CN104861969A - Aluminum calcium titanate solid-solution type red phosphor and preparation method thereof - Google Patents

Aluminum calcium titanate solid-solution type red phosphor and preparation method thereof Download PDF

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Publication number
CN104861969A
CN104861969A CN201510258153.0A CN201510258153A CN104861969A CN 104861969 A CN104861969 A CN 104861969A CN 201510258153 A CN201510258153 A CN 201510258153A CN 104861969 A CN104861969 A CN 104861969A
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red fluorescence
fluorescence powder
light
calcium titanate
solution type
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范艳伟
陈朝阳
张杰强
王军华
闫世友
谢永新
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
    • Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps

Abstract

The invention discloses an aluminum calcium titanate solid-solution type red phosphor which can be effectively excited by ultraviolet light and blue light simultaneously. The general chemical formula of the phosphor is Ca(1-x)(TiO3)(1-Y)/2(AlO2)y: xEu. According to the method, larger lattice distortion of a matrix of the phosphor is realized through introduction of aluminum ions, the symmetry degree of matrix lattice of the phosphor is reduced, and transition, from <5>D0 to <7>F2, of a trivalence europium ion electric dipole sensitive to the outside environment is greatly enhanced. The aluminum calcium titanate solid-solution type red phosphor can be effectively excited by 398 nm ultraviolet light and 467 nm blue light simultaneously, can be well matched with a near ultraviolet GaN LED with wavelength being 395-400 nm and a blue light GaN LED with wavelength being 465-480 nm, the fluorescence-emission peaks are located in the positions of 617 nm and 594 nm, and the emitting strength of red light in the position of 617 nm is remarkably higher than that of orange light in the position of 594 nm. According to the method, the preparation technology is simple, atmosphere protection is not required, the operation is easy, the production cost is lower, the chemical stability of a product is good, and the red phosphor is ideal and used for a white light LED.

Description

A kind of aluminium calcium titanate solid-solution type red fluorescence powder and preparation method thereof
Technical field
The present invention relates to a kind of aluminium calcium titanate solid-solution type red fluorescence powder that effectively can be excited by near ultraviolet or blue light, belong to field of optical functional material.
Background technology
In recent years, along with the decline gradually of raising and the cost gradually of photodiode (LED) luminous efficiency, semiconductor lighting becomes the development trend of modern illumination gradually.White light LEDs has the features such as current consumption is little, life-span length, environmental protection and is claimed to be the forth generation lighting source after incandescent light, luminescent lamp and high pressure gas discharge lamp, and being described as is " 21 century green light source ".
Commercial three primary colors fluorescent powder at present based near ultraviolet (NUV395-400 nanometer) GaN-LEDs is Y 2o 2s:Eu 3+(rouge and powder), BaMgAl 10o 17: Eu 2+(blue powder) and ZnS:Cu +, Al 3+(green powder) (Sun W T, Gu Y X, Zhang Q H etal.J.Alloy.Compd., 2010,493:561-564), and the luminous efficiency of red fluorescence powder is wherein far below blue and green emitting phosphor.The luminous efficiency of the red fluorescence material of traditional sulfide base is high but unstable, easily decomposes and releases harmful H 2s gas; Nitride red fluorescent material is as Sr 2si 5n 8: Eu 2+have the excellent characteristics of luminescence Deng (US Patent No. 6649946), but synthesis condition is harsh, cost is high.Therefore, develop a kind of environmental friendliness, the red fluorescence powder simultaneously possessing higher photoluminescence efficiency has been the active demand of industrial community.
Summary of the invention
The present invention seeks to wait deficiency for existing red light emitting phosphor efficiency is low, provide a kind of aluminium calcium titanate solid-solution type red fluorescence powder and preparation method thereof, the method develops the red fluorescence powder with higher photoluminescence efficiency by aluminum ions introducing.Aluminum ions introducing makes the matrix of this fluorescent material produce larger lattice distortion, reduces the symmetry of its matrix lattice, greatly strengthen the europium ion electric dipole to outside environment sensitive transition ( 5d 0→ 7f 2), this transition corresponds to the red emission of 617 nanometers.The aluminium calcium titanate solid-solution type red fluorescence powder of gained of the present invention can effectively be excited by the blue light of the near-ultraviolet light of 398 nanometers and 467 nanometers simultaneously; Matched well can be carried out with near ultraviolet GaN-LED (395-400 nanometer) and blue light GaN-LED (465-480 nanometer), fluorescence emission peak lays respectively at 617 nanometers and 594 nanometers, and the red light-emitting intensity being positioned at 617 nanometers obviously will be better than the luminous intensity of the orange-colored light of 594 nanometers.With the Y of commercialization 2o 3: Eu series red fluorescence powder is compared, emission peak red shift, is conducive to the colour rendering index and the reduction colour temperature that improve white light LEDs; Product preparation process is simple and without the need to atmosphere protection, easy handling, and the lower and product chemistry good stability of production cost is a kind of desirable red fluorescent powder for white radiation LED.
A kind of aluminium calcium titanate solid-solution type red fluorescence powder of the present invention, the chemical constitution general formula of this red fluorescence powder is: Ca 1-x(TiO 3) 1-y/2(AlO 2) y: xEu; Wherein, 0.01≤x≤0.20,0.05≤y≤0.35.
The preparation method of described aluminium calcium titanate solid-solution type red fluorescence powder, follows these steps to carry out:
A, according to chemical general formula Ca 1-x(TiO 3) 1-y/2(AlO 2) y: the mol ratio of xEu takes Eu 2o 3, wherein, 0.01≤x≤0.20,0.05≤y≤0.35, joins in dehydrated alcohol, and dropwise drips concentrated nitric acid until Eu 2o 3dissolve completely, then under the condition stirred, add butyl (tetra) titanate, Ca (NO 3) 24H 2o and Al (NO 3) 39H 2o, obtains mixed solution;
Ammoniacal liquor or bicarbonate of ammonia is dropwise dripped until obtain glue flocks in b, the mixed solution that obtained by step a, drying obtains solid mixture, and wherein drying is stage drying, first at 80 DEG C dry 12 hours, be warming up to 120 DEG C of dryings 12 hours again, the solid mixture obtained;
C, the solid mixture obtained by step b grind, time 0.5-1 hour, then load crucible and carry out baking inphases, first be warming up to 500 DEG C with the temperature rise rate of temperature 4 DEG C/min, and be incubated 2-4 hour, then be warming up to 1200 DEG C, insulation 3-6 hour, is then down to room temperature naturally;
D, the product obtained by step c are pulverized, grinding, obtain Ca 1-x(TiO 3) 1-y/2(AlO 2) y: xEu red fluorescence powder.
This aluminium calcium titanate solid-solution type red fluorescence powder can effectively be excited by near-ultraviolet light and blue light and send red light simultaneously, near-ultraviolet light effectively excites wave band to be 390-410 nanometer, blue light effectively excites wave band to be 455-475 nanometer, the strongest excitation peak lays respectively at 398 nanometers and 467 nanometers, the strongest emission peak is positioned at 617 nanometers, can be used for preparing white light LEDs.
A kind of aluminium calcium titanate solid-solution type red fluorescence powder of the present invention is compared with existing red fluorescence powder, and tool has the following advantages:
(1) fluorescent material substrate mixture is prepared by solution method, and its matrix is more even, and the consistence of product is better;
(2) what baking inphases made various raw material mix is more even, facilitates fully carrying out of reaction through high-temperature roasting, is easy to form pure single-phase;
(3) chemically stable is good, and the preparation process of fluorescent material of the present invention completes in open environment, without the need to atmosphere protection in calcination process, even if therefore this product in hot environment also can not oxidized or decompose;
(4) raw materials used cheap and easy to get, be conducive to reducing production cost;
(5) equipment used is simple, easy handling.
Accompanying drawing explanation
Fig. 1 is Ca of the present invention 1-x(TiO 3) 1-y/2(AlO 2) y: the XRD figure spectrum of xEu material;
Fig. 2 is Ca of the present invention 1-x(TiO 3) 1-y/2(AlO 2) y: the exciting light spectrogram of xEu material under 617 nanometer light detections;
Fig. 3 is Ca of the present invention 1-x(TiO 3) 1-y/2(AlO 2) y: the utilizing emitted light spectrogram of xEu material under 398 nanometer optical excitation;
Fig. 4 is Ca of the present invention 1-x(TiO 3) 1-y/2(AlO 2) y: the utilizing emitted light spectrogram of xEu material under 467 nanometer optical excitation.
Embodiment
Embodiment 1
A, take 0.035 gram of Eu 2o 3join in dehydrated alcohol, and dropwise drip concentrated nitric acid until Eu 2o 3dissolving completely, when stirring, adding 6.058 grams of butyl (tetra) titanates respectively, 4.676 grams of Ca (NO 3) 24H 2o and 1.651 gram of Al (NO 3) 39H 2o, continues stirring 1 hour, obtains mixing solutions;
Dropwise drip ammoniacal liquor until solution becomes glue flocks in b, the mixing solutions that obtained by step a, then carry out stage drying, first dry 12 hours at temperature 80 DEG C, then be warming up to 120 DEG C of dryings 12 hours, obtain solid mixture;
C, the solid mixture obtained by step b grind, and 0.5 hour time, then pour in crucible, put into clock hood type furnace, carry out baking inphases, be first warming up to 500 DEG C with the temperature rise rate of temperature 4 DEG C/min and be incubated 2 hours, be warming up to 1200 DEG C again and be incubated 4 hours, being then naturally down to room temperature;
D, by step c product of roasting through pulverize, grinding, obtain Ca 0.99(TiO 3) 0.89(AlO 2) 0.22: the red fluorescence powder of 0.01Eu.
Embodiment 2
A, take 0.211 gram of Eu 2o 3join in dehydrated alcohol, and dropwise drip concentrated nitric acid until Eu 2o 3dissolving completely, when stirring, adding 6.399 grams of butyl (tetra) titanates respectively, 4.440 grams of Ca (NO 3) 24H 2o and 0.825 gram of Al (NO 3) 39H 2o, continues stirring 1 hour, obtains mixing solutions;
B, the mixing solutions obtained by step a dropwise drips bicarbonate of ammonia until solution becomes glue flocks, then carries out stage drying, first dries 12 hours at temperature 80 DEG C, then is warming up to 120 DEG C of dryings 12 hours, obtain solid mixture;
C, the solid mixture obtained by step b grind, and 1 hour time, then pour in crucible, put into clock hood type furnace, carry out baking inphases, be first warming up to 500 DEG C with the temperature rise rate of temperature 4 DEG C/min and be incubated 3 hours, be warming up to 1200 DEG C again and be incubated 5 hours, being then naturally down to room temperature;
D, by step c product of roasting through pulverize, grinding, obtain Ca 0.94(TiO 3) 0.94(AlO 2) 0.11: the red fluorescence powder of 0.06Eu.
Embodiment 3
A, take 0.211 gram of Eu 2o 3join in dehydrated alcohol, and dropwise drip concentrated nitric acid until Eu 2o 3dissolving completely, when stirring, adding 6.058 grams of butyl (tetra) titanates respectively, 4.440 grams of Ca (NO 3) 24H 2o and 1.651 gram of Al (NO 3) 39H 2o, continues stirring 1 hour, obtains mixing solutions;
Dropwise drip ammoniacal liquor until solution becomes glue flocks in b, the mixing solutions that obtained by step a, then carry out stage drying, first dry 12 hours at temperature 80 DEG C, then be warming up to 120 DEG C of dryings 12 hours, obtain solid mixture;
C, the solid mixture obtained by step b grind, and 0.5 hour time, then pour in crucible, put into clock hood type furnace, carry out baking inphases, be first warming up to 500 DEG C with the temperature rise rate of temperature 4 DEG C/min and be incubated 4 hours, be warming up to 1200 DEG C again and be incubated 4 hours, being then naturally down to room temperature;
D, by step c product of roasting through pulverize, grinding, obtain Ca 0.94(TiO 3) 0.89(AlO 2) 0.22: the red fluorescence powder of 0.06Eu.
Embodiment 4
A, take 0.211 gram of Eu 2o 3join in dehydrated alcohol, and dropwise drip concentrated nitric acid until Eu 2o 3dissolving completely, when stirring, adding 5.582 grams of butyl (tetra) titanates respectively, 4.440 grams of Ca (NO 3) 24H 2o and 2.626 gram of Al (NO 3) 39H 2o, continues stirring 1 hour, obtains mixing solutions;
Dropwise drip bicarbonate of ammonia until solution becomes glue flocks in b, the mixing solutions that obtained by step a, then carry out stage drying, first dry 12 hours at temperature 80 DEG C, then be warming up to 120 DEG C of dryings 12 hours, obtain solid mixture;
C, the solid mixture obtained by step b grind, and 0.5 hour time, then pour in crucible, put into clock hood type furnace, carry out baking inphases, be first warming up to 500 DEG C with the temperature rise rate of temperature 4 DEG C/min and be incubated 3 hours, be warming up to 1200 DEG C again and be incubated 6 hours, being then naturally down to room temperature;
D, by step c product of roasting through pulverize, grinding, obtain Ca 0.94(TiO 3) 0.82(AlO 2) 0.35: the red fluorescence powder of 0.06Eu.
Embodiment 5
A, take 0.528 gram of Eu 2o 3join in dehydrated alcohol, and dropwise drip concentrated nitric acid until Eu 2o 3dissolving completely, when stirring, adding 6.058 grams of butyl (tetra) titanates respectively, 4.015 grams of Ca (NO 3) 24H 2o and 1.651 gram of Al (NO 3) 39H 2o, continues stirring 1 hour, obtains mixing solutions;
Dropwise drip ammoniacal liquor until solution becomes glue flocks in b, the mixing solutions that obtained by step a, then carry out stage drying, first dry 12 hours at temperature 80 DEG C, then be warming up to 120 DEG C of dryings 12 hours, the solid mixture obtained;
C, the solid mixture obtained by step b grind, and through grinding 0.5 hour, then pouring in crucible, putting into clock hood type furnace, carry out baking inphases, are first warming up to 500 DEG C with the temperature rise rate of temperature 4 DEG C/min and are incubated 2 hours; Be warming up to 1200 DEG C again and be incubated 4 hours, being then naturally down to room temperature;
D, by step c product of roasting through pulverize, grinding, obtain Ca 0.85(TiO 3) 0.89(AlO 2) 0.22: the red fluorescence powder of 0.15Eu.
Embodiment 6
Hitachi F-7000 type spectrophotofluorometer is used to carry out spectrum test to any one gained red fluorescence powder of embodiment 1-5, first its excitation spectrum is measured, monitoring wavelength is the utilizing emitted light of 617 nanometers, exciting light is scanned, sweep limit is 350-500 nanometer, obtain the excitation spectrum of material as accompanying drawing 2, its excitation peak lays respectively at 398 nanometers and 467 nanometers; Then its emmission spectrum is measured, the exciting light being 398 nanometers and 467 nanometers with wavelength respectively excites sample, its utilizing emitted light is scanned, sweep limit is 560-650 nanometer, obtain the emmission spectrum of material as accompanying drawing 3 and accompanying drawing 4, its emission peak lays respectively at 617 nanometers and 594 nanometers, and 617 nanometers are for launch envelope the most by force.

Claims (4)

1. an aluminium calcium titanate solid-solution type red fluorescence powder, is characterized in that the chemical constitution general formula of this red fluorescence powder is: Ca 1-x(TiO 3) 1-y/2(AlO 2) y: xEu; Wherein, 0.01≤x≤0.20,0.05≤y≤0.35.
2. the preparation method of aluminium calcium titanate solid-solution type red fluorescence powder according to claim 1, is characterized in that following these steps to carry out:
A, according to chemical general formula Ca 1-x(TiO 3) 1-y/2(AlO 2) y: the mol ratio of xEu takes Eu 2o 3, wherein, 0.01≤x≤0.20,0.05≤y≤0.35, joins in dehydrated alcohol, and dropwise drips concentrated nitric acid until Eu 2o 3dissolve completely, then under the condition stirred, add butyl (tetra) titanate, Ca (NO 3) 24H 2o and Al (NO 3) 39H 2o, obtains mixed solution;
Ammoniacal liquor or bicarbonate of ammonia is dropwise dripped until obtain glue flocks in b, the mixed solution that obtained by step a, drying obtains solid mixture, and wherein drying is stage drying, first at 80 DEG C dry 12 hours, be warming up to 120 DEG C of dryings 12 hours again, the solid mixture obtained;
C, the solid mixture obtained by step b grind, time 0.5-1 hour, then load crucible and carry out baking inphases, first be warming up to 500 DEG C with the temperature rise rate of temperature 4 DEG C/min, and be incubated 2-4 hour, then be warming up to 1200 DEG C, insulation 3-6 hour, is then down to room temperature naturally;
D, the product obtained by step c are pulverized, grinding, obtain Ca 1-x(TiO 3) 1-y/2(AlO 2) y: xEu red fluorescence powder.
3. an aluminium calcium titanate solid-solution type red fluorescence powder as claimed in claim 1 is preparing the purposes in white light LEDs.
4. aluminium calcium titanate solid-solution type red fluorescence powder purposes according to claim 3, it is characterized in that, described red fluorescence powder can effectively be excited by near-ultraviolet light and blue light and send red light simultaneously, near-ultraviolet light effectively excites wave band to be 390-410 nanometer, and blue light effectively excites wave band to be 455-475 nanometer; The strongest excitation peak lays respectively at 398 nanometers and 467 nanometers; The strongest emission peak is positioned at 617 nanometers.
CN201510258153.0A 2015-05-20 2015-05-20 Aluminum calcium titanate solid-solution type red phosphor and preparation method thereof Pending CN104861969A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106747414A (en) * 2016-12-15 2017-05-31 武汉科技大学 A kind of micropore titanium calcium aluminate raw material and preparation method thereof
CN108707456A (en) * 2018-05-20 2018-10-26 河南城建学院 A kind of preparation method of red light fluorescent powder

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JPH10298550A (en) * 1997-04-28 1998-11-10 Hitachi Maxell Ltd Infrared light-emitting fluorescent material
CN1912049A (en) * 2006-08-18 2007-02-14 浙江大学 High brilliancy environmental protection type alkaline earth ion solid solution titanate fluorescent powder and its preparation method
JP2009155376A (en) * 2007-12-25 2009-07-16 National Institute Of Advanced Industrial & Technology Oxide phosphor epitaxial thin film

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JPH10298550A (en) * 1997-04-28 1998-11-10 Hitachi Maxell Ltd Infrared light-emitting fluorescent material
CN1912049A (en) * 2006-08-18 2007-02-14 浙江大学 High brilliancy environmental protection type alkaline earth ion solid solution titanate fluorescent powder and its preparation method
JP2009155376A (en) * 2007-12-25 2009-07-16 National Institute Of Advanced Industrial & Technology Oxide phosphor epitaxial thin film

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YULONG WANG等: "Effect of replacement of Ca by Zn on the structure and optical property of CaTiO3:Eu3+ red phosphor prepared by sol-gel method", 《LUMINESCENCE》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106747414A (en) * 2016-12-15 2017-05-31 武汉科技大学 A kind of micropore titanium calcium aluminate raw material and preparation method thereof
CN106747414B (en) * 2016-12-15 2020-04-10 武汉科技大学 Microporous calcium titanium aluminate raw material and preparation method thereof
CN108707456A (en) * 2018-05-20 2018-10-26 河南城建学院 A kind of preparation method of red light fluorescent powder
CN108707456B (en) * 2018-05-20 2021-02-12 河南城建学院 Preparation method of red-light fluorescent powder

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