CN102660265B - Eu2+ activated borate yellow fluorescent powder and preparing method thereof - Google Patents
Eu2+ activated borate yellow fluorescent powder and preparing method thereof Download PDFInfo
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Abstract
The invention relates to Eu2+ activated borate yellow fluorescent powder and a preparing method thereof, belonging to the technical field of inorganic light-emitting materials. The chemical general formula of the fluorescent powder is Ba1-xEuxCsB3O6, wherein x is the mole percent of Eu2+ doping, and is greater than or equal to 0.0001 and less than or equal to 0.25. The method comprises the following step of: weighing each raw material according to the stoichiometric ratio of the corresponding element in the formula so as to obtain the product by a high-temperature solid phase method or a chemical solution method. The Eu2+ activated borate yellow fluorescent powder emits bright yellow fluorescent light under excitation of 350-400 nm near ultraviolet, and is high in luminous intensity, wide in excitation wavelength, and good in stability and color rendering property; and the emission wavelength of the borate yellow fluorescent powder is very coincided with that of a near ultraviolet semiconductor chip. The method provided by the invention is simple and good in reproducibility; the product obtained by the method is stable in quality; and the method is easy for operation and industrial production.
Description
Technical field
The present invention relates to a kind of fluorescence luminescent material and preparation method thereof, particularly a kind ofly under near ultraviolet excitation, launch fluorescent material of yellow fluorescence and preparation method thereof, it can be applicable to, in the white light LEDs of near ultraviolet excitation, belong to fluorescent material technical field.
Background technology
White light LEDs is the green light source getting most of the attention 21 century, has wide market and application prospect.Adopt near-ultraviolet light 350～410nm InGaN tube core to excite three primary colors fluorescent powder to realize white light LEDs and become at present one of focus of these field research and development in the world, be considered to the leading of White-light LED illumination of new generation, and the fluorescent material of efficient near ultraviolet excitation lacks at present very much.
Fluorescent RE powder for white light LEDs must meet two conditions, and the firstth, the excitation spectrum of fluorescent material will match with the emmission spectrum of selected photodiode, guarantees to obtain higher light conversion efficiency; The secondth, fluorescent material is under the exciting of UV-light, and its emmission spectrum can send white light, or the blue light of the light sending under the exciting of blue light and photodiode ejaculation is compounded to form white light.
At present, the technology of preparing of white light LEDs mainly contains 3 kinds: the combination of (1) red, green, blue three-color LED, and this method can arbitrarily be adjusted color, but power supply is complicated, and cost is higher.(2) blue-ray LED and YAG (Y
3al
5o
12): Ce
3+yellow fluorescent powder combination, this method relative cost is lower, and efficiency is higher, but owing to lacking red composition, colour rendering index is poor; In addition, because the absorption peak of the light-converting material of blue-light LED chip requires to be positioned at 420-470nm, the fluorescent material that can meet this requirement is considerably less, absorption intensity neither be very large, find this class fluorescent material and have suitable difficulty, so the wavelength of LED chip, along with the development of manufacturing process, more and more moves toward shortwave direction, makes " near ultraviolet (360～410nm) type white light LEDs (NUV-LED) " become the most active system of current research.(3) combination of ultraviolet or near ultraviolet LED and three primary colors fluorescent powder, this method color developing is best, but luminous efficiency is lower.Therefore, development of new redness, green and blue colour fluorescent powder efficient, Heat stability is good is the key that improves white light LEDs luminous mass.
Borate is the emphasis of people as luminous host research for a long time always, and the borate of different ions doping has been carried out to a large amount of research and development.Be (Y as U.S. patent of invention USP6042747 discloses a kind of chemical formula
1-a-b-cgd
cm
beu
a) BO
3novel borate rouge and powder material, wherein, 0.01≤a≤0.1,0.1≤b≤0.5, C≤0.1; Chinese invention patent CN101696356A discloses a kind of manufacture method of borate green emitting phosphor, is a kind of green emitting phosphor take borate as matrix, and it is (Y that formula adopts chemical formula
1-x-y-zgd
xm
ytb
z) BO
3, wherein 0 < x < 0.5,0.0 < y < 0.05,0.1 < z < 1.0, M is Al, Se or Ce element.
Summary of the invention
The object of the present invention is to provide a kind of degree of crystallinity high, luminous intensity is high, excitation wave length and width, stability and color developing good, with low cost, and preparation technology is simple, be easy to suitability for industrialized production, near ultraviolet excitated borate yellow fluorescence luminescent material and preparation method thereof.
For reaching above object, the technical solution used in the present invention is to provide a kind of Eu
2+the borate yellow fluorescent powder activating, its chemical general formula is Ba
1-xeu
xcsB
3o
6, wherein,
xfor Eu
2+the molecular fraction of doping, 0.0001≤
x≤ 0.25.
A kind of Eu provided by the invention
2+the borate yellow fluorescent powder activating, its preparation method adopts high temperature solid-state method, comprises the following steps:
(1) to contain barium ion Ba
2+compound, contain europium ion Eu
2+compound, contain Cs
+compound, contain B
3+compound be raw material, by Formula B a
1-xeu
xcsB
3o
6the stoichiometric ratio of middle corresponding element takes each raw material, wherein
xfor Eu
2+the molecular fraction of doping, 0.0001≤
x≤ 0.25; The raw material taking is ground respectively, mix;
(2) by mixture under the temperature condition of 100～250 ℃ drying treatment to without fixed shape;
(3) step (2) is obtained dry, without fixed mixture naturally cooling, grind and mix, under air atmosphere, calcine, calcining temperature is 200～500 ℃, calcination time is 1～5 hour;
(4) after naturally cooling, grind and mix, under reducing atmosphere, calcine, calcining temperature is 500～900 ℃, and calcination time is 2～8 hours, obtains a kind of borate yellow fluorescent powder.
A kind of Eu provided by the invention
2+the borate yellow fluorescent powder activating, its preparation method adopts chemical solution method, comprises the following steps:
(1) to contain barium ion Ba
2+compound, contain europium ion Eu
2+compound, contain Cs
+compound, contain B
3+compound be raw material, by Formula B a
1-xeu
xcsB
3o
6the stoichiometric ratio of middle corresponding element takes each raw material, wherein
xfor Eu
2+the molecular fraction of doping, 0.0001≤
x≤ 0.25; By the material dissolution taking, in deionized water or nitric acid, then the 0.5～2.0wt% that presses total reactant quality adds complexing agent citric acid or oxalic acid, obtains mixed solution;
(2) step (1) is obtained to mixed solution and be heated to 50～100 ℃, stir 1～2 hour, after leaving standstill, drying, obtain fluffy presoma;
(3) presoma is placed in to calcining for the first time among air atmosphere, calcining temperature is 250～400 ℃, is incubated 1～4 hour; Calcining for the second time in reducing atmosphere after again the powder obtaining being ground, calcining temperature is 450～900 ℃, is incubated 2～10 hours, obtains a kind of borate yellow fluorescent powder.
The barium ion Ba that contains of the present invention
2+compound be a kind of in barium oxide, nitrate of baryta, barium carbonate, barium sulfate or their combination; The described europium ion Eu that contains
3+compound be a kind of in europium sesquioxide, europium nitrate or their combination; The described cesium ion Cs that contains
+compound be a kind of in Cs2O, cesium carbonate, cesium hydroxide, cesium nitrate, cesium sulfate, cesium oxalate or their combination; The described boron ion B that contains
3+compound be a kind of in boric acid, boron trioxide or their combination.
Eu provided by the invention
2+the preparation method of the borate yellow fluorescent powder activating, while adopting high temperature solid-state method to prepare, preferred scheme is: the temperature condition of drying treatment is 150～200 ℃; Reducing atmosphere is the atmosphere that is connected with carbon monoxide or hydrogen.
Eu provided by the invention
2+the preparation method of the borate yellow fluorescent powder activating, while adopting chemical solution method to prepare, preferred scheme is: calcining temperature is 300～400 ℃ for the first time, and calcination time is 2～4 hours; Calcining temperature is 450～850 ℃ for the second time, and calcination time is 2～7 hours; Reducing atmosphere is the atmosphere that is connected with carbon monoxide or hydrogen.
Compared with prior art, the remarkable advantage of technical solution of the present invention is:
1, the substrate material that technical solution of the present invention provides, be easy to the reduction of the divalence that realizes rare earth ion, and bivalent rare earth ion can stable existence among this matrix, the light that the InGaN tube core of its excitation area and 350～410nm near-ultraviolet radiation of use at present excites matches, therefore, can be applied in the LED fluorescent material that the InGaN tube core of near-ultraviolet radiation excites.
2, the fluorescent material making has good luminous intensity, stability, color developing and granularity, is conducive to realize the high-power LED of preparation.
The CIE coordinate of the fluorescent material 3, making is x=0.4235, and y=0.5247 sends gold-tinted under ultraviolet excitation, coordinates other color fluorescent material can prepare white light LEDs.
Accompanying drawing explanation
Fig. 1 is the X-ray powder diffraction collection of illustrative plates of the material sample prepared by the technology of the present invention;
Fig. 2 is the luminescent spectrum figure that the material sample to preparing by the technology of the present invention obtains under 355nm is near ultraviolet excitated;
Fig. 3 is the material sample exciting light spectrogram under 545 nm and 620 nm respectively of preparing by the technology of the present invention;
Fig. 4 is the decay of luminescence figure that material sample prepared by the embodiment of the present invention obtains under 550nm excites.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described.
According to chemical formula CsBa
0.93eu
0.07b
3o
6in the stoichiometric ratio of each element, weigh respectively Cs
2cO
3: 1.086 grams, BaCO
3: 1.2236 grams, H
3bO
3: 1.2366 grams, Eu
2o
3: 0.0821 gram, after grinding in agate mortar and mixing, select air atmosphere drying treatment, the temperature of calcining is 160 ℃, calcination time 2 hours, then be chilled to room temperature, take out sample without fixed phenomenon, even abundant compound mixed grinding, among air atmosphere, calcining for the second time at 200 ℃, calcination time is 1.5 hours, is cooled to room temperature, takes out sample, again even abundant compound mixed grinding, among reducing atmosphere, sintering for the third time at 500 ℃, sintering time is 3 hours, be cooled to room temperature, obtain target product.
Referring to accompanying drawing 1, it is the X-ray powder diffraction collection of illustrative plates of the material sample prepared by the present embodiment technology.Test result demonstration, prepared material is single-phase CsBaB
3o
6material.
Referring to accompanying drawing 2, it is that material sample to preparing by the present embodiment technology detects the utilizing emitted light spectrogram that 355nm obtains under near ultraviolet excitated, as can be seen from the figure, emission peak is a broadband, main peak is positioned near 550nm, illustrates that this sample can be applicable in LED green emitting phosphor that the InGaN tube core of near ultraviolet (350～410nm) radiation excites.
Referring to accompanying drawing 3, it is the material sample excitation spectrum under 545 nm and 620 nm respectively of preparing by the present embodiment technology, and excitation peak is asymmetric broadband.
Referring to accompanying drawing 4, it is the decay of luminescence figure that material sample prepared by the present embodiment obtains under 550nm excites, the luminous life-span is about 200 nanoseconds, is the characteristic decay of divalent europium, and result shows does not have twilight sunset.
Embodiment 2
According to chemical formula CsBa
0.995eu
0.005b
3o
6in the stoichiometric ratio of each element, weigh respectively Cs
2cO
3: 1.086 grams, Ba (NO
3)
2: 1.7336 grams, H
3bO
3: 1.2366 grams, Eu (NO
3)
2: 0.00833 gram, after grinding in agate mortar and mixing, select air atmosphere to calcine for the first time, temperature is 170 ℃, calcination time 2.5 hours, is then chilled to room temperature, takes out sample.After the raw material of calcining for the first time, again even abundant compound mixed grinding, among air atmosphere, calcining for the second time at 250 ℃, calcination time is 2 hours, is cooled to room temperature, take out sample, after the raw material of calcining for the second time, again even abundant compound mixed grinding, among reducing atmosphere, sintering for the third time at 550 ℃, sintering time is 4 hours, is cooled to room temperature, obtains target product.Main structure properties, excitation spectrum and luminescent spectrum are similar to embodiment 1.
Embodiment 3
According to chemical formula CsBa
0.99eu
0.01b
3o
6in the stoichiometric ratio of each element, weigh respectively Cs
2cO
3: 1.086 grams, BaCO
3: 1.306 grams, H
3bO
3: 1.2366 grams, Eu (NO
3)
2: 0.016667 gram, after grinding in agate mortar and mixing, select air atmosphere to calcine for the first time, temperature is 180 ℃, calcination time 3 hours, is then chilled to room temperature, takes out sample.After the raw material of calcining for the first time, again even abundant compound mixed grinding, among air atmosphere, calcining for the second time at 300 ℃, calcination time is 3 hours, is cooled to room temperature, take out sample, after the raw material of calcining for the second time, again even abundant compound mixed grinding, among reducing atmosphere, sintering for the third time at 600 ℃, sintering time is 4 hours, is cooled to room temperature, obtains target product.Main structure properties, excitation spectrum and luminescent spectrum are similar to embodiment 1.
Embodiment 4
According to chemical formula CsBa
0.97eu
0.03b
3o
6in the stoichiometric ratio of each element, weigh respectively Cs
2cO
3: 1.086 grams, BaCO
3: 1.2762 grams, H
3bO
3: 1.2366 grams, Eu
2o
3: 0.03872 gram, after grinding in agate mortar and mixing, select air atmosphere to calcine for the first time, temperature is 190 ℃, calcination time 3.5 hours, is then chilled to room temperature, takes out sample.After the raw material of calcining for the first time, again even abundant compound mixed grinding, among air atmosphere, calcining for the second time at 350 ℃, calcination time is 3.5 hours, is cooled to room temperature, take out sample, after the raw material of calcining for the second time, again even abundant compound mixed grinding, among reducing atmosphere, sintering for the third time at 700 ℃, sintering time is 4 hours, is cooled to room temperature, obtains target product.Main structure properties, excitation spectrum and luminescent spectrum are similar to embodiment 1.
Embodiment 5
According to chemical formula CsBa
0.95eu
0.05b
3o
6in the stoichiometric ratio of each element, weigh respectively Cs
2cO
3: 1.086 grams, Ba (NO
3)
2: 1.655 grams, H
3bO
3: 1.2366 grams, Eu
2o
3: 0.0587 gram, then take the citric acid of the 0.5wt% of above medicine total mass; By the Eu taking
2o
3with appropriate nitric acid dissolve, add appropriate deionized water and citric acid post-heating to 55 ℃ to carry out stir process; In above-mentioned solution, add Cs
2cO
3, H
3bO
3, Ba (NO
3)
2, heated and stirred 2 hours, leaves standstill, and dries, and obtains fluffy presoma; Presoma is placed in to air and calcines, calcining temperature is 300 ℃, and calcination time is 2 hours; The powder obtaining is ground in the retort furnace that is placed on reducing atmosphere protection and calcined, and calcining temperature is 500 ℃, and calcination time is 3 hours, obtains a kind of borate yellow fluorescent powder.Main structure properties, excitation spectrum and luminescent spectrum are similar to embodiment 1.
Embodiment 6
According to chemical formula CsBa
0.9eu
0.1b
3o
6in the stoichiometric ratio of each element, weigh respectively Cs
2cO
3: 1.086 grams, Ba (NO
3)
2: 1.1841 grams, H
3bO
3: 1.2366 grams, Eu (NO
3)
2: 0.0833 gram, take the citric acid of the 0.5wt% of above medicine total mass; To take to obtain Eu (NO
3)
2with appropriate nitric acid dissolve, add appropriate deionized water and citric acid post-heating to 55 ℃ to carry out stir process; In above-mentioned solution, add Cs
2cO
3, H
3bO
3, Ba (NO
3)
2, heated and stirred leaves standstill for 2 hours, dries, and obtains fluffy presoma; Presoma is placed in to air and calcines, calcining temperature is 400 ℃, and calcination time is 4 hours; The powder obtaining is ground in the retort furnace that is placed on reducing atmosphere protection and calcined, and calcining temperature is 800 ℃, and calcination time is 6 hours, obtains a kind of borate yellow fluorescent powder.Main structure properties, excitation spectrum and luminescent spectrum are similar to embodiment 1.
Embodiment 7
According to chemical formula CsBa
0.8eu
0.2b
3o
6in the stoichiometric ratio of each element, weigh respectively Cs
2cO
3: 1.086 grams, Ba (NO
3)
2: 1.3983 grams, H
3bO
3: 1.2366 grams, Eu
2o
3: 0.2346 gram, take the citric acid of the 0.5wt% of above medicine total mass; To take to obtain Eu
2o
3with appropriate nitric acid dissolve, add appropriate deionized water and citric acid post-heating to 55 ℃ to carry out stir process; In above-mentioned solution, add Cs
2cO
3, H
3bO
3, Ba (NO
3)
2, heated and stirred leaves standstill for 2 hours, dries, and obtains fluffy presoma; Presoma is placed in to air and calcines, calcining temperature is 350 ℃, and calcination time is 3 hours; The powder obtaining is ground in the retort furnace that is placed on reducing atmosphere protection and calcined, and calcining temperature is 700 ℃, and calcination time is 5 hours, obtains a kind of borate yellow fluorescent powder.Main structure properties, excitation spectrum and luminescent spectrum are similar to embodiment 1.
Claims (9)
1. an Eu
2+the borate yellow fluorescent powder activating, is characterized in that: its chemical general formula is Ba
1-xeu
xcsB
3o
6, wherein,
xfor Eu
2+the molecular fraction of doping, 0.0001≤
x≤ 0.25.
2. an Eu as claimed in claim 1
2+the preparation method of the borate yellow fluorescent powder activating, is characterized in that adopting high temperature solid-state method, comprises the following steps:
(1) to contain barium ion Ba
2+compound, contain europium ion Eu
2+compound, contain Cs
+compound, contain B
3+compound be raw material, by Formula B a
1-xeu
xcsB
3o
6the stoichiometric ratio of middle corresponding element takes each raw material, wherein
xfor Eu
2+the molecular fraction of doping, 0.0001≤
x≤ 0.25; The raw material taking is ground respectively, mix;
(2) by mixture under the temperature condition of 100～250 ℃ drying treatment to without fixed shape;
(3) step (2) is obtained dry, without fixed mixture naturally cooling, grind and mix, under air atmosphere, calcine, calcining temperature is 200～500 ℃, calcination time is 1～5 hour;
(4) after naturally cooling, grind and mix, under reducing atmosphere, calcine, calcining temperature is 500～900 ℃, and calcination time is 2～8 hours, obtains a kind of borate yellow fluorescent powder.
3. a kind of Eu according to claim 2
2+the preparation method of the borate yellow fluorescent powder activating, is characterized in that: the drying temperature of step (2) is 150～200 ℃.
4. an Eu as claimed in claim 1
2+the preparation method of the borate yellow fluorescent powder activating, is characterized in that adopting chemical solution method, comprises the following steps:
(1) to contain barium ion Ba
2+compound, contain europium ion Eu
2+compound, contain Cs
+compound, contain B
3+compound be raw material, by Formula B a
1-xeu
xcsB
3o
6the stoichiometric ratio of middle corresponding element takes each raw material, wherein
xfor Eu
2+the molecular fraction of doping, 0.0001≤
x≤ 0.25; By the material dissolution taking, in deionized water or nitric acid, then the 0.5～2.0wt% that presses total reactant quality adds complexing agent citric acid or oxalic acid, obtains mixed solution;
(2) step (1) is obtained to mixed solution and be heated to 50～100 ℃, stir 1～2 hour, after leaving standstill, drying, obtain fluffy presoma;
(3) presoma is placed in to calcining for the first time among air atmosphere, calcining temperature is 250～400 ℃, is incubated 1～4 hour; Calcining for the second time in reducing atmosphere after again the powder obtaining being ground, calcining temperature is 450～900 ℃, is incubated 2～10 hours, obtains a kind of borate yellow fluorescent powder.
5. according to a kind of Eu described in claim 2 or 4
2+the preparation method of borate yellow fluorescent powder who activates, is characterized in that: the described barium ion Ba that contains
2+compound be a kind of in barium oxide, nitrate of baryta, barium carbonate, barium sulfate or their combination.
6. according to a kind of Eu described in claim 2 or 4
2+the preparation method of borate yellow fluorescent powder who activates, is characterized in that: the described cesium ion Cs that contains
+compound be a kind of in Cs2O, cesium carbonate, cesium hydroxide, cesium nitrate, cesium sulfate, cesium oxalate or their combination.
7. according to a kind of Eu described in claim 2 or 4
2+the preparation method of borate yellow fluorescent powder who activates, is characterized in that: the described boron ion B that contains
3+compound be a kind of in boric acid, boron trioxide or their combination.
8. a kind of Eu according to claim 4
2+the preparation method of the borate yellow fluorescent powder activating, is characterized in that: step (3) for the first time calcining temperature is 300～400 ℃, and calcination time is 2～4 hours; Calcining temperature is 450～850 ℃ for the second time, and calcination time is 2～7 hours.
9. according to a kind of Eu described in claim 2 or 4
2+the preparation method of the borate yellow fluorescent powder activating, is characterized in that: described reducing atmosphere is the atmosphere that is connected with carbon monoxide or hydrogen.
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| CN100454603C (en) * | 2005-01-10 | 2009-01-21 | 清华大学 | Organic electroluminescent device |
| TWI362413B (en) * | 2008-02-25 | 2012-04-21 | Ind Tech Res Inst | Borate phosphor and white light illumination device utilizing the same |
| CN101545138B (en) * | 2008-03-25 | 2012-08-22 | 中国科学院福建物质结构研究所 | Non-linear optical crystal-sodium beryllate borate, growth method and application thereof |
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Application publication date: 20120912 Assignee: Jiangxi Dongpeng New Materials Co., Ltd. Assignor: Soochow University Contract record no.: 2014320010163 Denomination of invention: Eu2+ activated borate yellow fluorescent powder and preparing method thereof Granted publication date: 20140514 License type: Exclusive License Record date: 20141015 |
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