WO2023123386A1 - Matériau de lumière rouge profond à base de nitrure, procédé de préparation et dispositif - Google Patents

Matériau de lumière rouge profond à base de nitrure, procédé de préparation et dispositif Download PDF

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WO2023123386A1
WO2023123386A1 PCT/CN2021/143756 CN2021143756W WO2023123386A1 WO 2023123386 A1 WO2023123386 A1 WO 2023123386A1 CN 2021143756 W CN2021143756 W CN 2021143756W WO 2023123386 A1 WO2023123386 A1 WO 2023123386A1
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deep red
precursor
nitride
red light
light material
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PCT/CN2021/143756
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Chinese (zh)
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周天亮
倪国琴
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苏州君诺新材科技有限公司
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Priority to PCT/CN2021/143756 priority Critical patent/WO2023123386A1/fr
Priority to CN202180105271.1A priority patent/CN118414403A/zh
Publication of WO2023123386A1 publication Critical patent/WO2023123386A1/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
    • C09K11/59—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing silicon
    • 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
    • C09K11/64—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing aluminium

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  • the invention relates to the technical field of preparation of luminescent materials, in particular to a nitride deep red light material, a preparation method and a device.
  • Patent Document 1 Cho Xiaodong, Lan Yanting, Chu Qingquan, Zhao Wenxiang, Zhao Peng, Ma Xiaoping, Plant Growth Lamp and Plant Growth System, CN204901494U
  • red/deep red light and blue light have the greatest effect on plant growth.
  • the plant lighting control system includes: a lamp, including: a first LED module; and a second LED module, wherein the spectra emitted by the first LED module and the second LED module are different; and a control module, according to the Lighting conditions are used to control the first LED module and a second LED module.
  • the technical solution for realizing red and blue light with all LEDs also has certain limitations.
  • the life and reliability of red LEDs are not as good as blue LEDs, which will lead to early failure of the device;
  • the operating voltage of red LEDs is different from that of blue LEDs, so the power input control of the technical solution for full LED to realize red and blue light is more complicated;
  • the spectral half-maximum width of a single type of red LED is narrow, and it is difficult to completely cover all the red light components required by plant growth, and increasing the types of red LEDs will reduce the reliability and cost of plant lighting devices.
  • red/deep red fluorescent material As an improved technical solution, using blue light diodes to excite red/deep red fluorescent materials to achieve red and blue light output is currently the most popular plant lighting technology solution. Therefore, it is of great practical significance to develop deep red fluorescent materials suitable for blue light excitation and for plant lighting. Recently, some red/deep red fluorescent material patents have been published, such as patent document 3 (Xiao Siguo, Wang Wenbo, an improved Mn 4+ doped lanthanum calcium tungstate deep red fluorescent material and its preparation method and application, CN109810708B) A Mn 4+ doped lanthanum calcium tungstate deep red fluorescent material is disclosed.
  • the general chemical formula of the fluorescent material is Ca 3-2X-2 YLa 2+2X+2 YW 2-XY Mn X R YO 12 .
  • the material can emit deep red light of 650-800nm, which coincides with the main absorption wavelength (650-760nm) of plant phytochrome PFR.
  • Mn 4+ as the luminescence center of this material, the full width at half maximum of the emission spectrum is less than 20nm, and the concentrated energy distribution area cannot completely cover the needs of plant growth.
  • Patent Document 4 (Yang Xiaoliang, Chen Tiejin, Xiao Siguo, A Broadband Crimson Light Conversion Material and Its Preparation Method, CN106634970A) discloses a broadband deep red light conversion material.
  • the chemical formula of the deep red light conversion material is Li 2 MgTiO 4 : xCr, where 0.003 ⁇ x ⁇ 0.015.
  • the deep red light conversion material has an excitation bandwidth and an emission wavelength at 726nm.
  • the material contains Li, it has poor stability and is not resistant to water, so it is difficult to apply it to plant lighting.
  • Patent document 5 Wang Ting, Xiu Liang, Wang Shaoqing, Yu Xue, Guo Longchao, Li Ziyang, Ma Qianrui, Guo Haihong, a dark red niobate phosphor for agricultural lighting and its preparation method, CN112625684A discloses a
  • the deep red niobate phosphor used for agricultural lighting has a general chemical formula of Ba 2-x LuNbO 6 : x Mn 4+ , where 0 ⁇ x ⁇ 0.02; the red phosphor has broad ultraviolet and blue light absorption, It can produce reflection in the range of 600-800nm, and the luminous center is located at 700nm, and can be applied in white LED lighting and red LED lights for plant growth.
  • Similar to Patent Document 3 since this material uses Mn 4+ as the luminescent center, the FWHM of the emission spectrum is less than 20nm, and the concentrated energy distribution area cannot fully cover the needs of plant growth.
  • Patent document 6 (Xiao Siguo, Long Zheng, a deep red light-emitting fluorescent material for plant cultivation LED that can be excited by ultraviolet light and blue light and its preparation method, CN112760094A) discloses a plant cultivation that can be excited by ultraviolet light and blue light Deep red fluorescent material for LED.
  • the general chemical formula of the fluorescent material is K 0.5 La 0.5 AMgW 1-x O 6 :xMn 4+ , wherein 0.001 ⁇ x ⁇ 0.03, and A is Sr or Ca.
  • the fluorescent material can emit 650-800nm far-red light after being excited by light in the 300-570nm band, which coincides with the main absorption wavelength (650-760nm) of plant phytochrome PFR. Since the material contains K, it has poor stability and is not resistant to water, so it is difficult to apply it to plant lighting.
  • Patent Document 7 (Qiao Juan, Jia Zhen, A Crimson-Near-Infrared Light-Emitting Device, CN113097403A) discloses a deep-red-near-infrared light-emitting device based on a deep-red-near-infrared luminescent quantum dot material. But the instability of quantum dot materials is known to reduce the reliability of devices.
  • Patent document 8 (Li Juan, Li Guanwei, Che Shenglei, Zheng Jingwu, Qiao Liang, Ying Yao, Li Wangchang, Yu Liang, Cai Wei, a manganese-doped deep red phosphor material and its preparation method, CN112480918A) discloses a A deep red phosphor material doped with manganese, its general chemical formula is: A 2-2x CaB' 1-x O 6 :2xR 3+ , xMn 4+ , wherein: A is one of Sr and Ba; B ' is one of Mo and W; R is one of La, Gd, Eu, Y, Sm, Nd and Dy; the value range of x is 0.001 ⁇ x ⁇ 0.130.
  • the phosphor can be used in the field of LED lighting and artificial light sources for plant growth, and patent document 3, etc., because the material uses Mn 4+ as the luminescent center, the half-width of the emission spectrum is less than 20nm, and the area where the energy is concentrated and distributed cannot be completely Cover the needs of plant growth.
  • Patent Document 9 (You Hongpeng, Zhang Liang, Yin Shuwen, A Mn-doped crimson luminescent material for LED plant growth and its preparation method and application, CN113528137A) discloses a Mn4+-doped deep red luminescent material for LED plant growth.
  • the dark red luminescent material for growth has the structural formula: Sr 2 InSb 1-x O 6 : xMn 4+ , where 0.0005 ⁇ x ⁇ 0.015.
  • the emission wavelength range of the deep red luminescent material is within 600-750nm. Similar to Patent Document 3, etc., since this material uses Mn 4+ as the luminescent center, the FWHM of the emission spectrum is less than 20nm, and the concentrated energy distribution area cannot fully cover the needs of plant growth.
  • Patent document 10 (Chang Gui, Li Zhiyong, Zhao Xiaoxia, Wang Yuhua, Seto Xiaojun, Liu Dongwei, Wang Lin, A photoconversion film capable of promoting plant growth and its preparation method and application, CN110698811A) discloses a photoconversion film capable of promoting plant growth Light conversion film.
  • the light conversion film is an Al 2 O 3 :Cr 3+ mixed Y 3 Al 5 O 12 :Ce 3+ light conversion film.
  • the material uses Cr 3+ as the luminescent center
  • Cr 3+ is in a strong crystal field environment
  • the emission spectrum is narrow-band emission
  • the half-maximum width of the emission spectrum is less than 5nm
  • the concentrated energy distribution area cannot completely cover the growth of plants. need.
  • Patent Document 11 (Xia Mao, Zhou Zhi, Zeng Shaobo, Jiang Kuiming, Liu Qingling, A deep red phosphor and its application, CN105154080A) discloses a deep red phosphor with the following molecular formula (M 1-y Ln y ) 14 Al 10-x (Zn 1-z Mg z ) 6 O 35 : xMn 4+ ; where M is one or more of alkaline earth metals Ca, Sr, Ba; Ln is Y, La, Gd, Lu One or more; 0 ⁇ x ⁇ 0.5, 0 ⁇ y ⁇ 0.3, 0 ⁇ z ⁇ 0.2.
  • the fluorescent powder can be excited by light in the wavelength range of 380-520nm, emits far-red light of 650-750nm, can be applied to LED plant growth lamps, improves plant growth efficiency, reduces energy consumption, and saves costs. Similar to Patent Document 3, etc., since this material uses Mn 4+ as the luminescent center, the FWHM of the emission spectrum is less than 20nm, and the concentrated energy distribution area cannot fully cover the needs of plant growth.
  • Patent document 12 discloses a Mn 4+ doped M' x M 2-2x AX
  • M' comprises an alkaline earth metal cation
  • M comprises an alkali metal cation
  • x is in the range of 0-1
  • A comprises a tetravalent cation comprising at least silicon
  • X comprises a monovalent anion comprising at least fluorine .
  • Patent document 13 (Wang Yuhua, Seto Xiaojun, Yan Mengwen, a fluorescent powder for plant growth and its preparation method, CN110157430A) discloses a fluorescent powder for plant growth, whose chemical expression is Y 2-x BaAl 4 - y SiO 12 : xCe 3+ , yCr 3+ ; 0.01 ⁇ x ⁇ 0.05, 0.02 ⁇ y ⁇ 0.3.
  • the excitation spectrum of the phosphor basically covers the entire visible light region, can effectively convert sunlight into red light required by plants, improves the utilization rate of sunlight by plants, and promotes plant growth.
  • its red light emission depends on the luminescence of Cr 3+ , and there is energy transfer from Ce 3+ to Cr 3+ , which leads to low luminous efficiency of the phosphor.
  • Patent document 14 (Shao Qiyue, Shi Meiling, Dong Yan, Jiang Jianqing, A deep red fluorescent powder for LED plant growth lamps and its preparation method, CN110358537A) discloses a deep red fluorescent powder for LED plant growth lamps Material, RX 3 (BO 3 ) 4 :yCr; wherein R is at least one of La, Lu, Gd, Y, and Nd, X is at least one of Al, Ga, and Sc, wherein 0.005 ⁇ y ⁇ 0.2.
  • the fluorescent powder can be effectively excited by blue light, and emit deep red and near-infrared light in the range of 650nm to 900nm.
  • the main peak of the emission spectrum of the fluorescent material is above 740nm, and the matching degree with the main absorption wavelength (650-760nm) of the plant phytochrome PFR is low.
  • Patent document 15 discloses a nitride-based deep red phosphor: the phosphor has the general formula M a M b B c (N, D): Eu 2+ , wherein M a is a divalent alkaline earth metal such as Mg, Ca, Sr, Ba; M b is a trivalent metal such as Al, Ga, Bi, Y, La and Sm; and M c is a tetravalent element such as Si, Ge, P and B; N is nitrogen and D is a halogen such as F, Cl or Br. Since the material contains halogen, the corrosion of the halogen will lead to accelerated failure of the silver wire and the reflective bowl in the packaged device.
  • M a is a divalent alkaline earth metal such as Mg, Ca, Sr, Ba
  • M b is a trivalent metal such as Al, Ga, Bi, Y, La and Sm
  • M c is a tetravalent element such as Si, Ge, P and B
  • N
  • Patent document 16 (Xia Zhiguo, Liu Gaochao, A near-infrared luminescent material and its preparation method and conversion-type LED light-emitting device, CN112251226A) discloses a near-infrared luminescent material, which contains the general formula A x B y C z O Inorganic compound of q D p , A is Li or Na, B is In, Lu, Sc, Ga, Al, Zr, Ti, Hf, Sn or Ge element, C is Sb, Nb, Ta, Zr, Ti, Hf, Sn or Ge element, O is oxygen element, D is Mn, Cr, Ni, Bi, Pr, Nd, Tm, Eu, Yb, Er or Ho element; 0.8 ⁇ x ⁇ 1.2, 1.5 ⁇ y ⁇ 2, 0.5 ⁇ Z ⁇ 1, 5 ⁇ q ⁇ 7, 0 ⁇ p ⁇ 0.2.
  • the material contains Li, it has poor stability and is not resistant to water, so it is difficult to apply it to plant lighting.
  • Patent Document 17 (Xia Zhiguo, Yang Zhiyu, Gallate Red Fluorescent Material and Preparation Method and White LED Light-Emitting Device, CN112480924A) discloses a gallate red fluorescent material whose chemical formula is Sr 2 Sc 0.5 Ga 1.5 O 5 :xEu 2+ , where 0.02 ⁇ x ⁇ 0.15. Although the luminous efficiency of this material is high, the raw material contains volatile Ga 2 O 3 , which can easily lead to deviations in the chemical composition of the material, so the synthesis of this material is difficult; and the thermal quenching characteristics of this material are relatively poor.
  • Non-patent document 1 Zhiyu Yang, Yayun Zhou, Jianwei Qiao, Maxim S.Molokeev, Zhiguo Xia, Rapid Synthesis of Red-Emitting Sr 2 Sc 0.5 Ga 1.5 O 5 : Eu 2+ Phosphors and the Tunable Photoluminescence Via Sr/Ba Substitution, Advanced Optical Materials, DOI: 10.1002/adom.202100131).
  • Patent Document 18 (Xia Zhiguo, Yang Zhiyu, A Red Phosphor Powder Excited by Blue Light and Its Preparation Method, CN113416542A) discloses a technical solution of using the oxide SrLaScO4 as the phosphor matrix and doping Eu 2+ to achieve red light emission , and by adding S-containing compounds as additives in the synthesis process, it can effectively promote the reduction of Eu 3+ to Eu 2+ to a greater extent, so as to increase the actual content of Eu 2+ in the phosphor, thereby improving the luminous efficiency of the red phosphor. Because S powder is added during the synthesis process, and S powder is extremely corrosive to the silica gel used in packaging the device, which will inevitably lead to a decrease in the reliability of the packaged device.
  • Patent document 19 discloses that the structural formula is ZnGa 2- x O 4 : xCr 3+ Far-red fluorescent material, wherein, 0.002 ⁇ x ⁇ 0.0016.
  • the raw material contains volatile Ga 2 O 3 , it is very easy to cause deviations in the chemical composition of the material, so the synthesis of the material is difficult.
  • Patent document 20 Wang Dajian, Li Guanghao, Mao Zhiyong, Song Weiwei, Sun Taolu, Zhijuan, a fluorescent glass-ceramic for plant laser lighting and its preparation method, CN104402231B discloses a fluorescent glass-ceramic for plant laser lighting. It consists of a glass matrix and a red fluorescent powder, wherein the content of the red fluorescent powder is 5-30 wt%, and the balance is the glass matrix.
  • Such a high preparation temperature and holding time will lead to oxidation of the fluorescent material and reduce the luminous intensity of the final fluorescent glass-ceramic.
  • the first object of the present invention is to protect a nitride deep red light material.
  • the general chemical formula of the nitride deep red light material is: La 2 BaSiAl 2-x Cr x N 6 , where 0 ⁇ x ⁇ 0.2; under the excitation of blue light, the main peak of emission wavelength produced by the deep red light material is The range is between 680-730nm, and the half-maximum width of the emission spectrum is greater than or equal to 180nm.
  • x 0.02; optionally, the luminous intensity of the nitride magenta material at 200°C is not less than 50% of the luminous intensity at room temperature %.
  • the second object of the present invention is to provide a method for preparing a nitride deep red light material.
  • the preparation method comprises: mixing La precursors, Ba precursors, Si precursors, Al precursors and Cr precursors, and performing a high-temperature solid-state reaction in a reducing atmosphere to obtain a nitride deep red light material.
  • the molar ratio of La precursor, Ba precursor, Si precursor, Al precursor and Cr precursor is 2:1:1:(2-x):x
  • the chemical formula of the obtained material is: La 2 BaSiAl 2-x Cr x N 6 , where 0 ⁇ x ⁇ 0.2.
  • the present invention also provides a deep red fluorescent glass and a preparation method thereof.
  • the deep red fluorescent glass is obtained by mixing the nitride deep red material with glass powder and performing a high-temperature solid-state reaction. Specifically, in the air Under the atmosphere, a high-temperature solid-phase reaction is carried out, the temperature of the high-temperature solid-phase reaction is 450-550° C., and the time of the high-temperature solid-phase reaction is 0.1-1 h.
  • the present invention also provides a red light device for plant growth, the device includes a blue light diode and a light emitting layer, and the light emitting layer includes the deep red fluorescent glass.
  • a nitride deep red light material the general chemical formula of the material is:
  • x 0.02.
  • the second object of the present invention is to provide a method for preparing a nitride deep red light material.
  • the preparation method is as follows:
  • La precursor, Ba precursor, Si precursor, Al precursor and Cr precursor are mixed, under reducing atmosphere, carry out high-temperature solid phase reaction, obtain described nitride deep red light material.
  • the molar ratio of La, Ba, Si, Al and Cr in the La precursor, Ba precursor, Si precursor, Al precursor and Cr precursor is 2:1:1:(2-x) :x.
  • the La precursor is selected from LaN; optionally, the Ba precursor is selected from Ba 3 N 2 ; optionally, the Si precursor is one or more of Si and Si 3 N 4 species, wherein Si is necessary; optionally, the Al precursor is AlN; optionally, the Cr precursor is CrN.
  • the purity of La precursor, Ba precursor, Si precursor, Al precursor and Cr precursor is not lower than 99.5wt%.
  • the temperature of the high-temperature solid-state reaction is between 1000°C and 1200°C, and the time for the high-temperature solid-state reaction is between 4 and 10 hours under a reducing atmosphere.
  • the invention also protects a fluorescent glass based on nitride deep red light material.
  • the production method is as follows: the nitride deep red light material is mixed with glass powder, and then subjected to a high-temperature solid-state reaction under nitrogen atmosphere to obtain the nitride deep red light fluorescent glass.
  • the mass ratio of the nitride magenta material to the glass frit is 1:1 ⁇ 1:2.
  • the melting point of the glass powder is 450-550°C.
  • the temperature for the high-temperature solid-state reaction between the nitride magenta material and the glass frit is 450-550° C.
  • the time for the high-temperature solid-state reaction is 0.1-1 h.
  • the invention also protects a light-emitting device made of fluorescent glass based on nitride deep red light material.
  • the light emitting device includes a blue light diode and a light emitting layer, the light emitting layer includes the nitride deep red fluorescent glass, and the light emitting layer is excited by the blue light diode to emit deep red light.
  • the present invention provides a nitride deep red light material and its preparation method and application.
  • the general chemical formula of the nitride deep red light material is La 2 BaSiAl 2-x Cr x N 6 , where 0 ⁇ x ⁇ 0.2; Under the excitation of blue light, the main peak of emission wavelength produced by the deep red fluorescent material is in the range of 680-730nm, and the half-maximum width of the emission spectrum is greater than or equal to 180nm.
  • a nitride deep red light material prepared by the present invention has a brand-new chemical composition, a wide emission spectrum, good thermal quenching characteristics, and stable chemical properties, so that the light-emitting material can be used in Plant lighting industry.
  • Fig. 1 is the emission spectrogram of the luminescent material obtained in Example 3 of the present invention.
  • Fig. 2 is the excitation spectrum diagram of the luminescent material obtained in Example 3 of the present invention.
  • the general chemical formula of the nitride deep red light material is as follows:
  • the x is preferably 0.001, and the precursor of Si is preferably Si; in some embodiments provided by the present invention, the x is preferably 0.005, and the precursor of Si is preferably Si; In some embodiments provided by the present invention, the x is preferably 0.02, and the precursor of Si is preferably Si; in some embodiments provided by the present invention, the x is preferably 0.04, and the precursor of Si is preferably Si; In some embodiments provided by the present invention, the x is preferably 0.08, and the precursor of Si is preferably Si; in some embodiments provided by the present invention, the x is preferably 0.1, and the precursor of Si is preferably Si; In some embodiments provided by the present invention, the x is preferably 0.15, and the precursor of Si is preferably Si; in some embodiments provided by the present invention, the x is preferably 0.2, and the precursor of Si is preferably Si; In some embodiments provided by the present invention, the x is preferably 0.02, and the precursor of
  • the La precursor, the Ba precursor, the Si precursor, the Al precursor and the Cr precursor are mixed, and a high-temperature solid-state reaction is carried out under a reducing atmosphere to obtain a nitride deep red light material.
  • the molar ratio of La, Ba, Si, Al and Cr is 2:1:1:(2-x):x, and the general chemical formula of the obtained material is: La 2 BaSiAl 2-x Cr x N 6 , Among them, 0 ⁇ x ⁇ 0.2.
  • the La precursor is selected from LaN; the Ba precursor is selected from Ba 3 N 2 ; the Si precursor is one or more of Si and Si 3 N 4 , wherein Si is necessary; the Al precursor is AlN; Cr precursor is CrN.
  • the purity of the La precursor, Ba precursor, Si precursor, Al precursor and Cr precursor is not lower than 99.5%. The higher the purity, the less impurities in the obtained luminescent material.
  • the reducing atmosphere can be ammonia gas or nitrogen-ammonia gas mixture (dry) atmosphere well known to those skilled in the art, wherein the volume content of nitrogen in the nitrogen-ammonia gas mixture is 25% to 75%, and there is no special requirement for others. Restrictions, ammonia is preferred in the present invention.
  • the temperature of the high-temperature solid phase in the step is preferably 1000-1200°C, and the atmosphere is ammonia gas. In some embodiments provided by the present invention, the temperature of the high-temperature solid phase is preferably 1100°C.
  • the high-temperature solid-phase time in the step is preferably 4-10 hours, more preferably 5-8 hours; in some embodiments provided by the present invention, the high-temperature solid-phase time is preferably 6 hours.
  • the high-temperature solid reaction phase is preferably carried out in a high-temperature furnace. After the reaction is carried out, it is cooled to room temperature with the furnace, and a nitride deep red light material can be obtained.
  • the invention adopts high-temperature solid-state reaction to successfully prepare a nitride deep red light material.
  • the plant lighting device made of nitride deep red light material at least consists of a blue light diode and a light emitting layer.
  • the luminous layer is a deep red fluorescent glass.
  • the deep red fluorescent glass is made of a nitride deep red light material with a low melting point and a general chemical formula: La 2 BaSiAl 2-x Cr x N 6 (wherein, 0 ⁇ x ⁇ 0.2) After the glass powder is mixed, it undergoes a high-temperature solid-state reaction and is finally prepared.
  • the preparation of the deep red fluorescent glass is carried out under a nitrogen atmosphere, and the temperature of the high-temperature solid-state reaction is preferably 450-550°C.
  • the temperature of the high-temperature solid-state reaction is preferably 500°C;
  • the time for the high-temperature solid-state reaction is preferably 0.1-1 h, and in some embodiments provided by the present invention, the time for the high-temperature solid-state reaction is preferably 0.5 h, and finally a deep red fluorescent glass is obtained.
  • nitride deep red light material provided by the present invention and its preparation method are described in detail below in conjunction with examples.
  • the chemical stability of fluorescent materials was evaluated with reference to the method given in Chinese patent CN104422676A (Xie Rongjun, Zhou Tianliang, Rapid Aging Equipment, CN104422676A).
  • the heat quenching characteristic of the phosphor is tested with a phosphor powder heat quenching measuring instrument, the measurement temperature range is: 25-200°C, and the temperature control accuracy is ⁇ 1°C.
  • raise the temperature of the sample to 200°C record the luminous intensity of the phosphor again, and convert it to relative intensity based on the luminous intensity at 25°C strength. It is generally believed that if the luminous intensity of the phosphor at 200°C reaches or exceeds 50% of the luminous intensity of the sample at 25°C (ie when the relative intensity is 50), it can be considered that the phosphor has good thermal quenching properties.
  • the La precursors, Ba precursors, Si precursors, Al precursors, and Cr precursors used in the comparative examples and examples are only examples, and do not constitute restrictions on the raw materials of the precursors.
  • the purity of the precursors is not lower than 99.5 wt%.
  • the material described in this comparative example contains the compound chemical formula: La 2 BaSiAl 1.98 Cr 0.02 N 6 .
  • LaN, BaN, Si 3 N 4 , AlN and CrN as raw materials, accurately weigh the raw materials according to their stoichiometric ratio of La 2 BaSiAl 1.98 Cr 0.02 N 6 , and sinter at 1100°C for 6 hours in a nitrogen-hydrogen mixed atmosphere , after cooling, the nominal chemical composition of the material can be obtained as La 2 BaSiAl 1.98 Cr 0.02 N 6 .
  • the emission spectrum of the obtained luminescent material was measured by a fluorescence spectrometer, and the full width at half maximum of the emission spectrum and the position of the main peak of the emission spectrum are shown in Table 1.
  • the material obtained in Comparative Example 1 is a nitride deep red light material. Measure the luminous intensity at 25°C and define it as 100 (relative intensity), then heat the material to 200°C, record its luminous intensity, and find that its luminous intensity is low, see Table 1 for details. Measure the luminous intensity of the measurement at 25°C and define it as 100 (relative intensity), then put the material into the rapid aging equipment, take it out after aging for 48 hours at 200°C, measure the luminous intensity before and after aging, and find that its luminous intensity is 37. It can be seen that the material corresponding to Comparative Example 1 is a deep red fluorescent material with a broad emission spectrum, general thermal quenching characteristics, and unstable chemical properties.
  • the material described in this embodiment contains a compound chemical formula: La 2 BaSiAl 1.999 Cr 0.001 N 6 .
  • LaN, BaN, Si, AlN and CrN as raw materials, accurately weigh the raw materials according to their stoichiometric ratio of La 2 BaSiAl 1.999 Cr 0.001 N 6 , sinter at 1100°C for 6 hours in a mixed atmosphere of nitrogen and hydrogen, and wait for cooling After that, the nominal chemical composition of the material can be obtained as La 2 BaSiAl 1.999 Cr 0.001 N 6 .
  • the emission spectrum of the obtained luminescent material was measured by a fluorescence spectrometer, and the full width at half maximum of the emission spectrum and the position of the main peak of the emission spectrum are shown in Table 1.
  • Example 1 the material obtained in Example 1 is a nitride deep red light material. Measure the luminous intensity at 25°C and define it as 100 (relative intensity), then heat the material to 200°C, record its luminous intensity, and find that its luminous intensity is relatively high, see Table 1 for details. Measure the luminous intensity of the measurement at 25°C and define it as 100 (relative intensity), then put the material into the rapid aging equipment, take it out after aging for 48 hours at 200°C, measure the luminous intensity before and after aging, and find that its luminous intensity is 78. It can be seen that the material corresponding to Example 1 is a deep red fluorescent material with a broad emission spectrum, good thermal quenching characteristics, and stable chemical properties.
  • the material described in this embodiment contains a compound chemical formula: La 2 BaSiAl 1.995 Cr 0.005 N 6 .
  • LaN, BaN, Si, AlN and CrN as raw materials, accurately weigh the raw materials according to their stoichiometric ratio of La 2 BaSiAl 1.995 Cr 0.005 N 6 , sinter at 1100°C for 6 hours in a mixed atmosphere of nitrogen and hydrogen, and wait for cooling After that, the nominal chemical composition of the material can be obtained as La 2 BaSiAl 1.995 Cr 0.005 N 6 .
  • the emission spectrum of the obtained luminescent material was measured by a fluorescence spectrometer, and the full width at half maximum of the emission spectrum and the position of the main peak of the emission spectrum are shown in Table 1.
  • Example 2 It can be seen from Table 1 that the material obtained in Example 2 is a nitride deep red light material. Measure the luminous intensity at 25°C and define it as 100 (relative intensity), then heat the material to 200°C, record its luminous intensity, and find that its luminous intensity is relatively high, see Table 1 for details. It can be seen that the material corresponding to Example 2 is a deep red fluorescent material with a broad emission spectrum and good thermal quenching properties.
  • the material described in this embodiment contains the compound chemical formula: La 2 BaSiAl 1.98 Cr 0.02 N 6 .
  • LaN, BaN, Si, AlN and CrN as raw materials, accurately weigh the raw materials according to their stoichiometric ratio of La 2 BaSiAl 1.98 Cr 0.02 N 6 , sinter at 1100°C for 6 hours in a mixed atmosphere of nitrogen and hydrogen, and wait for cooling After that, the nominal chemical composition of the material can be obtained as La 2 BaSiAl 1.98 Cr 0.02 N 6 .
  • the emission spectrum of the obtained luminescent material was measured by a fluorescence spectrometer, and the full width at half maximum of the emission spectrum and the position of the main peak of the emission spectrum are shown in Table 1.
  • Example 3 It can be seen from Table 1 that the material obtained in Example 3 is a nitride deep red light material. Measure the luminous intensity at 25°C and define it as 100 (relative intensity), then heat the material to 200°C, record its luminous intensity, and find that its luminous intensity is relatively high, see Table 1 for details. It can be seen that the material corresponding to Example 3 is a deep red fluorescent material with a broad emission spectrum and good thermal quenching properties.
  • the material described in this embodiment contains a compound chemical formula: La 2 BaSiAl 1.96 Cr 0.04 N 6 .
  • LaN, BaN, Si, AlN and CrN as raw materials, accurately weigh the raw materials according to their stoichiometric ratio of La 2 BaSiAl 1.96 Cr 0.04 N 6 , sinter at 1100°C for 6 hours in a mixed atmosphere of nitrogen and hydrogen, and wait for cooling After that, the nominal chemical composition of the material can be obtained as La 2 BaSiAl 1.96 Cr 0.04 N 6 .
  • the emission spectrum of the obtained luminescent material was measured by a fluorescence spectrometer, and the full width at half maximum of the emission spectrum and the position of the main peak of the emission spectrum are shown in Table 1.
  • Example 4 It can be seen from Table 1 that the material obtained in Example 4 is a nitride deep red light material. Measure the luminous intensity at 25°C and define it as 100 (relative intensity), then heat the material to 200°C, record its luminous intensity, and find that its luminous intensity is relatively high, see Table 1 for details. It can be seen that the material corresponding to Example 4 is a deep red fluorescent material with a broad emission spectrum and good thermal quenching properties.
  • the material described in this embodiment contains a compound chemical formula: La 2 BaSiAl 1.92 Cr 0.08 N 6 .
  • LaN, BaN, Si, AlN and CrN as raw materials, accurately weigh the raw materials according to their stoichiometric ratio of La 2 BaSiAl 1.92 Cr 0.08 N 6 , sinter at 1100°C for 6 hours in a mixed atmosphere of nitrogen and hydrogen, and wait for cooling After that, the nominal chemical composition of the material can be obtained as La 2 BaSiAl 1.92 Cr 0.08 N 6 .
  • the emission spectrum of the obtained luminescent material was measured by a fluorescence spectrometer, and the full width at half maximum of the emission spectrum and the position of the main peak of the emission spectrum are shown in Table 1.
  • Example 5 It can be seen from Table 1 that the material obtained in Example 5 is a nitride deep red light material. Measure the luminous intensity at 25°C and define it as 100 (relative intensity), then heat the material to 200°C, record its luminous intensity, and find that its luminous intensity is relatively high, see Table 1 for details. It can be seen that the material corresponding to Example 5 is a deep red fluorescent material with a broad emission spectrum and good thermal quenching properties.
  • the material described in this embodiment contains a compound chemical formula: La 2 BaSiAl 1.9 Cr 0.1 N 6 .
  • LaN, BaN, Si, AlN and CrN as raw materials, accurately weigh the raw materials according to their stoichiometric ratio of La 2 BaSiAl 1.9 Cr 0.1 N 6 , sinter at 1100°C for 6 hours in a mixed atmosphere of nitrogen and hydrogen, and wait for cooling After that, the nominal chemical composition of the material can be obtained as La 2 BaSiAl 1.9 Cr 0.1 N 6 .
  • the emission spectrum of the obtained luminescent material was measured by a fluorescence spectrometer, and the full width at half maximum of the emission spectrum and the position of the main peak of the emission spectrum are shown in Table 1.
  • Example 6 It can be seen from Table 1 that the material obtained in Example 6 is a nitride deep red light material. Measure the luminous intensity at 25°C and define it as 100 (relative intensity), then heat the material to 200°C, record its luminous intensity, and find that its luminous intensity is relatively high, see Table 1 for details. It can be seen that the material corresponding to Example 6 is a deep red fluorescent material with a broad emission spectrum and good thermal quenching properties.
  • the material described in this embodiment contains the compound chemical formula: La 2 BaSiAl 1.85 Cr 0.15 N 6 .
  • LaN, BaN, Si, AlN and CrN as raw materials, accurately weigh the raw materials according to their stoichiometric ratio of La 2 BaSiAl 1.85 Cr 0.15 N 6 , sinter at 1100°C for 6 hours in a mixed atmosphere of nitrogen and hydrogen, and wait for cooling After that, the nominal chemical composition of the material can be obtained as La 2 BaSiAl 1.85 Cr 0.15 N 6 .
  • the emission spectrum of the obtained luminescent material was measured by a fluorescence spectrometer, and the full width at half maximum of the emission spectrum and the position of the main peak of the emission spectrum are shown in Table 1.
  • Example 7 It can be seen from Table 1 that the material obtained in Example 7 is a nitride deep red light material. Measure the luminous intensity at 25°C and define it as 100 (relative intensity), then heat the material to 200°C, record its luminous intensity, and find that its luminous intensity is relatively high, see Table 1 for details. It can be seen that the material corresponding to Example 7 is a deep red fluorescent material with a broad emission spectrum and good thermal quenching properties.
  • the material described in this embodiment contains a chemical compound of the formula: La 2 BaSiAl 1.8 Cr 0.2 N 6 .
  • LaN, BaN, Si, Si 3 N 4 , AlN and CrN as raw materials, accurately weigh the raw materials according to their stoichiometric ratio of La 2 BaSiAl 1.8 Cr 0.2 N 6 , in a mixed atmosphere of nitrogen and hydrogen at 1100°C After sintering for 6 hours and cooling, the nominal chemical composition of the material can be obtained as La 2 BaSiAl 1.8 Cr 0.2 N 6 .
  • the emission spectrum of the obtained luminescent material was measured by a fluorescence spectrometer, and the full width at half maximum of the emission spectrum and the position of the main peak of the emission spectrum are shown in Table 1.
  • Example 8 It can be seen from Table 1 that the material obtained in Example 8 is a nitride deep red light material. Measure the luminous intensity at 25°C and define it as 100 (relative intensity), then heat the material to 200°C, record its luminous intensity, and find that its luminous intensity is relatively high, see Table 1 for details. It can be seen that the material corresponding to Example 8 is a deep red fluorescent material with a broad emission spectrum and good thermal quenching properties.
  • the material described in this embodiment contains the compound chemical formula: La 2 BaSiAl 1.98 Cr 0.02 N 6 .
  • LaN, BaN, Si, Si 3 N 4 , AlN and CrN as raw materials, accurately weigh the raw materials according to their stoichiometric ratio of La 2 BaSiAl 1.98 Cr 0.02 N 6 , at 1100°C in a mixed atmosphere of nitrogen and hydrogen After sintering for 6 hours and cooling, the nominal chemical composition of the material can be obtained as La 2 BaSiAl 1.98 Cr 0.02 N 6 .
  • the emission spectrum of the obtained luminescent material was measured by a fluorescence spectrometer, and the full width at half maximum of the emission spectrum and the position of the main peak of the emission spectrum are shown in Table 1.
  • Example 9 It can be seen from Table 1 that the material obtained in Example 9 is a nitride deep red light material. Measure the luminous intensity at 25°C and define it as 100 (relative intensity), then heat the material to 200°C, record its luminous intensity, and find that its luminous intensity is relatively high, see Table 1 for details. It can be seen that the material corresponding to Example 9 is a deep red fluorescent material with a broad emission spectrum and good thermal quenching properties.
  • the material described in this embodiment contains the compound chemical formula: La 2 BaSiAl 1.98 Cr 0.02 N 6 .
  • LaN, BaN, Si, Si 3 N 4 , AlN and CrN as raw materials, accurately weigh the raw materials according to their stoichiometric ratio of La 2 BaSiAl 1.98 Cr 0.02 N 6 , at 1100°C in a mixed atmosphere of nitrogen and hydrogen After sintering for 6 hours and cooling, the nominal chemical composition of the material can be obtained as La 2 BaSiAl 1.98 Cr 0.02 N 6 .
  • the emission spectrum of the obtained luminescent material was measured by a fluorescence spectrometer, and the full width at half maximum of the emission spectrum and the position of the main peak of the emission spectrum are shown in Table 1.
  • Example 10 It can be seen from Table 1 that the material obtained in Example 10 is a nitride deep red light material. Measure the luminous intensity at 25°C and define it as 100 (relative intensity), then heat the material to 200°C, record its luminous intensity, and find that its luminous intensity is relatively high, see Table 1 for details. It can be seen that the material corresponding to Example 10 is a deep red fluorescent material with a broad emission spectrum and good thermal quenching properties.
  • the material described in this embodiment contains the compound chemical formula: La 2 BaSiAl 1.98 Cr 0.02 N 6 .
  • LaN, BaN, Si, Si 3 N 4 , AlN and CrN as raw materials, accurately weigh the raw materials according to their stoichiometric ratio of La 2 BaSiAl 1.98 Cr 0.02 N 6 , at 1100°C in a mixed atmosphere of nitrogen and hydrogen After sintering for 6 hours and cooling, the nominal chemical composition of the material can be obtained as La 2 BaSiAl 1.98 Cr 0.02 N 6 .
  • the emission spectrum of the obtained luminescent material was measured by a fluorescence spectrometer, and the full width at half maximum of the emission spectrum and the position of the main peak of the emission spectrum are shown in Table 1.
  • Example 11 It can be seen from Table 1 that the material obtained in Example 11 is a nitride deep red light material. Measure the luminous intensity at 25°C and define it as 100 (relative intensity), then heat the material to 200°C, record its luminous intensity, and find that its luminous intensity is relatively high, see Table 1 for details. It can be seen that the material corresponding to Example 11 is a deep red fluorescent material with a broad emission spectrum and good thermal quenching properties.
  • the material described in this embodiment contains a chemical compound of La 2 BaSiAl 1.98 Cr 0.02 N 6 .
  • LaN, BaN, Si, Si 3 N 4 , AlN and CrN as raw materials, accurately weigh the raw materials according to their stoichiometric ratio of La 2 BaSiAl 1.98 Cr 0.02 N 6 , at 1100°C in a mixed atmosphere of nitrogen and hydrogen After sintering for 6 hours and cooling, the nominal chemical composition of the material can be obtained as La 2 BaSiAl 1.98 Cr 0.02 N 6 .
  • the emission spectrum of the obtained luminescent material was measured by a fluorescence spectrometer, and the full width at half maximum of the emission spectrum and the position of the main peak of the emission spectrum are shown in Table 1.
  • Example 12 It can be seen from Table 1 that the material obtained in Example 12 is a nitride deep red light material. Measure the luminous intensity at 25°C and define it as 100 (relative intensity), then heat the material to 200°C, record its luminous intensity, and find that its luminous intensity is relatively high, see Table 1 for details. It can be seen that the material corresponding to Example 12 is a deep red fluorescent material with a broad emission spectrum and good thermal quenching properties.
  • the material described in this embodiment contains the compound chemical formula: La 2 BaSiAl 1.98 Cr 0.02 N 6 .
  • LaN, BaN, Si, Si 3 N 4 , AlN and CrN as raw materials, accurately weigh the raw materials according to their stoichiometric ratio of La 2 BaSiAl 1.98 Cr 0.02 N 6 , at 1100°C in a mixed atmosphere of nitrogen and hydrogen After sintering for 6 hours and cooling, the nominal chemical composition of the material can be obtained as La 2 BaSiAl 1.98 Cr 0.02 N 6 .
  • the emission spectrum of the obtained luminescent material was measured by a fluorescence spectrometer, and the full width at half maximum of the emission spectrum and the position of the main peak of the emission spectrum are shown in Table 1.
  • Example 13 It can be seen from Table 1 that the material obtained in Example 13 is a nitride deep red light material. Measure the luminous intensity at 25°C and define it as 100 (relative intensity), then heat the material to 200°C, record its luminous intensity, and find that its luminous intensity is relatively high, see Table 1 for details. It can be seen that the material corresponding to Example 13 is a deep red fluorescent material with a broad emission spectrum, good thermal quenching characteristics, and stable chemical properties.
  • the chemical composition synthesized in Example 3 is La 2 BaSiAl 1.98 Cr 0.02 N 6 deep red fluorescent material.
  • a deep red light plant lighting source can be obtained by encapsulating the above-mentioned deep red fluorescent glass with a blue light diode with an emission wavelength of 450 nm.

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

Abstract

La présente invention porte sur un matériau de lumière rouge profond à base de nitrure et sur son procédé de préparation et son application ; la formule chimique générale du matériau de lumière rouge profond à base de nitrure est La2BaSiAl2-xCrxN6, dans laquelle 0<x≤0. 2 ; sous l'excitation de la lumière bleue, la plage de crête principale de la longueur d'onde d'émission générée par le matériau fluorescent à lumière rouge intense est comprise entre 680 et 730 nm, et la largeur totale à mi-hauteur du spectre d'émission est supérieure ou égale à 180 nm. Par comparaison avec la technique existante, le matériau de lumière rouge profond à base de nitrure préparé par la présente invention possède une composition chimique entièrement nouvelle, un spectre d'émission relativement large, de bonnes caractéristiques de trempe thermique et des propriétés chimiques stables afin que le matériau d'émission de lumière puisse être appliqué à l'industrie de l'éclairage des plantes.
PCT/CN2021/143756 2021-12-31 2021-12-31 Matériau de lumière rouge profond à base de nitrure, procédé de préparation et dispositif WO2023123386A1 (fr)

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CN202180105271.1A CN118414403A (zh) 2021-12-31 2021-12-31 一种氮化物深红光材料及制备方法与器件

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006117984A1 (fr) * 2005-04-27 2006-11-09 Nichia Corporation Luminophore a base de nitrure et dispositif electroluminescent l'utilisant
EP2998381A1 (fr) * 2013-05-14 2016-03-23 National Institute for Materials Science Luminophore, son procédé de production, dispositif électroluminescent, dispositif d'affichage d'image, et absorbeur d'ultraviolet
CN109796970A (zh) * 2018-12-27 2019-05-24 英特美光电（苏州）有限公司 一种氮化物红色荧光粉及其制备方法
CN111187617A (zh) * 2020-03-06 2020-05-22 英特美光电（苏州）有限公司 一种氮化物红色荧光粉的制备方法
CN112210372A (zh) * 2020-09-22 2021-01-12 厦门大学 一种近红外荧光材料和荧光玻璃与激光近红外器件及其制备方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006117984A1 (fr) * 2005-04-27 2006-11-09 Nichia Corporation Luminophore a base de nitrure et dispositif electroluminescent l'utilisant
EP2998381A1 (fr) * 2013-05-14 2016-03-23 National Institute for Materials Science Luminophore, son procédé de production, dispositif électroluminescent, dispositif d'affichage d'image, et absorbeur d'ultraviolet
CN109796970A (zh) * 2018-12-27 2019-05-24 英特美光电（苏州）有限公司 一种氮化物红色荧光粉及其制备方法
CN111187617A (zh) * 2020-03-06 2020-05-22 英特美光电（苏州）有限公司 一种氮化物红色荧光粉的制备方法
CN112210372A (zh) * 2020-09-22 2021-01-12 厦门大学 一种近红外荧光材料和荧光玻璃与激光近红外器件及其制备方法

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