WO2022116726A1 - Matériau électroluminescent et dispositif électroluminescent le comprenant - Google Patents

Matériau électroluminescent et dispositif électroluminescent le comprenant Download PDF

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WO2022116726A1
WO2022116726A1 PCT/CN2021/125248 CN2021125248W WO2022116726A1 WO 2022116726 A1 WO2022116726 A1 WO 2022116726A1 CN 2021125248 W CN2021125248 W CN 2021125248W WO 2022116726 A1 WO2022116726 A1 WO 2022116726A1
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light
luminescent material
luminescent
present
emitting material
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Chinese (zh)
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刘荣辉
孙志聪
刘元红
陈晓霞
高彤宇
马小乐
薛原
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有研稀土新材料股份有限公司
河北雄安稀土功能材料创新中心有限公司
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Publication of WO2022116726A1 publication Critical patent/WO2022116726A1/fr

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    • 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
    • C09K11/681—Chalcogenides
    • C09K11/684—Chalcogenides with alkaline earth metals
    • 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
    • C09K11/7715—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing cerium
    • C09K11/7722—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
    • C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
    • C09K11/7736—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
    • C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
    • C09K11/7776—Vanadates; Chromates; Molybdates; Tungstates
    • 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
    • H01L33/504—Elements with two or more wavelength conversion materials

Definitions

  • the present invention relates to the field of light-emitting materials, in particular, to a light-emitting material, a preparation method thereof, and a light-emitting device comprising the same.
  • the broad spectrum from 650 nm to 1050 nm covers the frequency doubling and frequency combination characteristic information of the vibrations of hydrogen-containing groups (OH, NH, CH).
  • the characteristic information of the hydrogen-containing group of the organic molecule in the sample can be obtained, which can be widely used in the field of food detection.
  • the 700-1600nm band broadband or multi-spectrum can be used in medical testing, standard light sources, plant lighting and other fields. The entire near-infrared LED field has huge market application prospects.
  • the near-infrared light-emitting material is the key material, and its luminous performance directly determines the quality of the fluorescence conversion LED.
  • the currently published patent document "Near infrared doped phosphors having an alkaline gallate matrix" discloses that the composition is LiGaO 2 : 0.001Cr 3+ , 0.001Ni 2+ , Under the excitation of ultraviolet light, it can produce near-infrared luminescence between 1000nm and 1500nm, the luminescence spectral range is narrow, and the luminescence intensity is low.
  • Phosphors Ca 3 Sc 2 Si 3 O 12 : Ce 3+ , Nd 3+ can generate near-infrared luminescence between 800nm and 1100nm, and the luminescence intensity is low.
  • Patent literature (Shao Qiyue, Ding Hao, Dong Yan, Jiang Jianqing, a phosphor material for near-infrared LED and its preparation method, CN107573937A) discloses a phosphor material for near-infrared LED, the chemical The composition is MBO 3 : xCr; M is at least one of Sc, Al, Lu, Gd, and Y.
  • the phosphor material provided by the invention can emit near-infrared light with a peak wavelength in the range of 750nm-800nm under blue light excitation.
  • Patent literature (Xie Rongjun, Zeng Huatao, Zhou Tianliang, a non-stoichiometric near-infrared luminescent material and its preparation method, CN109810709A) discloses a phosphor material for near-infrared LEDs, which can be excited at 460nm. It emits infrared light with a peak wavelength of 800nm to 900nm, and the luminous intensity is relatively low.
  • the problem to be solved by the present invention is the deficiencies of the above-mentioned luminescent materials, and one of its objectives is to obtain a luminescent material that can be excited by visible light with a rich wavelength range to generate high-efficiency near-infrared light. Furthermore, another object of the present invention is to provide a device that uses the luminescent material of the present invention to obtain near-infrared luminescence under the excitation of a visible light source.
  • a first aspect of the present invention provides a light-emitting material comprising an inorganic compound containing M element, A element, E element and X element, the M element being selected from Ca, Sr, Ba, La, Lu , at least one of Y, Sc, Gd, and M element cannot be Ca alone, A element is selected from at least one of Hf, Zr, Ti, Ge, Si, Al, Ga, In, E element is selected from O , at least one of N, F, and must contain O, X element is selected from at least one of Cr, Nd, Yb, Er, Ce, Eu, and must contain Cr, Nd, Yb, Er. , the inorganic compound has a perovskite crystal structure.
  • the M element is selected from one or both of Ca, Sr, Ba, La, Lu, Y, Sc, and Gd
  • the A element is selected from Hf, Zr, Ti, Ge, Si, Al, Ga
  • One or both of In E element is selected from one or both of O, N, F
  • X element is selected from one or both of Cr, Nd, Yb, Er, Ce, Eu, but
  • the M element is mainly Sr and Ga, and also contains a very small amount of Ba and/or Ca, which is also within the protection scope of the present invention.
  • the inorganic compound is represented by the composition formula Ma A b E d X x , wherein 0.8 ⁇ a ⁇ 1.2, 0.8 ⁇ b ⁇ 1.2, 2.8 ⁇ d ⁇ 3.2, 0.0001 ⁇ x ⁇ 0.4.
  • the inorganic compound has the same perovskite crystal structure as SrHfO, and has more diverse structures and compositions compared to other structures, which can provide a flexible local coordination environment for luminescent ions, so that excellent luminescent properties can be obtained.
  • the crystal structure of the compound is slightly different from the crystal structure of SrHfO 3 caused by each doping component, forming a CaHfO 3 or BaHfO 3 perovskite crystal structure, or in the middle of them.
  • the inter-evolving perovskite crystal structure is regarded as the protection scope of the present invention.
  • the lower limit of a is selected from 0.8, 0.98, 0.99 or 1.0
  • the upper limit of a is selected from 0.98, 0.99, 1.0 or 1.2
  • the lower limit of b is selected from 0.8, 0.99 or 1
  • the upper limit of b is selected from 0.99, 1 or 1.2
  • the lower limit of d is selected from 2.8, 2.97, 3.005 or 3.01
  • the upper limit of d is selected from 2.97, 3.005, 3.01 or 3.2
  • the lower limit of x is selected from 0.0001, 0.01 or 0.02, and the upper limit of x is selected from 0.01, 0.02 or 0.4.
  • the A element is composed of two elements, A1 and A2, wherein, the A1 element is selected from one of Hf, Zr, Ti, Ge, and Si, the A2 element is selected from one of Al, Ga, and In, and the A2 element
  • the molar ratio to element A is e, 0.005% ⁇ e ⁇ 10%.
  • the lower limit of e is selected from 0.005% or 5%, and the upper limit of e is selected from 5% or 10%.
  • Appropriate doping of Al, Ga, and In elements in element A can cause local microscopic local distortion, change the crystal field strength, and shift the spectrum in short wavelengths.
  • the spectrum of the invention material can be controlled and tuned; in addition, the valence states and ionic radii of Al, Ga, and In elements have a certain similarity with the X element doped ions that play a luminescent role, which can provide more favorable occupancy for the luminescent doped ions , to obtain higher luminous intensity, but the proportion of each constituent element doped in A should be kept in the range of 0.005% ⁇ e ⁇ 10% to prevent the lattice from being strongly twisted and contracted and then destroying the structure of the unit cell; further, A When the elements are Ga and In, the effect is better. As a better one, when e satisfies 3% ⁇ e ⁇ 6%, the luminous intensity of the material is higher.
  • the M element is composed of two elements, M1 and M2, the M1 element is selected from one of Ca, Sr, and Ba, and the M2 element is selected from one of La, Lu, Y, Sc, and Gd. species, the molar ratio of M2 element to M element is f, 0.005% ⁇ f ⁇ 10%.
  • the value of f in this range can not only ensure that the macroscopic and microstructure of the original system will not be affected, but also can adjust the proportion of doping elements in the M element to achieve the purpose of regulating the crystal field where the luminescent center is located, and realizing the purpose of regulating the luminescent spectrum.
  • the M1 element is selected from one of Sr and Ba
  • M2 is selected from one of La, Lu, Y, Sc, and Gd, and has a higher luminous intensity than when the M1 element is Ca.
  • the M element is Sr and La
  • the A element is Hf and Ga. At this time, the structure and light-emitting performance of the light-emitting material are better.
  • the X element is one or two selected from Cr, Ce, and Eu, and Cr element must be contained therein.
  • Cr ion is the luminescent center of the material, which can absorb blue and red light well, and its 3d orbital is regulated by the size of the crystal field. Placing it in a host material with a weak field environment can achieve broadband near-infrared emission.
  • the sensitizers Ce 3+ and Eu 2+ have strong 4f-5d transition absorption characteristics, which can transfer the absorbed energy to Cr ions and effectively enhance the near-infrared luminescence properties.
  • the X elements are Cr and Ce.
  • the Ce element transfers part of the energy to the luminescent center Cr, which can better improve the energy transfer and luminous efficiency, and effectively improve the luminescent properties of the luminescent material.
  • the M element is Sr element
  • the X element is Cr and Ce.
  • the M element when the M element must contain the Sr element, and the A element must contain the Hf element, a suitable occupancy and crystal field can be provided for the luminescent center, which is beneficial to luminescence.
  • the preparation method of the luminescent material in the present invention includes:
  • the raw materials are mixed and sintered to obtain a light-emitting material.
  • the raw materials are preferably oxides, carbonates, nitrates or fluorides of M, A, E, and X elements; the particle size of the raw materials is preferably 2-10 ⁇ m.
  • the sintering conditions include:
  • the sintering temperature is 1200-1600°C, and the sintering time is 2-10 hours.
  • the present invention provides a light-emitting device.
  • the device includes a light source and a light-emitting material.
  • the light-emitting material is any one of the light-emitting materials described above.
  • the light-emitting material in the present invention has strong absorption at 400-540 nm.
  • the excitation light source of the light-emitting device is a semiconductor chip with an emission peak wavelength range of 400-540 nm.
  • the present invention provides a luminescent material that can be excited by a visible light source, especially blue light, to generate high-intensity near-infrared luminescence, and a luminescent device comprising the same.
  • the emission spectrum of the luminescent material can be controllably tuned.
  • Example 1 is the XRD spectrum diagram of the luminescent material in Example 1 of the present invention.
  • Fig. 2 is the excitation emission spectrum diagram of the luminescent material in Example 1 of the present invention.
  • Example 3 is an emission spectrum diagram of a luminescent material in Example 2 of the present invention.
  • Example 4 is an emission spectrum diagram of a luminescent material in Example 3 of the present invention.
  • Example 10 is an emission spectrum diagram of the luminescent material in Example 10 of the present invention.
  • Example 12 is an emission spectrum diagram of the luminescent material in Example 12 of the present invention.
  • Example 7 is an emission spectrum diagram of the luminescent material in Example 14 of the present invention.
  • Example 18 is an emission spectrum diagram of the luminescent material in Example 18 of the present invention.
  • Example 19 is an emission spectrum diagram of the luminescent material in Example 19 of the present invention.
  • Example 21 of the present invention is an emission spectrum diagram of the luminescent material in Example 21 of the present invention.
  • Example 22 of the present invention is an emission spectrum diagram of the luminescent material in Example 22 of the present invention.
  • Example 12 is an emission spectrum diagram of the luminescent material in Example 24 of the present invention.
  • Example 13 is an emission spectrum diagram of the luminescent material in Example 25 of the present invention.
  • FIG. 14 is an emission spectrum diagram of the luminescent material in Example 27 of the present invention.
  • the luminescent material of the present invention can be obtained by the following preparation method, including the following steps:
  • the luminescent material obtained in the comparative example was analyzed by a fluorescence spectrometer, and the material had an emission with a peak wavelength of 780 nm under the excitation of 460 nm blue light, and its relative luminescence intensity was set as 100.
  • Example 1 The luminescent material obtained in Example 1 was detected by X-ray spectroscopy, and its XRD diffraction pattern was consistent with PDF#89-5606, and it was a perovskite-type SrHfO 3 crystal structure, as shown in FIG. 1 .
  • Example 1 was analyzed by a fluorescence spectrometer. The material had a broad spectrum of near-infrared luminescence under the excitation of 460 nm blue light, with a peak wavelength of 1012 nm (as shown in Figure 2) and a relative intensity of 230.
  • SrCO 3 , HfO 2 , Ga 2 O 3 and Cr 2 O 3 having an average particle size of 4.0 ⁇ m were used as raw powders, in order to obtain a compound represented by the composition formula SrGa 0.05 Hf 0.94 O 2.97 Cr 0.01 (the constituent elements are shown in Table 1 ), weigh 40.60% by weight of SrCO 3 , 57.89% by weight of HfO 2 , 1.30% by weight of Ga 2 O 3 , and 0.21% by weight of Cr 2 O 3 raw materials, grind and mix the above raw materials into a crucible, and place them in a crucible under air. Under the atmosphere, sintered in a high-temperature furnace with a temperature of 1400° C.
  • Example 1 The luminescent material obtained in Example 1 was analyzed by a fluorescence spectrometer. The material had a broad spectrum emission of 700-1300 nm under the excitation of 460 nm blue light, with a peak wavelength at 990 nm, as shown in Figure 3, and the relative luminescence intensity was 300.
  • the luminescent material obtained in Example 3 was analyzed by a fluorescence spectrometer. Excited in blue light at 460 nm, the material has multi-spectral luminescence in the near-infrared spectrum, and the strongest peak wavelength is 1069 nm, and its spectrum is shown in Figure 4.
  • the preparation methods and characterization methods of the luminescent materials in Examples 4-38 are the same as those in Example 1, except that according to the composition of the target compound in each example, an appropriate amount of compound is selected for mixing, grinding, appropriate calcination conditions and post-treatment to obtain luminescence. material product.
  • an appropriate amount of compound is selected for mixing, grinding, appropriate calcination conditions and post-treatment to obtain luminescence. material product.
  • FIGS. 5-14 the compositions of Examples 4-38, the peak wavelengths and relative luminescence intensities under excitation by a 460 nm blue light source are shown in Table 3.
  • the embodiment of the present invention can realize the near-infrared light spectrum emission with a peak wavelength of more than 900 nm, and the relative luminous intensity is more than 1.6 times that of the comparative example, which has better performance. It can better make up for the lack of materials with high-efficiency near-infrared broad-spectrum emission above 900 nm and multi-spectral high-efficiency emission, and can adjust the spectrum and luminous intensity through the method of composition adjustment.
  • element A is composed of two elements, A1 and A2, wherein the element A1 is selected from the group consisting of A1 and A2.
  • One of Hf, Zr, Ti, Ge, Si, A2 element is selected from one of Al, Ga, In, and the molar ratio of A2 element to A element is e, and 0.005% ⁇ e ⁇ 10%, when Element A can be used as a charge compensator to compensate for the charge imbalance caused by Cr-substituted lattice ions, effectively improving the luminous intensity; when the value of e is between 3% and 5%, the luminous intensity can be further improved.
  • the M element is composed of two elements, M1 and M2, and the M1 element is selected from one of Ca, Sr, and Ba.
  • the M2 element is selected from one of La, Lu, Y, Sc, and Gd, and the molar ratio of the M2 element to the M element is f, and 0.005% ⁇ f ⁇ 10%.
  • the value of f in this range can not only ensure that the macroscopic and microstructure of the original system will not be affected, but also can adjust the proportion of doping elements in the M element to achieve the control of the crystal field where the luminescence center is located, and to realize the regulation of luminescence spectrum and the improvement of luminescence intensity.
  • M1 element is selected from one of Sr and Ba
  • M2 is selected from one of La, Lu, Y, Sc, Gd, and has a higher luminous intensity than when M1 element is Ca; further, when When f satisfies 3% ⁇ f ⁇ 5.6%, it has better luminous intensity.
  • the Generate charge imbalance introduce an appropriate amount of trivalent ions at the M 2+ position, such as La 3+ , Lu 3+ , Y 3+ , Sc 3+ , Gd 3+ for charge compensation, when 0.8 ⁇ f/(e+x)
  • the purpose of charge compensation can be achieved, and the stability of the crystal structure can be maintained, and the luminous intensity of the corresponding material is higher.
  • the M element is Sr and La
  • the A element is Hf and Ga
  • the peak wavelength of the luminescent material is about 987 nm
  • the relative intensity can reach more than 300, especially after the introduction of Ce, the relative intensity can reach 349.

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  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
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Abstract

Matériau électroluminescent et dispositif électroluminescent le comprenant. Le matériau électroluminescent comprend un composé inorganique. Le composé inorganique contient un élément M, un élément A, un élément E et un élément X, l'élément M étant choisi parmi au moins un élément parmi Ca, Sr, Ba, La, Lu, Y, Sc et Gd et l'élément M ne pouvant pas être Ca seul, l'élément A étant choisi parmi au moins un élément parmi Hf, Zr, Ti, Ge, Si, Al, Ga et In, l'élément E étant choisi parmi au moins un élément parmi O, N et F et devant comprendre O et l'élément X étant choisi parmi au moins un élément parmi Cr, Nd, Yb, Er, Ce et Eu et devant comprendre un élément parmi Cr, Nd, Yb et Er. Le composé inorganique présente une structure cristalline de type pérovskite. Le matériau électroluminescent peut être excité par un spectre de lumière visible pour générer une émission de lumière proche infrarouge et présente une intensité d'émission de lumière relativement élevée.
PCT/CN2021/125248 2020-12-04 2021-10-21 Matériau électroluminescent et dispositif électroluminescent le comprenant WO2022116726A1 (fr)

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CN116376546A (zh) * 2023-03-15 2023-07-04 有研稀土新材料股份有限公司 一种近红外荧光粉及包含该荧光粉的光学装置

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