CN102250616B - Double-perovskite structured red fluorescent powder as well as preparation method and application thereof - Google Patents
Double-perovskite structured red fluorescent powder as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses double-perovskite structured red fluorescent powder as well as a preparation method and application thereof, belonging to the field of fluorescent materials. The chemical formula of the fluorescent powder can be shown as Ln2-xAMO6:xEu and meets the following conditions: Ln is one, two or three of La, Gd and Y; A is one, two or three of Li, Na and K; M is one, two or three of Sb, Nb and Ta; and Eu is a luminescent center and is doped in the Ln position and the doping value x is 0.01-1.0. The fluorescent powder disclosed by the invention can emit fluorescence of 570-640 nm under the excitation of a green light chip (528-533 nm), a blue light chip (460-470 nm) or a near-ultraviolet light chip (390-399 nm), and red fluorescence is of 600-620 nm. The fluorescent powder can be used for white LED (light-emitting diode) and related display and lighting devices, has a simple preparation process, stable chemical properties and excellent luminescent performance, and is ideal fluorescent powder used for white LED.
Description
Technical field
The present invention is specifically related to a kind of structure of double perovskite red fluorescence powder and its preparation method and application, belongs to the fluorescent material field.
Background technology
White light LEDs be after incandescent light, fluorescent lamp and electricity-saving lamp the 4th generation lighting electric light source, be called as the 21 century green light source, there is environmental protection, overlong service life, energy-efficient, anti-adverse environment, simple in structure, volume is little, lightweight, response is fast, operating voltage is low and the good characteristics of security.It is trend of the times that the LED solid state light emitter substitutes the traditional lighting light source.
The mode that current white light LEDs sends white light is mainly to utilize the fluorescent material transformation approach.Business-like white light LEDs is that the InGaN tube core of emission blue streak (460nm) forms with the YAG:Ce of emission gold-tinted.This mode technique is simple, and cost is lower.But the method exists the shortcoming that color developing is poor, colour temperature is higher.Utilize this scheme to realize low colour temperature, high color rendering index (CRI) (Ra>80) that 5000K is following, the warm white LED of high brightness is more difficult.If add, can be improved colour rendering index, reduce colour temperature by blue-light excited red fluorescence powder, the photochromic meeting of LED becomes softer or bright-coloured, to adapt to different application needs.Yet research and development can more effectively be excited by blue light, the red fluorescence powder difficulty that photon conversion efficiency is higher is larger.The application of this type of LED fluorescent material is also at the early-stage, need to further carry out deep research and development.
The commercial red fluorescence powder that white light LEDs is used (Sr for example
2si
5n
8: Eu
2+, ZnS:Cu
2+deng) be confined to nitride, oxynitride and sulfide base material, there are complicated, the characteristics such as cost is higher, military service poor stability that prepare.Even, YAG:Ce
3+bloom has 20% luminous intensity decay under 80 ℃.Exploitation has good luminous characteristic, stable chemical nature, novel high-performance red LED fluorescent material that cost is low, extremely urgent.
Therefore the outstanding substrate material of fluorescent material is most important, must meet there is good chemical stability, suitable energy gap and crystalline structure and low production cost.In sum, the LED that finds good substrate material and then prepare the luminescent properties excellence has great science and realistic meaning with fluorescent material, the present invention just is being based on this purpose, the outstanding substrate material of performance of series of new is proposed, this series phosphor powder has strong emitting red light under blue streak excites, there is good stability and lower cost simultaneously, can make up the shortcoming of existing similar LED fluorescent material, there is larger using value.
Summary of the invention
The object of the present invention is to provide a kind of structure of double perovskite red fluorescence powder, preparation method and application thereof.Specifically the invention provides a kind of red fluorescence powder for White-light LED illumination excited by green glow chip, blue streak chip or near-ultraviolet light photodiode that can be used for, the chemical expression of described red fluorescence powder is Ln
2-xaMO
6: xEu, and its preparation method and application.In formula (in Ln=La, Gd and Y any one, two kinds or three kinds of combinations; In A=Li, Na and K any one, two kinds or three kinds of combinations; In M=Sb, Nb and Ta any one, two kinds or three kinds of combinations)
Technical scheme of the present invention is:
The red fluorescence powder that a kind of LED excites, the chemical formula of this material can be expressed as Ln
2-xaMO
6: xEu, in formula: any one or its combination that Ln is La, Gd and Y, any one or its combination that A is Li, Na and K, any one or its combination that M is Sb, Nb and Ta; Wherein, Ln=La
2-x-m-ngd
my
n(0≤m+n≤2-x, m and the combination of n arbitrary proportion, the doping that x is Eu), A=Li
1-y-zna
yk
z(0≤y+z≤1, y and the combination of z arbitrary proportion) and M=Sb
1-p-qnb
pta
q(0≤p+q≤1, p and the combination of q arbitrary proportion); Eu is luminescence center, and doping is positioned at the Ln position, doping value 0.01≤x≤1.0, and best x value is 0.2.The novel red luminescent material that this LED excites, under green glow chip (528-533nm), blue streak chip (460-470nm) or near-ultraviolet light chip (390-399nm) excite, launch as the fluorescence between 570-640nm, red fluorescence is between 600-620nm.
The red fluorescence powder Ln that LED excites
2-xaMO
6: xEu (Ln=La, Gd, Y; A=Li, Na, K; M=Sb, Nb, Ta) preparation be to adopt solid phase reaction method.At first press Ln
2-xaMO
6: xEu chemical constitution proportioning selects appropriate raw material to be prepared burden, and takes ball mill mixing, makes batch mixing refinement fully mixed; Then the batch mixing after ball milling is packed in corundum crucible or other container, carry out pre-burning in stove, temperature is 500～1000 ℃, and the time is 10～24h; Pre-burning gained powder is fired again at 800～1400 ℃ after grinding, and the reaction times is 12～48h; Last process can repeat; Prepared fluorescent powder ball milling, refinement and screening, obtain red fluorescence material; Or after batch mixing without pre-burning and, at 800～1400 ℃, the reaction times is directly to fire (embodiment 3) under the 12-48h condition.
The raw material of the Ln position that the present invention adopts is oxide compound, metal-powder, nitrate or acetate; Eu is oxide compound, and the raw material of A position is oxide compound, carbonate, nitrate; The raw material of M position is oxide compound or metal-powder.
Innovation of the present invention is Ln
2aMO
6material is by rare earth Eu
3+doping obtains the high brightness ruddiness excited by blue look LED, can be up to 20mol% in the doping content of Ln position, and do not cause fluorescent quenching, doping content is considerably beyond common fluorescent material optimum value (being usually less than 5-10%).The matrix of this fluorescent material has the above band gap of 3eV, and overall fluorescent powder table color is white, under blue streak excites, presents redness, very stable under concentrated acid, can overcome the YAG:Ce bloom and have the characteristic of decay under high-temperature (50-80 ℃).611nm place under blue streak excites fluorescent emission intensity reaches 980000～3600000.
Material of the present invention can be used for white light LEDs and be correlated with demonstration, illuminating device.Mentality of designing uniqueness of the present invention, raw material is cheap and easy to get, and preparation technology is simple, the stable chemical nature of material, the luminescent properties excellence, be desirable phosphor for white light LED candidate material.
The accompanying drawing explanation
La in Fig. 1: embodiment 1
1.8naTaO
6: the powder X-ray RD spectrum of 0.2Eu sample;
La in Fig. 2: embodiment 1
1.8naTaO
6: the excitation spectrum of 0.2Eu sample;
La in Fig. 3: embodiment 1
1.8naTaO
6: the emmission spectrum of 0.2Eu sample.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail, further to illustrate actual features of the present invention and significant progressive.
Embodiment 1,
At first by raw material La
2o
3, Na
2cO
3, Ta
2o
5, Eu
2o
3according to La
1.8naTaO
6: the stoichiometric ratio of 0.2Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement fully mixed; Then the batch mixing after ball milling is packed in corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder is fired again at 1400 ℃ after grinding, and the reaction times is 12h; Prepared fluorescent powder ball milling, refinement and screening, obtain the red fluorescence material (XRD is shown in Fig. 1) of pure phase, the excitation spectrum of sample is shown in Fig. 2, the fluorescent emission intensity at the 611nm place under the 465nm blue streak excites reaches 3060000 (seeing Fig. 3), the fluorescent emission intensity at the 611nm place under the 465nm blue streak excites reaches 1360000, and the fluorescent emission intensity at the 617nm place under the 395nm near ultraviolet excitation reaches 920000.
Embodiment 2,
At first by raw material La
2o
3, Na
2cO
3, Ta
2o
5, Eu
2o
3according to La
1.8naTaO
6: the stoichiometric ratio of 0.2Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement fully mixed; Then the batch mixing after ball milling is packed in corundum crucible, carry out pre-burning in stove, temperature is 500 ℃, and the time is 24h; Pre-burning gained powder is fired again at 1000 ℃ after grinding, and the reaction times is 12h; Pre-burning gained powder is fired again at 1400 ℃ after grinding, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening, obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at 611nm place of sample under the 465nm blue streak excites reaches 3500000.
Embodiment 3,
At first by raw material La
2o
3, Na
2cO
3, Ta
2o
5, Eu
2o
3according to La
1.8naTaO
6: the stoichiometric ratio of 0.2Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement fully mixed; Then the batch mixing after ball milling is packed in corundum crucible, without pre-burning, directly fired in stove, temperature is 1400 ℃, and the time is 48h.Prepared fluorescent powder ball milling, refinement and screening, obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at 611nm place of sample under the 465nm blue streak excites reaches 2000000.
Embodiment 4,
At first by raw material La
2o
3, Na
2cO
3, Ta
2o
5, Eu
2o
3according to La
1.99naTaO
6: the stoichiometric ratio of 0.01Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement fully mixed; Then the batch mixing after ball milling is packed in corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder is fired again at 1400 ℃ after grinding, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening, obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at 611nm place of sample under the 465nm blue streak excites reaches 1184000.
Embodiment 5,
At first by raw material La
2o
3, Na
2cO
3, Ta
2o
5, Eu
2o
3according to LaNaTaO
6: the stoichiometric ratio of Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement fully mixed; Then the batch mixing after ball milling is packed in corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder is fired again at 1400 ℃ after grinding, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening, obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at 611nm place of sample under the 465nm blue streak excites reaches 980000.
Embodiment 6,
At first by raw material Gd
2o
3, Li
2cO
3, Sb
2o
5, Eu
2o
3according to Gd
1.9liSbO
6: the stoichiometric ratio of 0.1Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement fully mixed; Then the batch mixing after ball milling is packed in corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder is fired again at 1400 ℃ after grinding, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening, obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at 611nm place of sample under the 465nm blue streak excites reaches 2240000.
Embodiment 7,
At first by raw material Y
2o
3, KNO
3, Nb
2o
5, Eu
2o
3according to Y
1.8kNbO
6: the stoichiometric ratio of 0.2Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement fully mixed; Then the batch mixing after ball milling is packed in corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder is fired again at 1400 ℃ after grinding, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening, obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at 611nm place of sample under the 465nm blue streak excites reaches 2720000.
Embodiment 8,
At first by raw material La
2o
3, Gd
2o
3, Na
2cO
3, Ta
2o
5, Eu
2o
3according to La
0.8gdNaTaO
6: the stoichiometric ratio of 0.2Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement fully mixed; Then the batch mixing after ball milling is packed in corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder is fired again at 1400 ℃ after grinding, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening, obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at 611nm place of sample under the 465nm blue streak excites reaches 2530000.
Embodiment 9,
At first by raw material La
2o
3, Gd
2o
3, Y
2o
3, Na
2cO
3, Ta
2o
5, Eu
2o
3according to La
0.8gd
0.5y
0.5naTaO
6: the stoichiometric ratio of 0.2Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement fully mixed; Then the batch mixing after ball milling is packed in corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder is fired again at 1400 ℃ after grinding, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening, obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at 611nm place of sample under the 465nm blue streak excites reaches 2850000.
Embodiment 10,
At first by raw material La (Ac)
3, Na
2cO
3, Sb
2o
5, Eu
2o
3according to La
1.8naSbO
6: the stoichiometric ratio of 0.2Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement fully mixed; Then the batch mixing after ball milling is packed in corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder is fired again at 1400 ℃ after grinding, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening, obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at 611nm place of sample under the 465nm blue streak excites reaches 2643000.
Embodiment 11,
At first by raw material La
2o
3, Na
2cO
3, Li
2cO
3, Ta
2o
5, Eu
2o
3according to La
1.8na
0.5li
0.5taO
6: the stoichiometric ratio of 0.2Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement fully mixed; Then the batch mixing after ball milling is packed in corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder is fired again at 1400 ℃ after grinding, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening, obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at 611nm place of sample under the 465nm blue streak excites reaches 2620000.
Embodiment 12,
At first by raw material La
2o
3, Na
2cO
3, Li
2cO
3, K
2cO
3, Ta
2o
5, Eu
2o
3according to La
1.8na
0.4li
0.3k
0.3taO
6: the stoichiometric ratio of 0.2Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement fully mixed; Then the batch mixing after ball milling is packed in corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder is fired again at 1400 ℃ after grinding, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening, obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at 611nm place of sample under the 465nm blue streak excites reaches 1800000.
Embodiment 13,
At first by raw material La
2o
3, Na
2cO
3, Ta
2o
5, Nb
2o
5, Eu
2o
3according to La
1.8naTa
0.5nb
0.5o
6: the stoichiometric ratio of 0.2Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement fully mixed; Then the batch mixing after ball milling is packed in corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder is fired again at 1400 ℃ after grinding, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening, obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at 611nm place of sample under the 465nm blue streak excites reaches 2020000.
Embodiment 14,
At first by raw material La
2o
3, Na
2cO
3, Ta
2o
5, Nb
2o
5, Sb
2o
5, Eu
2o
3according to La
1.8naTa
0.4nb
0.3sb
0.3o
6: the stoichiometric ratio of 0.2Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement fully mixed; Then the batch mixing after ball milling is packed in corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder is fired again at 1400 ℃ after grinding, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening, obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at 611nm place of sample under the 465nm blue streak excites reaches 1320000.
Embodiment 15,
At first by raw material La, Na
2o, Ta, Eu
2o
3according to La
1.8naTaO
6: the stoichiometric ratio of 0.2Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement fully mixed; Then the batch mixing after ball milling is packed in corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder is fired again at 1400 ℃ after grinding, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening, obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at 611nm place of sample under the 465nm blue streak excites reaches 2080000.
Embodiment 16,
At first by raw material La (NO
3)
3, NaNO
3, Ta, Eu
2o
3according to La
1.8naTaO
6: the stoichiometric ratio of 0.2Eu is carried out weighing, takes ball mill mixing, makes batch mixing refinement fully mixed; Then the batch mixing after ball milling is packed in corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder is fired again at 1400 ℃ after grinding, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening, obtain the red fluorescence material of pure phase, and the fluorescent emission intensity at 611nm place of sample under the 465nm blue streak excites reaches 1960000.
Claims (6)
1. a structure of double perovskite red fluorescence powder, is characterized in that the chemical formula of described red fluorescence powder is expressed as Ln
2-xaMO
6: xEu, in formula:
1. Eu is luminescence center, and doping is positioned at Ln position, doping 0.01≤x≤1.0;
2. Ln=La
2-x-m-ngd
my
n(0≤m+n≤2-x, m and the combination of n arbitrary proportion, the doping that x is Eu);
3. A=Li
1-y-zna
yk
z(0≤y+z≤1, y and the combination of z arbitrary proportion);
4. M=Sb
1-p-qnb
pta
q(0≤p+q≤1, p and the combination of q arbitrary proportion);
1) Ln be in La, Gd and Y any one, two kinds or three kinds of combinations;
2) A be in Li, Na and K any one, two kinds or three kinds of combinations;
3) M be in Sb, Nb and Ta any one, two kinds or three kinds of combinations.
2. the method for preparing red fluorescence powder as claimed in claim 1, is characterized in that adopting solid phase reaction method, and concrete steps are:
A) press Ln
2-xaMO
6: xEu chemical constitution proportioning selects appropriate raw material to be prepared burden, and takes ball mill mixing, makes batch mixing refinement fully mixed;
B) batch mixing after ball milling is packed in corundum crucible or other container, first carry out pre-burning or, without pre-burning, calcined temperature is 500～1000 ℃ in stove, the time is 10～24h; Pre-burning gained powder is fired again at 800～1400 ℃ after grinding, and the reaction times is 12～48h; Or without the mixture of the step (a) of pre-burning at 800-1400 ℃, the reaction times is directly to fire under the 12-48h condition;
C) the fluorescent powder ball milling, refinement and the screening that prepared by step (b).
3. by method claimed in claim 2, it is characterized in that:
1. the raw material of Ln position is oxide compound, metal-powder, nitrate or acetate;
2. the raw material of A position is oxide compound, carbonate or nitrate;
3. the raw material of M position is oxide compound or metal-powder.
4. the application of fluorescent material claimed in claim 1, is characterized in that in LED green glow chip, blue chip or near-ultraviolet light chip the red fluorescence for White-light LED illumination, for LED and relevant display and lighting device.
5. by application claimed in claim 4, it is characterized in that the red fluorescence of emission is between 600～620nm.
6. by application claimed in claim 5, it is characterized in that the fluorescent emission intensity at the 611nm place reaches 980000～3600000 under 465nm is blue-light excited.
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| CN115595153A (en) * | 2022-10-20 | 2023-01-13 | 四川化工职业技术学院（Cn） | Double perovskite type red fluorescent powder for LED, preparation method and application |
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