emitting device, a high-brightness backlight device, image display device, and signal device could be realized.

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Luminescent Compositions (AREA)
  • Led Device Packages (AREA)

Abstract

La présente invention porte sur : un luminophore en nitrure à base de (Sr, Ca)AlSiN3 pouvant émettre de la lumière rouge avec une luminance élevée ; et un dispositif électroluminescent qui atteint d'excellentes propriétés de rendu de couleur et efficience lumineuse grâce à l'utilisation de ce luminophore. Le luminophore selon la présente invention est caractérisé en ce qu'il est représenté par la formule générale M1aM2bM3cM4dNeOf, dans laquelle : M1 représente un ou plusieurs éléments choisis entre Eu et Ce ; M2 représente deux ou plus de deux éléments choisis parmi Mg, Ca, Sr, Ba et Zn, comprenant essentiellement Ca et Sr ; M3 représente un ou plusieurs éléments choisis parmi Al, Ga, In et Sc ; M4 représente un ou plusieurs éléments choisis parmi Si, Ge, Sn, Ti, Zr et Hf, comprenant essentiellement Si ; N représente l'atome d'azote ; O représente l'atome d'oxygène ; et a-f satisfont aux relations 0,0001 ≤ a ≤ 0,15, a + b = 1, 0,5 ≤ c ≤ 1,5, 0,5 ≤ d ≤ 1,5, c + d = 2, 2,5 ≤ e ≤ 3,0 et 0 ≤ f ≤ 0,5. Ce luminophore est également caractérisé en ce que la largeur à mi-hauteur de son spectre d'émission lorsqu'il est excité par de la lumière ayant une longueur d'onde de 455 nm est de 72 nm à 86 nm (inclus).
PCT/JP2014/067369 2013-07-03 2014-06-30 Luminophore et dispositif électroluminescent Ceased WO2015002139A1 (fr)

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JP2015142056A (ja) * 2014-01-29 2015-08-03 日亜化学工業株式会社 半導体発光装置
JP2015163689A (ja) * 2014-01-29 2015-09-10 日亜化学工業株式会社 蛍光体及びこれを用いた発光装置
JP2016204613A (ja) * 2015-04-28 2016-12-08 デンカ株式会社 赤色蛍光体及び発光装置
JP2016204616A (ja) * 2015-04-28 2016-12-08 デンカ株式会社 赤色蛍光体及び発光装置
JP2017017317A (ja) * 2015-06-30 2017-01-19 日亜化学工業株式会社 発光装置
WO2017128493A1 (fr) 2016-01-29 2017-08-03 江苏博睿光电有限公司 Particules électroluminescentes contenant de l'azote, leur procédé de préparation, corps électroluminescent contenant de l'azote, et dispositif électroluminescent
WO2017128492A1 (fr) 2016-01-29 2017-08-03 江苏博睿光电有限公司 Poudre fluorescente d'oxyde d'azote et son procédé de préparation, corps électroluminescent d'oxyde d'azote et dispositif électroluminescent
US9735323B2 (en) 2015-06-30 2017-08-15 Nichia Corporation Light emitting device having a triple phosphor fluorescent member
JP2017179187A (ja) * 2016-03-31 2017-10-05 デンカ株式会社 赤色蛍光体及び発光装置
WO2018003605A1 (fr) * 2016-07-01 2018-01-04 デンカ株式会社 Procédé de production de substance fluorescente rouge
JP2019019271A (ja) * 2017-07-20 2019-02-07 デンカ株式会社 赤色蛍光体及び発光装置
WO2019073864A1 (fr) * 2017-10-10 2019-04-18 デンカ株式会社 Substance luminescente rouge et dispositif électroluminescent
US10818827B2 (en) 2017-09-28 2020-10-27 Nichia Corporation Light-emitting device
KR20200135858A (ko) 2018-03-29 2020-12-03 덴카 주식회사 적색 형광체 및 발광 장치
CN112135889A (zh) * 2018-05-18 2020-12-25 电化株式会社 红色荧光体及发光装置

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WO2019073864A1 (fr) * 2017-10-10 2019-04-18 デンカ株式会社 Substance luminescente rouge et dispositif électroluminescent
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