CN102250616A - 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 production 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, have environmental protection, overlong service life, energy-efficient, anti-adverse environment, simple in structure, volume is little, in light weight, 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 present white light LEDs sends white light mainly is to utilize the fluorescent material transformation approach.Business-like white light LEDs is that the InGaN tube core of emission blue streak (460nm) is formed with the YAG:Ce that launches gold-tinted.This mode technology is simple, and cost is lower.But this 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 difficult.Can then can be improved colour rendering index, reduce colour temperature by blue-light excited red fluorescence powder if add, the photochromic meeting of LED becomes softer or bright-coloured, to adapt to different application needs.Yet research and development can be excited by blue light is more effective, and the red fluorescence powder difficulty that photon conversion efficiency is higher is bigger.The application of this type of LED fluorescent material is also at the early-stage, need 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 of preparation.Even, YAG:Ce
3+Bloom has 20% luminous intensity decay under 80 ℃.Exploitation has the novel high-performance red LED fluorescent material that good luminous characteristic, chemical property are stable, cost is low, and is extremely urgent.
Therefore the outstanding substrate material of fluorescent material is most important, must satisfy have good chemical stability, suitable energy gap and crystalline structure and low production cost.In sum, the LED that seeks good substrate material and then preparation luminescent properties excellence has great science and realistic meaning with fluorescent material, the present invention just is being based on this purpose, a series of novel outstanding substrate materials of performance are proposed, this series phosphor powder has the intensive emitting red light under blue streak excites, have good stability and lower cost simultaneously, can remedy the shortcoming of existing similar LED fluorescent material, have bigger 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 that is used for White-light LED illumination of being excited by green glow chip, blue streak chip or near-ultraviolet light photodiode of can be used for, the chemical expression of described red fluorescence powder is Ln
2-xAMO
6: xEu, and its production and application.In the formula (among Ln=La, Gd and the Y any one, two kinds or three kinds of combinations; Among A=Li, Na and the K any one, two kinds or three kinds of combinations; Among M=Sb, Nb and the 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 the formula: Ln is any one or its combination of La, Gd and Y, and A is any one or its combination of Li, Na and K, and M is any one or its combination of Sb, Nb and Ta; Wherein, Ln=La
2-x-m-nGd
mY
n(x is the doping of Eu for 0≤m+n≤2-x, m and the combination of n arbitrary proportion), 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 a luminescence center, mixes to be positioned at the Ln position, and doping value 0.01≤x≤1.0, best x value is 0.2.The novel red luminescent material that this LED excites, excite down at green glow chip (528-533nm), blue streak chip (460-470nm) or near-ultraviolet light chip (390-399nm), launch and be the fluorescence between the 570-640nm, red fluorescence is between the 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 for use an amount of raw material to prepare burden, and takes ball mill mixing, makes batch mixing refinement and fully mixed; Then the batch mixing behind the 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 grinds the back and fires once more at 800～1400 ℃, and the reaction times is 12～48h; Last process can repeat; Prepared fluorescent powder ball milling, refinement and screening promptly obtain red fluorescence material; Or behind the 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 an 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 part of the present invention is Ln
2AMO
6Material is by rare earth Eu
3+Mix to obtain the high brightness ruddiness that excites by blue look LED, can be in the doping content of Ln position up to 20mol%, 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, presents redness under blue streak excites, and is very stable under concentrated acid, can overcome the YAG:Ce bloom has decay under high-temperature (50-80 ℃) characteristic.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, and the chemical property of material is stable, and the luminescent properties excellence is an ideal phosphor for white light LED candidate material.
Description of drawings
La among Fig. 1: the embodiment 1
1.8NaTaO
6: the powder X-ray RD spectrum of 0.2Eu sample;
La among Fig. 2: the embodiment 1
1.8NaTaO
6: the excitation spectrum of 0.2Eu sample;
La among Fig. 3: the 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 obvious improvement.
Embodiment 1,
At first with 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 and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 12h; Prepared fluorescent powder ball milling, refinement and screening, promptly obtain the red fluorescence material (XRD sees Fig. 1) of pure phase, the excitation spectrum of sample is seen Fig. 2, the fluorescent emission intensity at the 611nm place under the 465nm blue streak excites reaches 3060000 (see figure 3)s, 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 with 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 and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 500 ℃, and the time is 24h; Pre-burning gained powder grinds the back and fires once more at 1000 ℃, and the reaction times is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening promptly 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 with 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 and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, without pre-burning, directly fire in stove, temperature is 1400 ℃, and the time is 48h.Prepared fluorescent powder ball milling, refinement and screening promptly 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 with 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 and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening promptly 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 with 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 and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening promptly 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 with 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 and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening promptly 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 with 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 and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening promptly 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 with 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 and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening promptly 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 with 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 and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening promptly 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.
At first with 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 and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening promptly 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 with 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 and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening promptly 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 with 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 and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening promptly 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 with 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 and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening promptly 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 with 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 and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening promptly 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 with 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 and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening promptly 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 with 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 and fully mixed; Then the batch mixing behind the ball milling is packed in the corundum crucible, carry out pre-burning in stove, temperature is 1000 ℃, and the time is 12h; Pre-burning gained powder grinds the back and fires once more at 1400 ℃, and the reaction times is 12h.Prepared fluorescent powder ball milling, refinement and screening promptly 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 (8)
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 the formula:
1. Eu is a luminescence center, mixes to be positioned at Ln position, doping 0.01≤X≤1.0;
2. Ln=La
2-x-m-nGd
mY
n(x is the doping of Eu for 0≤m+n≤2-x, m and the combination of n arbitrary proportion);
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).
2. by the described red fluorescence powder of claim 1, it is characterized in that:
The doping X=0.2 of Eu.
3. by the described red fluorescence powder of claim 1, it is characterized in that
1) Ln be among La, Gd and the Y any one, two kinds or three kinds of combinations;
2) A be among Li, Na and the K any one, two kinds or three kinds of combinations;
3) M be among Sb, Nb and the Ta any one, two kinds or three kinds of combinations;
The preparation as in the claim 1～3 each, the method for described red fluorescence powder is characterized in that adopting solid phase reaction method, concrete steps are:
A) press Ln
2-xAMO
6: xEu chemical constitution proportioning selects for use an amount of raw material to prepare burden, and takes ball mill mixing, makes batch mixing refinement and fully mixed;
B) batch mixing behind the ball milling is packed in corundum crucible or other container, carry out pre-burning earlier or without pre-burning, calcined temperature is 500～1000 ℃ in stove, the time is 10～24h; Pre-burning gained powder grinds the back and fires once more at 800～1400 ℃, 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) fluorescent powder ball milling, refinement and the screening that step (b) is prepared.
5. by the described method of claim 4, 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.
6. the application of the described fluorescent material of claim 1 is characterized in that being used for the red fluorescence of White-light LED illumination in LED green glow chip, blue streak chip or near-ultraviolet light chip, be used for LED and relevant the demonstration and illuminating device.
7. by the described application of claim 6, the red fluorescence that it is characterized in that launching is between 600～620nm.
8. by the described application of claim 7, the fluorescent emission intensity at the 611nm place reaches 980000～3600000 to it is characterized in that exciting down at the 465nm blue streak.
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