CN106634997A - Composite phosphate fluorophor and application thereof - Google Patents

Composite phosphate fluorophor and application thereof Download PDF

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CN106634997A
CN106634997A CN201610835979.3A CN201610835979A CN106634997A CN 106634997 A CN106634997 A CN 106634997A CN 201610835979 A CN201610835979 A CN 201610835979A CN 106634997 A CN106634997 A CN 106634997A
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fluorophor
light
illuminator
spectrum
luminous
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王海容
文会通
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    • H01L33/502—Wavelength conversion materials

Abstract

The invention relates to a composite phosphate fluorophor and application thereof. The chemical formula of the composite phosphate fluorophor is (M1-aREa)bAcP1-dDdOxEy, wherein M is at least one of Sr, Ca and Ba; RE is at least one of Eu, Ce, Yb, Nd, Pr, Sm, Ho, Er, Tb, Mn, Cr, Bi, Sn and Ni; A is at least one of Mg, Zn, Sc, Y, Gd, La, Lu, Li, Na, K, Rb and Cs; D is at least one of B, Al and Si; E is at least one of F and Cl; P is pentavalent phosphorus; O is oxygen; 0<=a<=0.3, 1.5<=b<=4, 0<=c<=3, 0<d<1, 4<=x<=11, 0<=v<1 and 2<=b+c. The composite phosphate fluorophor can achieve the properties of high-brightness illumination and excellent temperature quenching.

Description

A kind of composite phosphate fluorophor and its application
Technical field
The present invention relates to solid luminescent material field, relates in particular to a kind of composite phosphate fluorophor, further relate to contain There are light-emitting component, pigment and the ultra-violet absorber of this fluorophor.
Background technology
Fluorophor is applied to the every field for illuminating with showing, especially with the development of semiconductor illumination technique, should More and more extensive concern is received for the fluorophor in white light LEDs.White light LEDs photoelectric transformation efficiency height, energy-conserving and environment-protective, make With life-span length, safe and reliable, green illumination light source of future generation is acknowledged as.Currently realize that white light LEDs mainly there are 3 kinds of approach, the One kind is to combine to form white light by red, green and blue color LED chip, but realizes that white light is relatively difficult by this method, because It is very complicated in circuit design to consider the drive characteristic of three different colours chips.Second is to use quantum effect, fortune Prepare LED chip with the same semiconductor of different-grain diameter size to realize white light, the white light LEDs that this method is realized have compared with High efficiency, but it is relatively costly, while technically also immature.The third is using the LED core for sending out ultraviolet light or blue light Piece realizes white light plus fluorophor, and this method is most simple, while being also most ripe method.
LED receives the highest attention of countries in the world as the green illumination light source of energy-conserving and environment-protective of new generation, using ultraviolet Or blue-ray LED excited fluophor and produce the main flow that white light is the development of current white light LEDs, the performance of fluorophor directly affects white light The brightness of LED, colour temperature, heat endurance and colour rendering etc..As white light LEDs are to the development in high-power direction, the operating temperature of LED More and more higher, the operating temperature of current great power LED chips can reach 180 DEG C, and this requires to be applied in white light LEDs Fluorophor must possess excellent temperature quenching characteristic.
At present the fluorophor used in white light LEDs is mainly blue light activated YAG：Ce blooms, it can effectively absorb 460nm Neighbouring blue light, is excited by it and launches gold-tinted, and produces white light with LED blue lights.But due to YAG：Ce blooms send out Penetrate in spectrum and lack red and green spectral components, it is low with white light LEDs colour rendering index made by it, it is impossible to true display object Color；While YAG：The temperature quenching characteristic of Ce blooms is not outstanding, luminous intensity when its luminous intensity is room temperature at 150 DEG C 87%, 74% is then dropped to when 200 DEG C, it is impossible to meet the application demand of large power white light LED.
LED fluorophor newly developed in recent years mainly have silicate phosphor, nitride and nitrogen oxides fluorophor with And the LuAG fluorophor improved on the basis of YAG.Silicate phosphor has wider adjustable transmission wavelength, and luminous efficiency also compares It is higher, but existing silicate phosphor temperature characterisitic is poor, such as Sr3SiO5：Eu2And Sr2SiO4：Eu2Brightness ratio at 150 DEG C Room temperature declines respectively 32% and 62%, thus at present the practical application of silicate phosphor is simultaneously few.
Nitride and nitrogen oxides fluorophor are because having wider excitation spectrum and emission spectrum, and temperature-resistance characteristic and chemistry Stability is superior to YAG blooms, receives the very big concern of white light LEDs industry.With regard to current nitride and nitrogen oxides fluorophor For, fluorophor that can be practical is mainly Sr2Si5N8：Eu rouge and powder and CaAlSiN3：Eu rouge and powder, both nitride rouge and powder tools There is good physical and chemical stability and temperature quenching characteristic and excellent luminescent properties, but synthesis device is expensive, produces work Skill is complicated, and production cost is higher, is unfavorable for popularizing for market.
In YAG：Improved LuAG on the basis of Ce blooms：Ce fluorophor, with preferable luminous efficiency and excellent temperature Degree quenching characteristic, its luminous efficiency in the case where blue-ray LED is excited is about 90%, and the luminosity at 150 DEG C is under room temperature 97%, it is 90% when 200 DEG C, but LuAG：Costly, and synthesis technique is complex for the Ce fluorophor prices of raw materials.
And, in the case of generally fluorophor to be used for into illumination or display, in addition to luminous efficiency height is required, it is also desirable to The fluorophor of any emission wavelength can be selected.Its reason is, for lighting condition under, according to use condition, develop the color sometimes Property it is preferential, sometimes luminous flux is preferential.Therefore can obtain if the fluorophor that emission wavelength is arbitrary value, to improving lighting device Design freedom is useful.In addition, in the case that fluorophor is used for into display, Color reproduction scope can be changed according to purposes, carry The high free degree of display equipment design.
In sum, the fluorophor for using at present can't fully meet the needs of practical application, therefore develop new height The LED fluorophor of effect becomes the focus of domestic and international research.
The content of the invention
The purpose of the present invention is to be directed to the problems referred to above, there is provided a kind of good fluorophor of physical and chemical stability, it has Synthesize the relatively low and higher luminous intensity of easy, production cost and excellent temperature quenching feature, and only change its raw material Species or proportioning can change emission wavelength.
Another object of the present invention be use this fluorophor to provide luminous efficiency is high, heat endurance is good, design is free The light-emitting component spent.
It is a further object to provide having used the pigment and ultra-violet absorber of this fluorophor.
In order to solve above-mentioned problem, the present inventor is to PO4Tetrahedron enters for main substrate composed crystalline solid Go further investigation, as a result found, the specific activator ion of solid solution has been the excellent scheme for solving above-mentioned problem in this matrix, It is achieved thereby that of the invention.
The purpose of the present invention is achieved through the following technical solutions：
1st invention is a kind of composite phosphate fluorophor, it is characterised in that：The chemical composition formula of fluorophor is：
(M1-aREa)bAcP1-dDdOxEy, wherein, M is at least one of Sr, Ca, Ba；RE be Eu, Ce, Yb, Nd, Pr, Sm, At least one of Ho, Er, Tb, Mn, Cr, Bi, Sn, Ni；A be Mg, Zn, Sc, Y, Gd, La, Lu, Li, Na, K, Rb, Cs at least It is a kind of；D is at least one of B, Al, Si；E is at least one of F, Cl；P is pentavalent phosphorus；O is oxygen；0 ＜ a≤0.3,1.5≤b ≤ 4,0≤c≤3,0 ＜ d ＜ Isosorbide-5-Nitraes≤x≤11,0≤y ＜ 1,2≤b+c.
2nd invention is the involved fluorophor of the 1st invention, it is characterised in that：At least contain Eu in RE2+Or/and Ce3+。
3rd invention is the involved fluorophor of the 1st～2 any one invention, it is characterised in that：In D also comprising Ga, C, Ge, At least one of Ti, Zr, Hf, V, Nb, Ta.
4th invention is a kind of phosphate fluophor, it is characterised in that：The chemical formula of fluorophor is：Sr3-zMg2P2O10：Euz。
5th invention is the involved fluorophor of the 4th invention, it is characterised in that：0 ＜ z≤0.3.
6th invention is the involved fluorophor of the 4th～5 invention, it is characterised in that：Mg can partly or entirely be replaced by Zn.
7th invention is a kind of light-emitting component, and it includes the 1st illuminator and the 2nd illuminator, and the 1st illuminator is sent with the 1st The light of luminescent spectrum, the 2nd illuminator absorbs at least a portion of the light with the 1st luminescent spectrum, and send with and institute State the light of the 2nd different luminescent spectrum of the 1st luminescent spectrum；It is characterized in that：Contain the 1st～6 any one as the 2nd illuminator to send out Bright described fluorophor.
8th invention is the involved light-emitting component of the 7th invention, it is characterised in that：Light-emitting diodes are used as the 1st illuminator Pipe or laser diode, or based on low pressure or the discharge lamp of high pressure, or electroluminescent lamp.
9th invention is a kind of pigment, it is characterised in that：Containing the described fluorophor of the 1st～6 any one invention.
10th invention is a kind of ultra-violet absorber, it is characterised in that：Containing the described fluorescence of the 1st～6 any one invention Body.
Fluorophor of the present invention can be used with being associated with other ultraviolet sources or blue light source such as Nan dian Yao, Or be used in combination with blue light EL luminescent materials.EL represents electroluminescent.
Description of the drawings
Launching light spectrogram under Fig. 1 is the excitation spectrum of the fluorophor of the embodiment of the present invention 1 and 460nm wavelength blue lights are excited.
Fig. 2 is temperature quenching performance diagram of the fluorophor of the embodiment of the present invention 1 in the case where 460nm wavelength blue lights are excited.
Specific embodiment
Fluorophor of the present invention synthesis is easy, can be using high temperature solid phase synthesis, coprecipitation, sol-gal process, micro- Prepared by the conventional solid synthesis techniques such as ripple sintering synthetic method, without the need for high-pressure synthesis, operate without in glove box during dispensing, has Beneficial to mass production, therefore production cost is relatively low.The technical process of its high temperature solid phase synthesis is：Claim according to chemical formula component The simple substance or compound of respective element are taken, and add at least one of boric acid, halide, alkali carbonate as flux, The addition of flux is the 0～10% of raw material gross mass.After ground and mixed is uniform, reducing atmosphere is passed through in high temperature resistance furnace Or nitrogen, sintering obtains product in 1～30 hour at 800 DEG C～1800 DEG C.In addition, in order to obtain the uniform fluorescence of crystalline phase Body, it is also possible to which the fluorophor for obtaining is carried out repeating crushing, fired again.The reducing atmosphere is charcoal, carbon monoxide, hydrogen, nitrogen At least one in gas, ammonia.
The present invention is further illustrated below by embodiment, but as long as without departing from spirit of the invention, this It is bright not by following embodiments any restriction.
Embodiment 1：Sr1.47MgP0.8Al0.2O4.8：Eu0.03The synthesis of fluorophor：
In chemical composition formula (M1-aREa)bAcP1-dDdOxEyIn, RE=Eu, M=Sr, A=Mg, D=Al are set, weigh Various raw materials, so that each ion mol ratio for constituting fluorophor is Eu: Sr: Mg: P: D: O :=0.03: 1.47: 1: 0.8: 0.2: 4.8 (a=0.02, b=1.5, c=1, d=0.2, x=4.8, y=0).
Weigh 0.99gSrCO3、1.4gSrHPO4、0.4gMgO、0.1gAl2O3、0.05gEu2O3, and add 0.03gH3BO3 As cosolvent, it is fully ground after being well mixed, is fitted into corundum crucible roasting in reducing atmosphere, in 1400 DEG C 2 hours is incubated, Obtain final product the fluorophor.Its excitation spectrum and emission spectrum are shown in Fig. 1, and emission spectrum halfwidth is about 60nm, and transmitting main peak exists The red light region of 620nm；Excitation spectrum be a broadband excitation spectrum, the equal energy of ultraviolet or visible ray in the range of 200～500nm Effectively excite；It is 76% under its external quantum efficiency room temperature in the case where 460nm blue lights are excited, is 75% when 200 DEG C, with superior Luminescent properties.
Fig. 2 is embodiment 1Sr1.47MgP0.8Al0.2O4.8：Eu0.03The temperature quenching performance diagram of fluorophor.Can from Fig. 2 To find out that the fluorophor of embodiment 1 has excellent temperature quenching characteristic, in the range of 200 DEG C, its luminous intensity with temperature liter Height is kept approximately constant.
Embodiment 2～23：
In chemical composition formula (M1-aREa)bAcP1-dDdOxEyIn, set RE=(Eu, Ce), M=(Sr, Ca, Ba), A= (Mg, Zn, Sc, Y, Lu, Gd, La, Li, Na, K), D=(B, Al, Si, Ga, Ge, Ti, Zr, V, Nb), E=(F, Cl), by table 1 The specific chemical formula composition of each embodiment weighs various raw materials, and preparation process is same as Example 1, the fluorophor for obtaining it is luminous Characteristic is shown in Table 1.
The chemical formula and its characteristics of luminescence (excitation wavelength is 460nm) of the embodiment 1～23 of table 1
Embodiment 24：Ca2.3P0.8Al0.2O4.85：Ce0.05, Mn0.1, Bi0.05The synthesis of fluorophor：
In chemical composition formula (M1-aREa)bAcP1-dDdOxEyIn, RE=(Ce, Mn, Bi), M=Ca, D=Al are set, claim Various raw materials are measured, so that each ion mol ratio for constituting fluorophor is Ce: Mn: Bi: Ca: P: Al: O=0.05: 0.1: 0.05: 2.3: 0.8: 0.2: 4.85 (a=0.08, b=2.5, c=0, d=0.2, x=4.85, y=0).
Weigh 1.5gCaCO3、1.32gCaHPO4、0.1gAl2O3、0.08gCeO2、0.12gMnCO3、0.11gBi2O3, fully After ground and mixed is uniform, it is fitted into corundum crucible roasting in reducing atmosphere, in 1300 DEG C 2 hours is incubated, obtains final product the fluorophor. Its emission spectrum is located at 520nm and main peak and constitutes positioned at two broadbands of 595nm by main peak, and the emission spectrum at 520nm is Ce3+ Ion it is luminous, emission spectrum 595nm at is Mn2+Luminous, the Bi of ion3+Ion can effectively strengthen Ce3+Ion and Mn2+ Ion it is luminous；It is 75% under fluorophor external quantum efficiency room temperature in the case where 460nm blue lights are excited, is 73% when 200 DEG C, has Superior luminescent properties.
Embodiment 25：Sr2.25MgP0.8Al0.2O5.85：Ce0.1, Eu0.05, Mn0.1The synthesis of fluorophor：
In chemical composition formula (M1-aREa)bAcP1-dDdOxEyIn, set RE=(Ce, Eu, Mn), M=Sr, A=Mg, D= Al, weighs various raw materials, and each ion mol ratio for making fluorophor is Ce: Eu: Mn: Sr: Mg: P: Al: O=0.1: 0.05: 0.1: 2.25: 1: 0.8: 0.2: 5.85 (a=0.1, b=2.5, c=1, d=0.2, x=5.85, y=0).
Weigh 2.14gSrCO3、1.41gSrHPO4、0.4gMgO、0.1gAl2O3、0.17gCeO2、0.09gEu2O3、 0.12gMnCO3, and add 0.03gH3BO3As cosolvent, it is fully ground after being well mixed, loads corundum crucible in also Primordial Qi Roasting in atmosphere, in 1400 DEG C 2 hours are incubated, and obtain final product the fluorophor.Its emission spectrum is located at respectively 445nm, 525nm by main peak Constitute with three broadbands of 630nm, the emission spectrum at 445nm is Ce3+Ion it is luminous, emission spectrum 525nm at is Mn2 +Ion it is luminous, emission spectrum 630nm at is Eu2+Ion it is luminous；Fluorophor is presented under 400nm near ultraviolet excitations White light emission, is 69% under its external quantum efficiency room temperature, is 67% when 200 DEG C, with superior luminescent properties.
Embodiment 26：Sr1.5Ca0.8P0.8Si0.2O5：Ce0.1, Ho0.1The synthesis of fluorophor：
In chemical composition formula (M1-aREa)bAcP1-dDdOxEyIn, RE=(Ce, Ho), M=(Sr, Ca), D=Si are set, Various raw materials are weighed, each ion mol ratio for making fluorophor is Ce: Ho: Sr: Ca: P: Si: O=0.1: 0.1: 1.5: 0.8: 0.8: 0.2: 5 (a=0.08, b=2.5, c=0, d=0.2, x=5, y=0).
Weigh 2.2gSrCO3、1.32gCaHPO4、0.12gSiO2、0.17gCeO2、0.19gHo2O3, and add 0.03gH3BO3As cosolvent, it is fully ground after being well mixed, is fitted into corundum crucible roasting in reducing atmosphere, in 1400 DEG C Insulation 2 hours, obtains final product the fluorophor.Its emission spectrum is located at the broadband of 460nm by main peak and main peak is located at the arrowband of 520nm Spectral composition, the emission spectrum at 460nm is Ce3+Ion it is luminous, emission spectrum 520nm at is Ho3+Ion it is luminous； Fluorophor is 65% under its external quantum efficiency room temperature under 400nm near ultraviolet excitations, is 63% when 200 DEG C, with superior Luminescent properties.
Embodiment 27：Sr1.5Ca0.8P0.8Si0.2O5：Ce0.1, Sm0.1The synthesis of fluorophor：
In chemical composition formula (M1-aREa)bAcP1-dDdOxEyIn, RE=(Ce, Sm), M=(Sr, Ca), D=Si are set, Various raw materials are weighed, each ion mol ratio for making fluorophor is Ce: Sm: Sr: Ca: P: Si: O=0.1: 0.1: 1.5: 0.8: 0.8: 0.2: 5 (a=0.08, b=2.5, c=0, d=0.2, x=5, y=0).
Weigh 2.2gSrCO3、1.32gCaHPO4、0.12gSiO2、0.17gCeO2、0.18gSm2O3, and add 0.03gH3BO3As cosolvent, it is fully ground after being well mixed, is fitted into corundum crucible roasting in reducing atmosphere, in 1400 DEG C Insulation 2 hours, obtains final product the fluorophor.Its emission spectrum is located at the broadband of 460nm by main peak and main peak is located at the arrowband of 591nm Spectral composition, the emission spectrum at 460nm is Ce3+Ion it is luminous, emission spectrum 591nm at is Sm3+Ion it is luminous： Fluorophor is 63% under its external quantum efficiency room temperature under 400nm near ultraviolet excitations, is 62% when 200 DEG C, with superior Luminescent properties.
Embodiment 28：Sr1.5Ca0.8P0.8Si0.2O5：Ce0.1, Pr0.1The synthesis of fluorophor：
In chemical composition formula (M1-aREa)bAcP1-dDdOxEyIn, RE=(Ce, Pr), M=(Sr, Ca), D=Si are set, Various raw materials are weighed, each ion mol ratio for making fluorophor is Ce: Pr: Sr: Ca: P: Si: O=0.1: 0.1: 1.5: 0.8: 0.8: 0.2: 5 (a=0.08, b=2.5, c=0, d=0.2, x=5, y=0).
Weigh 2.2gSrCO3、1.32gCaHPO4、0.12gSiO2、0.17gCeO2、0.18gPr6O11, and add 0.03gH3BO3As cosolvent, it is fully ground after being well mixed, is fitted into corundum crucible roasting in reducing atmosphere, in 1400 DEG C Insulation 2 hours, obtains final product the fluorophor.Its emission spectrum is located at the broadband of 460nm by main peak and main peak is located at the arrowband of 611nm Spectral composition, the emission spectrum at 460nm is Ce3+Ion it is luminous, emission spectrum 611nm at is Pr3+Ion it is luminous； Fluorophor is 61% under its external quantum efficiency room temperature under 400nm near ultraviolet excitations, is 60% when 200 DEG C, with superior Luminescent properties.
Embodiment 29：Sr1.32MgP0.8Al0.2O4.85：Eu0.08：Er0.1The synthesis of fluorophor：
In chemical composition formula (M1-aREa)bAcP1-dDdOxEyIn, RE=(Eu, Er), M=Sr, A=Mg, D=Al are set, Various raw materials are weighed, each ion mol ratio for making fluorophor is Eu: Er: Sr: Mg: P: Al: O=0.08: 0.1: 1.32: 1: 0.8: 0.2: 4.85 (a=0.12, b=1.5, c=1, d=0.2, x=4.85, y=0).
Weigh 0.77gSrCO3、1.4gSrHPO4、0.4gMgO、0.1gAl2O3、0.15gEu2O3、0.2gEr2O3, and add 0.03gH3BO3As cosolvent, it is fully ground after being well mixed, is fitted into corundum crucible roasting in reducing atmosphere, in 1400 DEG C Insulation 2 hours, obtains final product the fluorophor.Its emission spectrum is located at the broadband of 605nm by main peak and main peak is located at the arrowband of 667nm Spectral composition, the broadband emission spectra at 605nm is Eu2+Ion it is luminous, narrow band emission spectra 667nm at is Er3+Ion It is luminous；Fluorophor, in the case where 460nm blue lights are excited, is 68% under its external quantum efficiency room temperature, is 67% when 200 DEG C, with excellent Luminescent properties more.
Embodiment 30：Sr2.47MgP0.8Al0.2O5.9：Eu0.1, Ni0.03The synthesis of fluorophor：
In chemical composition formula (M1-aREa)bAcP1-dDdOxEyIn, RE=(Eu, Ni), M=Sr, A=Mg, D=Al are set, Various raw materials are weighed, each ion mol ratio for making fluorophor is Eu: Ni: Sr: Mg: P: Al: O=0.1: 0.03: 2.47: 1: 0.8: 0.2: 5.9 (a=0.05, b=2.6, c=1, d=0.2, x=5.9, y=0).
Weigh 2.46gSrCO3、1.4gSrHPO4、0.4gMgO、0.1gAl2O3、0.18gEu2O3、0.04gNiCO3, and add Enter 0.03gH3BO3As cosolvent, it is fully ground after being well mixed, is fitted into corundum crucible roasting in reducing atmosphere, in 1400 DEG C insulation 2 hours, obtain final product the fluorophor.Emission spectrum halfwidth is about 60nm, and transmitting main peak is in the red light region of 610nm； Excitation spectrum is a broadband excitation spectrum, and the ultraviolet or visible ray in the range of 200～500nm can be excited effectively；Ni2+Ion To Eu2+The luminous of ion has obvious humidification, in the case where 460nm blue lights are excited, is under fluorophor external quantum efficiency room temperature 78%, it is 76% when 200 DEG C, with superior luminescent properties.
Embodiment 31：Sr2.28MgP0.8Al0.2O5.71：Eu0.1, Nd0.02The synthesis of fluorophor：
In chemical composition formula (M1-aREa)bAcP1-dDdOxEyIn, RE=(Eu, Nd), M=Sr, A=Mg, D=Al are set, Various raw materials are weighed, each ion mol ratio for making fluorophor is Eu: Nd: Sr: Mg: P: Al: O=0.1: 0.02: 2.28: 1: 0.8: 0.2: 5.71 (a=0.05, b=2.4, c=1, d=0.2, x=5.71, y=0).
Weigh 2.18gSrCO3、1.4gSrHPO4、0.4gMgO、0.1gAl2O3、0.18gEu2O3、0.04gNd2O3, and add 0.03gH3BO3As cosolvent, it is fully ground after being well mixed, is fitted into corundum crucible roasting in reducing atmosphere, in 1400 DEG C Insulation 2 hours, obtains final product the fluorophor.Emission spectrum halfwidth is about 60nm, and transmitting main peak is in the red light region of 610nm；Swash Luminous spectrum is a broadband excitation spectrum, and the ultraviolet or visible ray in the range of 200～500nm can be excited effectively；It is blue in 460nm Light is excited down, is 70% under fluorophor external quantum efficiency room temperature, is 68% when 200 DEG C, with superior luminescent properties；Nd3+From Son is to Eu2+The luminous of ion has the effect for being significantly shorter persistence, is conducive to fluorophor in the application of field of display.
Embodiment 32：Sr2.28MgP0.8Al0.2O5.71：Eu0.1, Cr0.02The synthesis of fluorophor：
In chemical composition formula (M1-aREa)bAcP1-dDdOxEyIn, RE=(Eu, Cr), M=Sr, A=Mg, D=Al are set, Various raw materials are weighed, each ion mol ratio for making fluorophor is Eu: Cr: Sr: Mg: P: Al: O=0.1: 0.02: 2.28: 1: 0.8: 0.2: 5.71 (a=0.05, b=2.4, c=1, d=0.2, x=5.71, y=0).
Weigh 2.18gSrCO3、1.4gSrHPO4、0.4gMgO、0.1gAl2O3、0.18gEu2O3、0.02gCr2O3, and add 0.03gH3BO3As cosolvent, it is fully ground after being well mixed, is fitted into corundum crucible roasting in reducing atmosphere, in 1400 DEG C Insulation 2 hours, obtains final product the fluorophor.Emission spectrum halfwidth is about 60nm, and transmitting main peak is in the red light region of 610nm；Swash Luminous spectrum is a broadband excitation spectrum, and the ultraviolet or visible ray in the range of 200～500nm can be excited effectively；It is blue in 460nm Light is excited down, is 70% under fluorophor external quantum efficiency room temperature, is 68% when 200 DEG C, with superior luminescent properties；Cr3+From Son is to Eu2+The luminous of ion has the effect for being significantly shorter persistence, is conducive to fluorophor in the application of field of display.
Embodiment 33：Sr1.95MgP0.8Al0.2O5.3：Yb0.05The synthesis of fluorophor：
In chemical composition formula (M1-aREa)bAcP1-dDdOxEyIn, RE=Yb, M=Sr, A=Mg, D=Al are set, weigh Various raw materials, each ion mol ratio for making fluorophor is Yb: Sr: Mg: P: Al: O=0.05: 1.95: 1: 0.8: 0.2: 5.3 (a= 0.025th, b=2, c=1, d=0.2, x=5.3, y=0).
Weigh 1.7gSrCO3、1.4gSrHPO4、0.4gMgO、0.1gAl2O3、0.2gYb2O3, and add 0.03gH3BO3Make For cosolvent, it is fully ground after being well mixed, is fitted into corundum crucible roasting in reducing atmosphere, is incubated 2 hours in 1400 DEG C, i.e., Obtain the fluorophor.Emission spectrum halfwidth is about 80nm, and transmitting main peak is in the red light region of 615nm；Excitation spectrum is one wide Band excitation spectrum, the ultraviolet and visible ray in the range of 250～480nm can be excited effectively；It is glimmering in the case where 440nm blue lights are excited It is 62% under body of light external quantum efficiency room temperature, is 58% when 200 DEG C, with superior luminescent properties.
Embodiment 34：Sr1.47MgP0.8Al0.2O4.8：Sn0.03The synthesis of fluorophor：
In chemical composition formula (M1-aREa)bAcP1-dDdOxEyIn, RE=Sn, M=Sr, A=Mg, D=Al are set, weigh Various raw materials, each ion mol ratio for making fluorophor is Sn: Sr: Mg: P: Al: O=0.03: 1.47: 1: 0.8: 0.2: 4.8 (a= 0.02nd, b=1.5, c=1, d=0.2, x=4.8, y=0).
Weigh 0.99gSrCO3、1.4gSrHPO4、0.4gMgO、0.1gAl2O3、0.04gSnO2, and add 0.03gH3BO3 As cosolvent, it is fully ground after being well mixed, is fitted into corundum crucible roasting in reducing atmosphere, in 1400 DEG C 2 hours is incubated, Obtain final product the fluorophor.Emission spectrum halfwidth is about 100nm, and transmitting main peak is in the red light region of 620nm；Excitation spectrum is one Broadband excitation spectrum, the ultraviolet in the range of 200～400nm can be excited effectively；It is glimmering in the case where 365nm long wave ultraviolet lights are excited It is 73% under body of light external quantum efficiency room temperature, is 72% when 200 DEG C, with superior luminescent properties.
Embodiment 35：Sr1.98MgP0.8Al0.2O5.31：Tb0.02The synthesis of fluorophor：
In chemical composition formula (M1-aREa)bAcP1-dDdOxEyIn, RE=Tb, M=Sr, A=Mg, D=Al are set, weigh Various raw materials, each ion mol ratio for making fluorophor is Tb: Sr: Mg: P: Al: O=0.02: 1.98: 1: 0.8: 0.2: 5.31 (a =0.01, b=2, c=1, d=0.2, x=5.31, y=0).
Weigh 1.74gSrCO3、1.4gSrHPO4、0.4gMgO、0.1gAl2O3、0.04gTb4O7, and add 0.03gH3BO3 As cosolvent, it is fully ground after being well mixed, is fitted into corundum crucible roasting in reducing atmosphere, in 1400 DEG C 2 hours is incubated, Obtain final product the fluorophor.Its emission spectrum is made up of the narrow-band spectrum that main peak is located at 545nm, and fluorophor is in 365nm long wave ultraviolets Line is excited down, is 69% under its external quantum efficiency room temperature, is 67% when 200 DEG C, with superior luminescent properties.
Embodiment 36：Sr2.96Mg2P2O10：Eu0.04The synthesis of fluorophor：
In chemical formula Sr3-zMg2P2O10：EuzIn, z=0.04 is set, weigh 0.7gSrCO3、1.84gSrHPO4、 0.4gMgO、0.04gEu2O3, and add 0.03gH3BO3As cosolvent, it is fully ground after being well mixed, loads corundum crucible The roasting in reducing atmosphere, in 1400 DEG C 2 hours are incubated, and obtain final product the fluorophor.Emission spectrum halfwidth is about 60nm, transmitting Main peak is in the red light region of 625nm；Excitation spectrum be a broadband excitation spectrum, the ultraviolet or visible in the range of 200～500nm Light can be excited effectively；It is 75% under its external quantum efficiency room temperature in the case where 460nm blue lights are excited, is 74% when 200 DEG C, has Superior luminescent properties.
Embodiment 37：Sr2.94Mg1.5Zn0.5P2O10：Eu0.06The synthesis of fluorophor：
In chemical formula Sr3-zMg2P2O10：EuzIn, z=0.06 is set, and 0.5 mole of Mg is replaced with 0.5 mole of Zn, weigh 0.69gSrCO3、1.84gSrHPO4、0.3gMgO、0.21gZnO、0.06gEu2O3, and add 0.03gH3BO3As cosolvent, It is fully ground after being well mixed, is fitted into corundum crucible roasting in reducing atmosphere, in 1400 DEG C 2 hours are incubated, obtains final product described glimmering Body of light.Emission spectrum halfwidth is about 60nm, and transmitting main peak is in the red light region of 626nm；Excitation spectrum is a broadband excitation light Spectrum, the ultraviolet or visible ray in the range of 200～500nm can be excited effectively；In the case where 460nm blue lights are excited, its outer quantum effect It is 75% under rate room temperature, is 74% when 200 DEG C, with superior luminescent properties.
Embodiment 38：Sr2.9M[gZnP2O10：Eu0.1The synthesis of fluorophor：
In chemical formula Sr3-zMg2P2O10：EuzIn, z=0.1 is set, and 1 mole of Mg is replaced with 1 mole of Zn, weigh 0.66gSrCO3、1.84gSrHPO4、0.2gMgO、0.41gZnO、0.09gEu2O3, and add 0.03gH3BO3As cosolvent, It is fully ground after being well mixed, is fitted into corundum crucible roasting in reducing atmosphere, in 1400 DEG C 2 hours are incubated, obtains final product described glimmering Body of light.Emission spectrum halfwidth is about 60nm, and transmitting main peak is in the red light region of 628nm；Excitation spectrum is a broadband excitation light Spectrum, the ultraviolet or visible ray in the range of 200～500nm can be excited effectively；In the case where 460nm blue lights are excited, its outer quantum effect It is 73% under rate room temperature, is 72% when 200 DEG C, with superior luminescent properties.
The fluorophor of the present invention shows luminous, the more excellent thermal stability of briliancy higher than existing fluorophor, institute White light emitting device, ligthing paraphernalia, VFD, FED, PDP, CRT etc. are suitable for it.In addition, the fluorophor of the present invention can hold Change places and adjust the peak width of emission wavelength and glow peak, so practicality industrially is big, can expect to be flexibly applied to from now on Various light-emitting devices, illumination, the design of material of image display device, the development of Promoting Industrial.
Although being described in detail by the present invention using specific mode, it will be evident to those skilled in the art that can not take off It is variously changed in the intent and scope of the present invention.

Claims (10)

1. a kind of composite phosphate fluorophor, it is characterised in that：The chemical composition formula of fluorophor is：
(M1-aREa)bAcP1-dDdOxEy, wherein, M is at least one of Sr, Ca, Ba；RE be Eu, Ce, Yb, Nd, Pr, Sm, Ho, At least one of Er, Tb, Mn, Cr, Bi, Sn, Ni；A is at least one in Mg, Zn, Sc, Y, Gd, La, Lu, Li, Na, K, Rb, Cs Kind；D is at least one of B, Al, Si；E is at least one of F, Cl；P is pentavalent phosphorus；O is oxygen；0 ＜ a≤0.3,1.5≤b≤ 4,0≤c≤3,0 ＜ d ＜ Isosorbide-5-Nitraes≤x≤11,0≤y ＜ 1,2≤b+c.
2. fluorophor according to claim 1, it is characterised in that：At least contain Eu in RE2+Or/and Ce3+。
3. the fluorophor according to any one of claim 1～2, it is characterised in that：In D also comprising Ga, C, Ge, Ti, Zr, At least one of Hf, V, Nb, Ta.
4. a kind of phosphate fluophor, it is characterised in that：The chemical formula of fluorophor is：Sr3-zMg2P2O10：Euz。
5. fluorophor according to claim 4, it is characterised in that：0 ＜ z≤0.3.
6. the fluorophor according to claim 4～5, it is characterised in that：Mg can partly or entirely be replaced by Zn.
7. a kind of light-emitting component, it includes the 1st illuminator and the 2nd illuminator, and the 1st illuminator is sent with the 1st luminescent spectrum Light, the 2nd illuminator absorbs at least a portion of the light with the 1st luminescent spectrum, and send with and the described 1st luminous light The light of the 2nd different luminescent spectrum of spectrum；It is characterized in that：Contain with good grounds any one of claim 1～6 institute as the 2nd illuminator The fluorophor stated.
8. light-emitting component according to claim 7, it is characterised in that：Light emitting diode is used as the 1st illuminator or swash Optical diode, or based on low pressure or the discharge lamp of high pressure, or electroluminescent lamp.
9. a kind of pigment, it is characterised in that：The pigment is containing the fluorophor described in good grounds any one of claim 1～6.
10. a kind of ultra-violet absorber, it is characterised in that：The ultra-violet absorber contains with good grounds any one of claim 1～6 Described fluorophor.
CN201610835979.3A 2016-09-21 2016-09-21 Composite phosphate fluorophor and application thereof Pending CN106634997A (en)

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN106634996A (en) * 2016-09-21 2017-05-10 王海容 Fluorophor and application method thereof
CN108085004A (en) * 2017-12-22 2018-05-29 厦门大学 It is a kind of for blue colour fluorescent powder of three primary colours warm white LED and preparation method thereof
CN111760581A (en) * 2019-08-30 2020-10-13 万华化学（宁波）有限公司 Catalyst for preparing phosgene, preparation method thereof and method for preparing phosgene and comprehensively utilizing energy
CN114958332A (en) * 2022-05-31 2022-08-30 广州大学 Luminescent thermochromic fluorescent material and preparation method and application thereof

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Publication number Priority date Publication date Assignee Title
CN102559185A (en) * 2010-12-20 2012-07-11 财团法人交大思源基金会 Yellow luminescent material with voelckerite structure and preparation method thereof as well as white light-emitting diode device
CN104087300A (en) * 2014-03-20 2014-10-08 王海容 Thiophosphate phosphor and application thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102559185A (en) * 2010-12-20 2012-07-11 财团法人交大思源基金会 Yellow luminescent material with voelckerite structure and preparation method thereof as well as white light-emitting diode device
CN104087300A (en) * 2014-03-20 2014-10-08 王海容 Thiophosphate phosphor and application thereof

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106634996A (en) * 2016-09-21 2017-05-10 王海容 Fluorophor and application method thereof
CN108085004A (en) * 2017-12-22 2018-05-29 厦门大学 It is a kind of for blue colour fluorescent powder of three primary colours warm white LED and preparation method thereof
WO2019120265A1 (en) * 2017-12-22 2019-06-27 厦门大学 Blue fluorescent powder for three primary color warm white light led and preparation method therefor
CN108085004B (en) * 2017-12-22 2019-07-05 厦门大学 A kind of blue colour fluorescent powder and preparation method thereof for three primary colours warm white LED
US11142690B2 (en) 2017-12-22 2021-10-12 Xiamen University Blue fluorescent powder for three primary color warm white light LED and preparation method therefor
CN111760581A (en) * 2019-08-30 2020-10-13 万华化学（宁波）有限公司 Catalyst for preparing phosgene, preparation method thereof and method for preparing phosgene and comprehensively utilizing energy
CN114958332A (en) * 2022-05-31 2022-08-30 广州大学 Luminescent thermochromic fluorescent material and preparation method and application thereof

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