CN105733572A - Red fluoride fluorescent powder as well as preparation method and application thereof - Google Patents

Red fluoride fluorescent powder as well as preparation method and application thereof Download PDF

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Publication number
CN105733572A
CN105733572A CN201610179601.2A CN201610179601A CN105733572A CN 105733572 A CN105733572 A CN 105733572A CN 201610179601 A CN201610179601 A CN 201610179601A CN 105733572 A CN105733572 A CN 105733572A
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fluorescent material
xmn
red
preparation
fluoride fluorescent
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王静
朱怡雯
黄霖
龚书铭
苏锵
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National Sun Yat Sen University
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National Sun Yat Sen University
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Priority to CN201610179601.2A priority Critical patent/CN105733572A/en
Publication of CN105733572A publication Critical patent/CN105733572A/en
Priority to PCT/CN2016/100896 priority patent/WO2017161852A1/en
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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
    • C09K11/64—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing aluminium
    • 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
    • C09K11/644—Halogenides
    • C09K11/645—Halogenides with alkali or alkaline earth metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier 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 with at least one potential-jump barrier or surface barrier 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
    • Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps

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

Abstract

The invention provides a red fluoride fluorescent powder. A general formula of a chemical composition is A2A'M1-XF6:XMn<4+>; x is the molar percent coefficient of doped Mn<4+> ions relative to M; x is smaller than or equal to 0.3 and greater than 0. The invention further provides a preparation method of the fluorescent powder. The red fluoride fluorescent powder is available in raw material and simple in preparation method, and can be excited by a purple light and a blue light to generate a relatively strong red fluorescent light of which the main peak is 635nm. The red fluoride fluorescent powder is an excellent material which can be applied to encapsulation of a white-light LED and has great application prospect in the fields of illumination and display.

Description

A kind of red fluoride fluorescent material and its preparation method and application
Technical field
The present invention relates to luminescent material technical field, more particularly, to a kind of red fluoride fluorescent material and Preparation method and application.
Background technology
White light LEDs has energy-conservation, and the life-span is long, and advantages of environment protection will become the lighting source of a new generation. The commercial white light LEDs of main flow is to coat yellow by blue chip (emission wavelength 440-480nm) now Y3Al5O12:Ce3+(YAG:Ce3+) fluorescent material luminous realization together.But this method is usually because lack Red color light component, so colour temperature higher (CCT>4500K), color rendering index low (Ra<80).In order to solve This problem, it will usually mix appropriate red fluorescence powder to strengthen the white light LEDs transmitting in red light region. And traditional nitride business red fluorescence powder, emission peak is the widest, and HONGGUANG later for 650nm is unwise to human eye Sense, there is weight absorbing phenomenon when itself and the mixing of other yellow fluorescent powders, and prepares in the widest the making again of absorption spectrum Condition is harsh, economical not.Thus be restricted on using.
Summary of the invention
The present invention is according to the deficiency of white light LEDs material in prior art, it is provided that a kind of red fluoride fluorescence Powder.
Another object of the present invention is to provide the preparation method and application of above-mentioned fluorescent material.
Present invention success first is at K2NaAlF6And K2LiAlF6Fluorescent material substrate mixes Mn4+, synthesize Can be light activated by purple light and indigo plant, the stronger fluorescent material being positioned at 635nm HONGGUANG can be launched.Due to its energy Excited by ultraviolet and blue light, and red emission is a series of spikes, occur heavily to absorb with YAG hardly Phenomenon, so, this fluorescent material is expected to be used for encapsulating white light LEDs.
The present invention reaches above-mentioned technical purpose by the following technical programs:
The invention provides a kind of red fluoride fluorescent material, chemical composition is: A2A’M1-xF6:xMn4+,0<x ≤ 0.3, x are doping Mn4+Ion is relative to the molar percentage coefficient shared by M；
One or more during wherein A is K, Rb, Cs；
A ' is one or more in Li, Na, K, Rb；
M is one or more in Al, Sc, V, Ga, Y, In, Gd, Lu, Bi.
Preferably, wherein A is K.
Preferably, wherein A ' is Li or/and Na.
Preferably, wherein M is Al or/and Ga.
Preferably, described fluorescent material chemical composition is K2LiAl1-xF6:xMn4+、K2LiGa1-xF6:xMn4+、 K2NaAl1-xF6:xMn4+、K2NaGa1-xF6:xMn4+、Cs2NaSc1-xF6:xMn4+、Rb2KSc1-xF6:xMn4+ Or K2NaSc1-xF6:xMn4+。
It is highly preferred that described fluorescent material chemical composition is K2LiAl1-xF6:xMn4+Or K2NaAl1-xF6:xMn4+。
The present invention provides the preparation method of above-mentioned red fluoride fluorescent material, said method comprising the steps of:
S1. A is prepared2A’MF6；
S2. the A that will prepare in S12A’MF6Joining in Fluohydric acid. with fluorine potassium manganate and react, stirring is centrifugal The described red fluoride fluorescent material of rear acquisition；
A in described S12A’MF6By the villaumite containing metal A ', villaumite containing metal M with containing metal The fluoride reaction of A obtains；
The described villaumite containing metal A ', the villaumite containing metal M and the reaction of the fluoride containing metal A Mol ratio is (1～2): 1:3.
Preferably, in described S2, reaction temperature is room temperature.
Preferably, the described response time is 0.5～3h, uses washing with acetone in described S2 after being centrifuged.
Compared with prior art, there is advantages that
The invention discloses a kind of novel red fluoride fluorescent material, described fluorescent material is convieniently synthesized, and raw material is easy to get, And stronger HONGGUANG narrow emission can be produced under purple light and blue light excite, encapsulation white light LEDs material has Standby great application prospect.
Accompanying drawing explanation
Fig. 1 is K in embodiment 22LiAl0.99F6:0.01Mn4+The X-ray diffractogram of fluorescent material.
Fig. 2 is K in embodiment 22LiAl0.99F6:0.01Mn4+The stereoscan photograph of fluorescent material.
Fig. 3 is K in embodiment 22LiAl0.99F6:0.01Mn4+The excitation spectrum of fluorescent material and emission spectrum figure.
Fig. 4 is K in embodiment 72LiAl0.99F6:0.01Mn4+The X-ray diffractogram of fluorescent material.
Fig. 5 is K in embodiment 72LiAl0.99F6:0.01Mn4+The stereoscan photograph of fluorescent material.
Fig. 6 is K in embodiment 72LiAl0.99F6:0.01Mn4+The excitation spectrum of fluorescent material and emission spectrum figure.
Fig. 7 is K in embodiment 122NaAl0.997F6:0.003Mn4+The X-ray diffractogram of fluorescent material.
Fig. 8 is K in embodiment 122NaAl0.997F6:0.003Mn4+The stereoscan photograph of fluorescent material.
Fig. 9 is K in embodiment 122NaAl0.997F6:0.003Mn4+The excitation spectrum of fluorescent material and emission spectrum Figure.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further detailed.But skilled in the art realises that, following Embodiment is not limiting the scope of the invention, any improvement made on the basis of the present invention and change, All within protection scope of the present invention.
Preparation example is given below in the way of illustrating and noting limit.
Embodiment 1:K2MnF6Preparation
Prepare according to the method described in document Angew.Chem-Ger.Edit.65,304-304 (1953) K2MnF6Crystal.
By 0.45g KMnO4With 9g KHF2It is dissolved in 30ml Fluohydric acid. (49%), stirs 20 minutes, The most progressively instill about 1.2ml hydrogen peroxide (30wt.%), solution progressively generates the precipitation of yellow, by molten Liquid is precipitated thing after filtering, and within 2 hours, i.e. obtains K 60 DEG C of bakings after cleaning with acetone2MnF6。
Embodiment 2-6:K2LiAlF6:Mn4+The preparation of fluorescent material
Weigh lithium chloride (LiCl) 0.4239g, aluminum chloride (AlCl3·6H2O) 2.4143g, potassium bifluoride (KHF2) 2.3431g, adds in 20ml water, obtains white precipitate.By washing of precipitate, 70 DEG C are dried 24 hours, Obtain K2LiAlF6.Weigh fluoaluminic acid lithium potassium (K2LiAlF6) 0.2261g, fluorine potassium manganate (K2MnF6)0.0025 G, adds Fluohydric acid. 2ml, reaction 2 hour is stirred at room temperature, with washing with acetone gained solid, then in vacuum Being dried 24 hours in drying baker, last obtained powder is final K2LiAlF6:Mn4+Fluorescent material.
Fig. 1 is that X-ray powder diffraction shows that product is the K with Emission in Cubic2LiAlF6Structure.Scanning electron microscope Photo shows that the powder diameter of synthesis is about 300nm, as shown in Figure 2.By FSP920 type (Edinburgh Instrument) fluorescence spectrophotometer measures the excitation and emission spectra of fluorescent material, sees Fig. 3.Table 1 gives institute The important materialization of the fluorescent material of preparation and optical performance parameter, including the doping content of Mn, prepare proportioning raw materials And the luminous intensity of sample, with the strongest sample of luminescence for 100%, remaining is all expressed as the relative luminous to it Intensity.Wherein the sample absolute quantum yield synthesized by embodiment 4 is 54.11%, fluorescence lifetime 8.9ms. Hot-quenching is gone out better performances, and after optimum conditions, when temperature is heated to 425K, luminous intensity is room During temperature 75.5%.By the K in feed change2MnF6Quality, in the situation that other synthesis conditions are constant Under, can prepare the sample (see embodiment 3-6) of different Mn doping content, its concrete proportioning raw materials and Prepared fluorescent material information is given in Table 1 equally.
Table 1:K2LiAlF6:Mn4+Proportioning raw materials prepared by red fluorescence powder and relative luminous intensity
Embodiment 7-11:K2LiAlF6:Mn4+The preparation of fluorescent material
Weigh lithium chloride (LiCl) 0.8479g, aluminum chloride (AlCl3·6H2O) 2.4143g, potassium bifluoride (KHF2) 2.3431g, adds in 20ml water, obtains white precipitate.By washing of precipitate, 70 DEG C are dried 24 hours, Obtain K2LiAlF6.Weigh fluoaluminic acid lithium potassium (K2LiAlF6) 0.2261g, fluorine potassium manganate (K2MnF6)0.0025 G, adds Fluohydric acid. 2ml, reaction 30 minute is stirred at room temperature, with washing with acetone gained solid, then in vacuum Being dried 24 hours in drying baker, last obtained powder is final K2LiAlF6:Mn4+Fluorescent material.
Fig. 4 is that X-ray powder diffraction shows that product is the K with Emission in Cubic2LiAlF6Structure.Scanning electron microscope Photo shows that the powder diameter of synthesis is about 600nm, as shown in Figure 5.By FSP920 type (Edinburgh Instrument) fluorescence spectrophotometer measures the excitation and emission spectra of fluorescent material, sees Fig. 6.Table 2 gives institute The important materialization of the fluorescent material of preparation and optical performance parameter, including the doping content of Mn, prepare proportioning raw materials And the luminous intensity of sample, with the strongest sample of luminescence for 100%, remaining is all expressed as the relative luminous to it Intensity.Wherein the sample absolute quantum yield synthesized by embodiment 7 is 10.80%, fluorescence lifetime 7.9ms. By the K in feed change2MnF6Quality, in the case of other synthesis conditions are constant, can prepare The sample (see embodiment 8-11) of different Mn doping contents, its concrete proportioning raw materials and prepared fluorescent material letter Breath is given in Table 2 equally.
Table 2:K2LiAlF6:Mn4+Proportioning raw materials prepared by red fluorescence powder and relative luminous intensity
Embodiment 12-17:K2NaAlF6:Mn4+The preparation of fluorescent material
Weigh sodium chloride (NaCl) 0.5844g, aluminum chloride (AlCl3·6H2O) 2.4143g, potassium bifluoride (KHF2) 2.3431g, adds in 20ml water, obtains white precipitate.By washing of precipitate, 70 DEG C are dried 24 hours, Obtain K2NaAlF6.Weigh cryolite potassium (K2NaAlF6) 0.4843g, fluorine potassium manganate (K2MnF6) 0.0015g, adds Fluohydric acid. 2ml, and reaction 30 minute is stirred at room temperature, with washing with acetone gained solid, then Being dried 24 hours in vacuum drying oven, last obtained powder is final K2NaAlF6:Mn4+Fluorescent material.
Fig. 7 is that X-ray powder diffraction shows that product is the K with Emission in Cubic2NaAlF6Structure.Scanning electron microscope Photo shows that the powder diameter of synthesis is about 200-500nm, as shown in Figure 8.By FSP920 type (Edinburgh Instrument) fluorescence spectrophotometer measures the excitation and emission spectra of fluorescent material, sees Fig. 9.
Table 3 gives important materialization and the optical performance parameter of prepared fluorescent material, including the doping content of Mn, Preparation proportioning raw materials and the luminous intensity of sample, with the strongest sample of luminescence for 100%, it is right that remaining is all expressed as Its relative luminous intensity.Wherein the sample hot-quenching synthesized by embodiment 14 is gone out better performances, through synthesis bar After piece optimization, when temperature is heated to 425K, luminous intensity is 87.7% during room temperature.Pass through feed change In K2MnF6Quality, in the case of other synthesis conditions are constant, different Mn doping can be prepared The sample (see embodiment 13-17) of concentration, its concrete proportioning raw materials and prepared fluorescent material information are equally at table Be given in 3.
Table 3:K2NaAlF6:Mn4+Proportioning raw materials prepared by red fluorescence powder and relative luminous intensity

Claims (10)

1. a red fluoride fluorescent material, it is characterised in that chemical composition is: A2A’M1-xF6:xMn4+,0<x≤ 0.3, x is doping Mn4+Ion is relative to the molar percentage coefficient shared by M；
One or more during wherein A is K, Rb, Cs；
A ' is one or more in Li, Na, K, Rb；
M is one or more in Al, Sc, V, Ga, Y, In, Gd, Lu, Bi.
Red fluoride fluorescent material the most according to claim 1, it is characterised in that wherein A is K.
Red fluoride fluorescent material the most according to claim 1, it is characterised in that wherein A ' be Li or/and Na。
Red fluoride fluorescent material the most according to claim 1, it is characterised in that wherein M be Al or/and Ga。
Red fluoride fluorescent material the most according to claim 1, it is characterised in that described fluorescent material chemical group Become K2LiAl1-xF6:xMn4+、K2LiGa1-xF6:xMn4+、K2NaAl1-xF6:xMn4+、K2NaGa1-xF6: xMn4+、Cs2NaSc1-xF6:xMn4+、Rb2KSc1-xF6:xMn4+Or K2NaSc1-xF6:xMn4+。
Red fluoride fluorescent material the most according to claim 1, it is characterised in that described fluorescent material chemical group Become K2LiAl1-xF6:xMn4+Or K2NaAl1-xF6:xMn4+。
7. the preparation method of the red fluoride fluorescent material described in a claim 1, it is characterised in that described side Method comprises the following steps:
S1. A is prepared2A’MF6；
S2. the A that will prepare in S12A’MF6Join in Fluohydric acid. with fluorine potassium manganate and react, obtain after stirring is centrifugal Obtain described red fluoride fluorescent material.
Preparation method the most according to claim 7, it is characterised in that in described S2, reaction temperature is room temperature.
Preparation method the most according to claim 7, it is characterised in that the described response time is 0.5～3h, institute State and after S2 is centrifuged, use washing with acetone.
10. claim 1 to 6 arbitrary described fluorescent material application in illumination and display field.
CN201610179601.2A 2016-03-24 2016-03-24 Red fluoride fluorescent powder as well as preparation method and application thereof Pending CN105733572A (en)

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PCT/CN2016/100896 WO2017161852A1 (en) 2016-03-24 2016-09-29 Red fluoride phosphor powder and preparation method therefor and use thereof

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Cited By (9)

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WO2017161852A1 (en) * 2016-03-24 2017-09-28 中山大学 Red fluoride phosphor powder and preparation method therefor and use thereof
CN107722986A (en) * 2017-09-29 2018-02-23 华南理工大学 A kind of blue light activated Mn4+Adulterate fluoscandate red light material and preparation method thereof
CN109294572A (en) * 2018-10-18 2019-02-01 温州大学 A kind of preparation method of high colour developing white light LEDs red light material
CN110684527A (en) * 2019-07-24 2020-01-14 云南民族大学 Mn-doped blue light excitation4+Hexafluoroferrite red luminescent material and synthetic method thereof
CN111454719A (en) * 2020-05-28 2020-07-28 云南民族大学 double perovskite fluoride red luminescent material for white light LED
CN114989824A (en) * 2022-06-27 2022-09-02 东华理工大学 Short life spheroidal Mn 4+ Fluoride-doped red fluorescent powder, structure, preparation method and light-emitting device
CN115678557A (en) * 2022-11-04 2023-02-03 昆明理工大学 Heat-quenching-resistant up-conversion luminescence thermal enhancement material and preparation method and application thereof
CN116463121A (en) * 2023-03-16 2023-07-21 广东省科学院资源利用与稀土开发研究所 Tetravalent manganese ion and chromium ion co-doped scandium-based fluoride broadband near infrared luminescent material and preparation method thereof
CN116656355A (en) * 2023-04-25 2023-08-29 佛山科学技术学院 Red fluorescent material and optical temperature measurement application and application method thereof

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WO2017161852A1 (en) * 2016-03-24 2017-09-28 中山大学 Red fluoride phosphor powder and preparation method therefor and use thereof
CN107722986A (en) * 2017-09-29 2018-02-23 华南理工大学 A kind of blue light activated Mn4+Adulterate fluoscandate red light material and preparation method thereof
CN109294572A (en) * 2018-10-18 2019-02-01 温州大学 A kind of preparation method of high colour developing white light LEDs red light material
CN110684527A (en) * 2019-07-24 2020-01-14 云南民族大学 Mn-doped blue light excitation4+Hexafluoroferrite red luminescent material and synthetic method thereof
CN110684527B (en) * 2019-07-24 2022-07-12 云南民族大学 Mn-doped blue light excitation4+Hexafluoroferrite red luminescent material and synthetic method thereof
CN111454719A (en) * 2020-05-28 2020-07-28 云南民族大学 double perovskite fluoride red luminescent material for white light LED
CN114989824A (en) * 2022-06-27 2022-09-02 东华理工大学 Short life spheroidal Mn 4+ Fluoride-doped red fluorescent powder, structure, preparation method and light-emitting device
CN115678557A (en) * 2022-11-04 2023-02-03 昆明理工大学 Heat-quenching-resistant up-conversion luminescence thermal enhancement material and preparation method and application thereof
CN115678557B (en) * 2022-11-04 2023-10-03 昆明理工大学 Thermal quenching-resistant up-conversion luminescence thermal enhancement material and preparation method and application thereof
CN116463121A (en) * 2023-03-16 2023-07-21 广东省科学院资源利用与稀土开发研究所 Tetravalent manganese ion and chromium ion co-doped scandium-based fluoride broadband near infrared luminescent material and preparation method thereof
CN116463121B (en) * 2023-03-16 2024-02-02 广东省科学院资源利用与稀土开发研究所 Tetravalent manganese ion and chromium ion co-doped scandium-based fluoride broadband near infrared luminescent material and preparation method thereof
CN116656355A (en) * 2023-04-25 2023-08-29 佛山科学技术学院 Red fluorescent material and optical temperature measurement application and application method thereof

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Application publication date: 20160706