CN103396800B - Boron aluminate-based blue fluorescent powder, preparation method and application - Google Patents
Boron aluminate-based blue fluorescent powder, preparation method and application Download PDFInfo
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- CN103396800B CN103396800B CN201310324671.9A CN201310324671A CN103396800B CN 103396800 B CN103396800 B CN 103396800B CN 201310324671 A CN201310324671 A CN 201310324671A CN 103396800 B CN103396800 B CN 103396800B
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Abstract
The invention relates to boron aluminate-based blue fluorescent powder, a preparation method and an application, belonging to the technical field of inorganic luminous materials. The fluorescent powder is boron aluminate-based fluorescent powder activated by rare earth ions, the chemical formula is La1-xCexAl2B3O9, x represents the molar percent coefficient of Ce doped in a La position, x is not less than 0.005 and not more than 0.05, and the fluorescent powder is prepared by adopting a high-temperature solid phase method. The rare earth boron aluminate blue fluorescent powder provided by the invention can be effectively excited by ultraviolet light, the range of exciting light is 250-350nm, the emission wavelength is 350-500nm, the luminous intensity is high, the stability is good, and the rare earth boron aluminate blue fluorescent powder becomes an excellent blue component in high color rendering fluorescent powder and can be applied to lighting taking the ultraviolet light as an exciting source, and chromaticity regulation of display devices and photoluminescence. The sintering process of the fluorescent powder provided by the invention is simple, easy to operate and good in reproducibility, and the obtained product is stable in quality and suitable for industrial production.
Description
Technical field
The present invention relates to a kind of phosphor, particularly a kind of by the fluorescent material of ultraviolet excitation, preparation method and application thereof, belong to rare earth luminescent material technical field.
Background technology
The successful research and development of high brightness GaN blue LED and the white light LEDs of realizing have thus been described as maximum light source revolution since the Edison invented incandescent light that continues.Because its photoelectric efficiency having is high, the life-span is long, volume is little, power is low, the advantage such as solid-state energy-conservation and environmental protection, white light LEDs product is just attracting increasing concern.Energy-saving illumination is one of body matter of low-carbon economy.And rare-earth luminescent material is the critical material in electricity-saving lamp and white light LEDs light fixture, it has great importance for the performance index such as luminous efficiency, work-ing life, colour temperature, colour rendering index of improving such LED.
At present, the method for utilizing LED technology to realize white light mainly contains three kinds: the direct mixed-color method of three-primary color LED, ultraviolet transformation approach and blue chip add the method for yellow fluorescent powder.Wherein, the direct mixed-color method of three-primary color LED is directly the three primary colours chip portfolio of transmitting red, green, blue wavelength to be packaged together, and forms multi-chip type white light LEDs, by spacing color mixed principle, mate in accordance with the appropriate ratio, make the light of three kinds of colors be mixed into white light.But the weakness of this method is its mounting structure more complicated, the driving voltage of LED of all kinds, luminous efficiency, light distribution characteristic difference, need to pass through the intensity of current setting red, green, blue three primary colours, and circuit is more complicated on realizing.The method that blue chip adds yellow fluorescent powder is that the blue light (approximately 450 nanometer) that GaN base LED chip is sent carrys out excitation rare-earth fluorescent material YAG (Y
3al
5o
12): Ce
3+send gold-tinted, thereby form white light.But, because of shortcomings such as it lack red light portion radiation, and product exists colour rendering index low, and color reducibility is poor, in widespread adoption and the popularization of high-end lighting field, be restricted.And ultraviolet transformation approach becomes current main flow gradually, because it can, for fluorescent material provides higher excitation energy, be realized wavelength Conversion by fluorescent material and send visible ray.The combination of ultraviolet LED and three primary colors fluorescent powder, its color developing is best, and fluorescent material 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.
At present, can be used for being excited the blue colour fluorescent powder of use also few by ultraviolet LED.Wherein the more blue colour fluorescent powder of use adopts divalent europium (Eu conventionally
2+) as luminescence center, mainly take high temperature solid-state method as main.As commercial blue colour fluorescent powder BaMgAl
10o
17: Eu
2+, because its luminous efficiency is low, blue light is easy to, by red and green emitting phosphor absorption etc., affect ultraviolet-near ultraviolet excitated three primary colors fluorescent powder luminescent properties, thereby white light LEDs performance is reduced; Chinese invention patent CN101497791A discloses a kind of rare earth aluminate blue colour fluorescent powder and preparation method thereof and application, and its chemical formula is Mg
1-x-ysr
yal
2o
4: Eu
x(in formula, x is the mole number of europium atom, y is the mole number of strontium atom, 0.005≤x≤0.10,0.01≤y≤0.14), it is 463 nanometers that fluorescence spectrum is tested its transmitting main peak, and excitation center wavelength is 330 nanometers, sends blue light, but this process relates to the pre-treatment, batching, sintering, washing of raw material etc., preparation is relatively complicated; Chinese invention patent CN1605612A discloses a kind of RE(rare earth) borate blue colour fluorescent powder and preparation method thereof, and its molecular formula is (EuO)
m(MO)
n(B
2o
3)
p(MX
2)
q(wherein M is a kind of of Mg, Ca, Sr and Ba or its mixing, and X is a kind of or its mixing of Cl and Br and I; M, n, q>=0), this fluorescent material can be by ultraviolet ray excited, emmission spectrum main peak, between 430～460 nanometers, sends the blue light of higher-strength, but this fluorescent material component is more, can there is a certain amount of dephasign in final product, also relate to the dry operation that waits of spraying, and is unfavorable for actual production; And for example Chinese invention patent CN1190115A discloses BaMgAl
14o
23: the preparation method of Eu blue colour fluorescent powder is that carbon dust is directly covered on starting material, and this preparation method, because carbon dust is directly to contact with starting material, causes fluorescent material part Prevent Carbon Contamination, thereby causes the waste of starting material in preparation process.Therefore, this preparation method can not meet the needs of actual production well.The europium ion of divalence is not easy reduction fully, so this has also limited its luminescence center as blue colour fluorescent powder.
The substrate material that aluminium borate system provides, be easy to realize the trivalent reduction of rare earth ion, and trivalent rare earth ions is energy stable existence in this matrix, also there are raw material sources abundant simultaneously, the advantages such as synthesis technique adaptability is extensive, the high sapphirine aluminium borate system fluorescent material that searching is effectively excited at ultraviolet band, is expected to be used in white light LEDs field.
Summary of the invention
The deficiency existing in order to overcome prior art, the object of this invention is to provide a kind ofly there is stable performance, luminous intensity is high, aluminium borate base blue colour fluorescent powder that manufacturing process is simple, pollution-free, cost is low and preparation method thereof, it can be excited by ultraviolet leds, is applied to white light LEDs illuminating device.
For reaching above object, the technical solution used in the present invention is: a kind of aluminium borate base blue colour fluorescent powder is provided, and its chemical formula is La
1-x ce
x al
2b
3o
9, in formula, x represents the molecular fraction coefficient of La position Ce doping, 0.005≤x≤0.05; At wavelength, be that under the ultraviolet excitation of 250～350 nanometers, emission wavelength, between 350～500 nanometers, sends blue-fluorescence.
A method of preparing aluminium borate base blue colour fluorescent powder as above, adopts high temperature solid-state method, comprises the following steps:
1, to contain aluminum ion Al
3+compound, contain boron ion B
3+compound, contain lanthanum ion La
3+compound, contain cerium ion Ce
3+compound be raw material, by molecular formula La
1-x ce
x al
2b
3o
9the stoichiometric ratio of middle corresponding element takes each raw material, and x represents the molecular fraction coefficient of La position Ce doping, 0.005≤x≤0.05; The raw material taking is ground respectively, and remix is even, obtains mixture;
2, this mixture is calcined under air atmosphere, calcining temperature is 100～500 ℃, and calcination time is 1～12 hour;
3, by the mixture naturally cooling after calcining, grind and mix, under air atmosphere, calcine, calcining temperature is 400～900 ℃, and calcination time is 1～10 hour;
4, by the mixture naturally cooling after calcining, grind and mix, sintering in reducing atmosphere, calcining temperature is 700～1100 ℃, calcination time is 3～12 hours, obtains a kind of aluminium borate base blue colour fluorescent powder.
When the present invention adopts high temperature solid-state method, the calcining temperature described in step 2 is 200～400 ℃, and calcination time is 3～10 hours; Calcining temperature described in step 3 is 600～800 ℃, and calcination time is 4～9 hours; Calcining temperature described in step 4 is 800～1000 ℃, and calcination time is 4～10 hours.
The aluminum ion Al that contains of the present invention
3+compound comprise a kind of in aluminum oxide, aluminium hydroxide; Contain boron ion B
3+compound comprise a kind of in boron trioxide, boric acid; Contain lanthanum ion La
3+compound comprise a kind of in lanthanum trioxide, lanthanum nitrate; The described cerium ion Ce that contains
4+compound be cerium oxide.Reducing atmosphere described in step 4 is active carbon granule reducing atmosphere.
The present invention be take the aluminium borate base blue colour fluorescent powder that UV-light prepared as excitaton source and can be coordinated appropriate redness, green emitting phosphor, applies and is packaged in outside InGaN diode, prepares white light LEDs illuminating device.
Compared with prior art, the advantage of technical solution of the present invention is:
1, the substrate material that the aluminium borate base fluorescent powder that prepared by the present invention provides, is easy to realize rare earth ion Ce
4+reduction, and trivalent rare earth ions can stablize and deposit in this matrix, sulfur-bearing not, environmental friendliness, has higher luminous efficiency.
2, fluorescent material provided by the invention, its excitation spectrum is wider, this fluorescent material excite scope in 250～350 nanometers, emission wavelength is between 350～500 nanometers, applicable ultraviolet LED excites, and can stick on and on ultraviolet leds chip, obtain efficient blue-light-emitting.
3, aluminium borate base blue colour fluorescent powder, preparation method thereof provided by the invention is simple, easy handling, and preparation process is not added solubility promoter, is easy to suitability for industrialized production.With the comparison of simple aluminates system fluorescent material, synthesis temperature low (800～1000 ℃), thereby obviously reduce energy consumption and product cost, material preparation for the requirement of equipment well below similar fluorescent material.
4, synthesis material wide material sources used in the present invention, reactive behavior is high, and application prospect is extensive.Product easily collecting, discharges without waste water and gas simultaneously, and environmental friendliness is especially applicable to serialization and produces.
Accompanying drawing explanation
Fig. 1 is the X-ray powder diffraction collection of illustrative plates of the material sample prepared by the embodiment of the present invention 1 technical scheme;
Fig. 2 is the material sample prepared by the embodiment of the present invention 1 technical scheme luminescent spectrum figure under the ultraviolet excitation of 310 nanometers;
Fig. 3 is the exciting light spectrogram of the ultraviolet region that obtains under the light detection of 380 nanometers of the material sample prepared by the embodiment of the present invention 1 technical scheme.
Embodiment
Below in conjunction with drawings and Examples, technical solution of the present invention is further described.
Embodiment 1:
Preparation La
0.995ce
0.005al
2b
3o
9
According to chemical formula La
0.995ce
0.005al
2b
3o
9in the stoichiometric ratio of each element take respectively aluminium oxide Al
2o
3: 1.020 grams, boric acid H
3bO
3: 1.855 grams, lanthanum trioxide La
2o
3: 1.621 grams, cerium oxide CeO
2: 0.009 gram, after grinding in agate mortar and mixing, select air atmosphere to calcine for the first time, temperature is 200 ℃, calcination time 10 hours, is then cooled to room temperature, takes out sample; By the raw material of calcining for the first time, fully mixed grinding is even again, sintering again under air atmosphere, and 800 ℃ of temperature, calcination time 4 hours, is then chilled to room temperature, takes out sample; After finally it fully being ground again, be placed on reducing atmosphere sintering (being embedded in activated carbon powder) in retort furnace, calcining temperature is 1000 ℃, and calcination time is 4 hours, obtains powder shaped aluminium borate base blue colour fluorescent powder.
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 technical scheme, and XRD test result shows, prepared material is aluminium borate LaAl
2b
3o
9monophase materials.
Referring to accompanying drawing 2, it is 0.5% concentration C e
3+ion doping La
3+la prepared by position
0.995ce
0.005al
2b
3o
9in fluorescent material, with UV-light 310 nanometers, excite the luminescent spectrum obtaining, emission wavelength is between 300～500 nanometers, the main center emission wavelength of this material is about the blue-light-emitting wave band of 450 nanometers, by CIE, calculate simultaneously, the coordinate of learning it is x=0.152, y=0.071, also just in time drops on blue region, is applicable to the white light LEDs that UV-light is excitation light source.
Referring to accompanying drawing 3, what from material sample monitoring utilizing emitted light 380 nanometers to preparing by the technology of the present invention, obtain can find out the exciting light spectrogram of ultraviolet region, excitation area is handed over wide, the blue-light-emitting of this material excite source mainly between 250～350 nanometers, can mate well ultraviolet LED chip.
Embodiment 2:
Preparation La
0.99ce
0.01al
2b
3o
9
According to chemical formula La
0.99ce
0.01al
2b
3o
9in the stoichiometric ratio of each element take respectively aluminium hydroxide Al (OH)
3: 1.560 grams, boric acid H
3bO
3: 1.855 grams, lanthanum nitrate La (NO
3)
3: 3.217 grams, cerium oxide CeO
2: 0.018 gram, after grinding in agate mortar and mixing, select air atmosphere to calcine for the first time, temperature is 400 ℃, calcination time 3 hours, is then cooled to room temperature, takes out sample; By the raw material of calcining for the first time, fully mixed grinding is even again, sintering again under air atmosphere, and 600 ℃ of temperature, calcination time 9 hours, is then chilled to room temperature, takes out sample; After finally it fully being ground again, be placed on reducing atmosphere sintering (being embedded in activated carbon powder) in retort furnace, calcining temperature is 800 ℃, and calcination time is 10 hours, obtains powder shaped aluminium borate base blue colour fluorescent powder.Its main structure properties, excitation spectrum, luminescent spectrum are similar to embodiment 1.
Embodiment 3:
Preparation La
0.97ce
0.03al
2b
3o
9
According to chemical formula La
0.97ce
0.03al
2b
3o
9in the stoichiometric ratio of each element take respectively aluminium oxide Al
2o
3: 1.020 grams, boron oxide B
2o
3: 1.045 grams, lanthanum trioxide La
2o
3: 1.581 grams, cerium oxide CeO
2: 0.052 gram, after grinding in agate mortar and mixing, select air atmosphere to calcine for the first time, temperature is 300 ℃, calcination time 7 hours, is then cooled to room temperature, takes out sample; By the raw material of calcining for the first time, fully mixed grinding is even again, sintering again under air atmosphere, and 700 ℃ of temperature, calcination time 8 hours, is then chilled to room temperature, takes out sample; After finally it fully being ground again, be placed on reducing atmosphere sintering (being embedded in activated carbon powder) in retort furnace, calcining temperature is 900 ℃, and calcination time is 8 hours, obtains powder shaped aluminium borate base blue colour fluorescent powder.Its main structure properties, excitation spectrum, luminescent spectrum are similar to embodiment 1.
Embodiment 4:
Preparation La
0.95ce
0.05al
2b
3o
9
According to chemical formula La
0.95ce
0.05al
2b
3o
9in the stoichiometric ratio of each element take respectively aluminium hydroxide Al (OH)
3: 1.560 grams, boron oxide B
2o
3: 1.045 grams, lanthanum nitrate La (NO
3)
3: 3.087 grams, cerium oxide CeO
2: 0.087 gram, after grinding in agate mortar and mixing, select air atmosphere to calcine for the first time, temperature is 350 ℃, calcination time 8 hours, is then cooled to room temperature, takes out sample; By the raw material of calcining for the first time, fully mixed grinding is even again, sintering again under air atmosphere, and 750 ℃ of temperature, calcination time 9 hours, is then chilled to room temperature, takes out sample; After finally it fully being ground again, be placed on reducing atmosphere sintering (being embedded in activated carbon powder) in retort furnace, calcining temperature is 850 ℃, and calcination time is 10 hours, obtains powder shaped aluminium borate base blue colour fluorescent powder.Its main structure properties, excitation spectrum, luminescent spectrum are similar to embodiment 1.
Claims (10)
1. an aluminium borate base blue colour fluorescent powder, is characterized in that: its chemical formula is La
1-x ce
x al
2b
3o
9, in formula, x is the molar percentage coefficient of La position Ce doping, 0.005≤x≤0.05; Described fluorescent material is under the ultraviolet excitation of 250～350 nanometers at wavelength, and emission wavelength is the blue light between 350～500 nanometers.
2. a preparation method for aluminium borate base blue colour fluorescent powder as claimed in claim 1, is characterized in that adopting high temperature solid-state method, comprises the following steps:
(1) to contain aluminum ion Al
3+compound, contain boron ion B
3+compound, contain lanthanum ion La
3+compound, contain cerium ion Ce
4+compound be raw material, by molecular formula La
1-x ce
x al
2b
3o
9the stoichiometric ratio of middle corresponding element takes each raw material, and in formula, x represents the molar percentage coefficient of La position Ce doping, 0.005≤x≤0.05; The raw material taking is ground respectively, and remix is even, obtains mixture;
(2) mixture is calcined under air atmosphere, calcining temperature is 100～500 ℃, and calcination time is 1～12 hour;
(3) by the mixture naturally cooling after calcining, grind and mix, under air atmosphere, calcine, calcining temperature is 400～900 ℃, and calcination time is 1～10 hour;
(4) by the mixture naturally cooling after calcining, grind and mix, sintering in reducing atmosphere, calcining temperature is 700～1100 ℃, calcination time is 3～12 hours, obtains a kind of aluminium borate base blue colour fluorescent powder.
3. the preparation method of a kind of aluminium borate base blue colour fluorescent powder according to claim 2, is characterized in that: the described aluminum ion Al that contains
3+compound comprise a kind of in aluminum oxide, aluminium hydroxide.
4. the preparation method of a kind of aluminium borate base blue colour fluorescent powder according to claim 2, is characterized in that: the described boron ion B that contains
3+compound comprise a kind of in boron oxide, boric acid.
5. the preparation method of a kind of aluminium borate base blue colour fluorescent powder according to claim 2, is characterized in that: the described lanthanum ion La that contains
3+compound comprise a kind of in lanthanum trioxide, lanthanum nitrate.
6. the preparation method of a kind of aluminium borate base blue colour fluorescent powder according to claim 2, is characterized in that: the described cerium ion Ce that contains
4+compound be cerium oxide.
7. the preparation method of a kind of aluminium borate base blue colour fluorescent powder according to claim 2, is characterized in that: the described calcining temperature of step (2) is 200～400 ℃, and calcination time is 3～10 hours; The described calcining temperature of step (3) is 600～800 ℃, and calcination time is 4～9 hours; The described calcining temperature of step (4) is 800～1000 ℃, and calcination time is 4～10 hours.
8. the preparation method of a kind of aluminium borate base blue colour fluorescent powder according to claim 2, is characterized in that: the described reducing atmosphere of step (4) is active carbon granule reducing atmosphere.
9. an application for aluminium borate base blue colour fluorescent powder as claimed in claim 1, is characterized in that: for the preparation of take the colourity of illumination, display device and photoluminescence that UV-light is excitaton source, regulate.
10. an application for aluminium borate base blue colour fluorescent powder as claimed in claim 1, is characterized in that: described fluorescent material is coordinated to appropriate redness, green emitting phosphor, apply and be packaged in outside InGaN diode, prepare white light LEDs illuminating device.
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| CN107446573A (en) * | 2017-08-18 | 2017-12-08 | 苏州轻光材料科技有限公司 | A kind of UV excited white lights LED fluorescent material and preparation method thereof |
| CN108822836B (en) * | 2018-06-08 | 2019-07-09 | 南通纺织丝绸产业技术研究院 | A kind of phosphor powder activated by Eu2+ and Eu3+ europium ions, preparation method and application |
| CN111996002B (en) * | 2020-09-18 | 2023-05-05 | 中国科学院长春应用化学研究所 | A single-matrix white light phosphor, its preparation method and application |
| CN116875303B (en) * | 2023-06-02 | 2024-11-22 | 常熟理工学院 | Aluminate-based red luminescent material and preparation method and application thereof |
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Non-Patent Citations (2)
| Title |
|---|
| GIANCARLO DELLA VENTURA et al..Peprossiite-(Ce), a new mineral from Campagnano (Italy): the first anhydrous rare-earth-element borate.《Eur. J. Mineral.》.1993,第5卷第53-58页. |
| Peprossiite-(Ce), a new mineral from Campagnano (Italy): the first anhydrous rare-earth-element borate;GIANCARLO DELLA VENTURA et al.;《Eur. J. Mineral.》;19931231;第5卷;第53-58页 * |
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