CN102424751A - Bismuth-layer-structured red light emitting phosphor, preparation method thereof, and application thereof - Google Patents

Bismuth-layer-structured red light emitting phosphor, preparation method thereof, and application thereof Download PDF

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CN102424751A
CN102424751A CN2011102953802A CN201110295380A CN102424751A CN 102424751 A CN102424751 A CN 102424751A CN 2011102953802 A CN2011102953802 A CN 2011102953802A CN 201110295380 A CN201110295380 A CN 201110295380A CN 102424751 A CN102424751 A CN 102424751A
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马谦
吕孟凯
杨萍
张爱玉
曹永强
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University of Jinan
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Abstract

The invention discloses a bismuth-layer-structured red light emitting phosphor with a chemical general formula of Bi3-3xNbTiO9:xEu<3+>, wherein x is no less than 0.001 and no larger than 0.15. The invention also discloses a preparation method of the phosphor, and an application of the phosphor. The technological process is safe, simple, and easy to control. No complicated equipment is required. The obtained red light emitting phosphor is advantaged in good chemical stability, no toxicity, and no radiation. Under excitation of AlGaN (350-360nm) and GaN (390-400nm) purple light LEDs, red light emission peaks with relatively high luminous intensity can be obtained. Therefore, the bismuth-layer-structured red light emitting phosphor can be used in fields of white light LED illumination and displaying.

Description

A kind of bismuth laminated red-light fluorescent powder
Technical field
The present invention relates to a kind of red-light fluorescent powder, be specifically related to a kind of red-light fluorescent powder with bismuth laminated (Aurivillius structure), belong to the luminescent material technical field.
Background technology
Since the sixties in last century, people have succeeded in developing Y 2O 3: Eu 3+And YVO 4: Eu 3+Red-light fluorescent powder and promote it in colour television set since; Rear-earth-doped red-light fluorescent powder has obtained fast development, is widely used in pl-, cathodoluminescence and X ray various colored show and lighting field such as cathode ray tube (CRT), FPD (FPD), plasma show in (PDP), field emission (FED) and the solid-state illumination (SSL) such as luminous.
Recently; The application of trichromatic rare-earth doping fluorescent material in CTV of new generation and the 4th generation lighting source white light LEDs shown its huge market prospect, and they have mainly utilized three kinds of primary colours fluorescent material of red, green, blue to issue out the principle of the three coloured light collocation of varying strength at outer field action.The three primary colors fluorescent powder that excites based on AlGaN (350～360 nm) and GaN (390～400 nm) purple LED is the focus of research at present.The fluorescent material of blue primary and green primary reaches requirement basically, but red-light fluorescent powder since drawbacks limit such as self brightness is not high, color developing difference the development of three primary colors fluorescent powder.
Therefore, exploring novel inorganic rare earth red emission fluorescent material is the important directions of current research, and selects suitable substrate material to be considered to the most effectively solution route.In addition; The preparation method of conventional fluorescent powder mainly is 1300 ℃ of the high temperature (> of oxide compound) solid reaction process; This method exists reaction process to be difficult to control; The products therefrom stoichiometric ratio is inaccurate, can't make active ions equally distributed shortcoming in matrix, thereby has reduced the luminous intensity and the uniformity of chromaticity of fluor.How to improve Preparation of Fluorescent Material technology and improve its luminescent properties, also become the difficult point of present stage research.
Summary of the invention
The present invention is directed to the problem that existing red-light fluorescent powder exists in preparation and practical application, a kind of red-light fluorescent powder based on bismuth laminated (Aurivillius structure) is provided, the fluorescent material chemicalstability of this structure is good, luminosity is high.
The present invention also provides the preparation method of this fluorescent material, process safety, simple, be easy to control.
The present invention also provides the application of this fluorescent material; Because its good performance; Particularly excite the following bigger red emission peak of luminous intensity that all can obtain, therefore can be applicable in white light LEDs s illumination and the demonstration field at AlGaN (350～360 nm) and GaN (390～400 nm) purple LED.
The present invention realizes through following measure:
A kind of bismuth laminated red-light fluorescent powder is characterized in that chemical general formula is: Bi 3-3xNbTiO 9: xEu 3+, 0.001≤x≤0.15.
Fluorescent material general formula of the present invention is Bi 3-3xNbTiO 9: xEu 3+, wherein Eu replaces part Bi, its structure and Bi 3NbTiO 9Structure is identical, is Aurivillius structure (bismuth laminated).Aurivillius structure involved in the present invention can be used [Bi usually 2O 2] [A N-1B nO 3n+1] or [Bi 2A N-1B nO 3n+3] expression, wherein the A position mainly is suitable for the bigger positively charged ion of dodecahedron coordinate by some and occupies (like A=K +, Na +, Ba 2+, Pb 2+, Sr 2+, Bi 3+, La 3+Deng); The B position is mainly occupied (like B=Ti by the transition metal ion that some is suitable for octahedral coordination 4+, Ta 5+, Nb 5+, V 5+, W 6+Deng); N is illustrated in two [Bi 2O 2] 2+BO between the layer 6The quantity of octahedral layer (n=1～5).Bi 3NbTiO 9Be typical A urivillius type compound, belong to rhombic system, spacer does A2 1 Am, lattice parameter is a=0.5440 nm, b=0.5394 nm, c=2.5099 nm, Z=4.Bi 3NbTiO 9By positively charged [Bi 2O 2] 2+Layer and electronegative perovskite-like [BiNbTiO 7] 2-The laminate structure that the mutual overlapping combination of layer forms, [BiNbTiO 7] 2-Layer is embedded in [Bi 2O 2] 2+The centre of layer.For BiNbTiO 7, Nb 5+(Ti 4+) be in the octahedra center of O, form O-Nb/Ti-O linear chain, Bi to be total to the continuous mode in angle 3+Occupy Nb (Ti) O 6The gap of octahedra network, [BiNbTiO 7] 2-Has the perovskite structure of being similar to.Aurivillius structure Bi 3NbTiO 9XRD diffraction peak position corresponding to the data of international crystal standard diffraction card (JCPDS No. 39-0233).Fig. 1 is that the present invention is at 15 minutes Bi of 550 ℃ of burnings 2.85NbTiO 9: 0.05Eu 3+Red-light fluorescent powder shows among the figure that in the XRD figure spectrum of 700 ℃ of thermal anneal process after 2 hours the diffraction peak of fluorescent material can be preferably corresponding to Bi 3NbTiO 9Standard diffraction card (JCPDS No. 39-0233) data, show that red-light fluorescent powder of the present invention has the Aurivillius structure.
The preparation method of bismuth laminated red-light fluorescent powder among the present invention is characterized in that may further comprise the steps:
(1) Niobium Pentxoxide is dissolved in the hydrofluoric acid under 80～90 ℃, adds ammoniacal liquor then and regulate pH to 8.5～9.5, form the niobium hydroxide deposition; Reaction solution room temperature ageing 10～16h refilters, washs, and obtains niobium hydroxide; Niobium hydroxide is dissolved in the aqueous citric acid solution, obtains Nb-C 6H 8O 7Solution;
(2) Nb in molar ratio 5+: Ti 4+: Bi 3+: Eu 3+: EDTA=1:1:3～3x:3x:3～4.5 and mol ratio an ammonium nitrate: the ratio of Hydrocerol A=3～6:1 joins the Nb-C that step (1) makes successively with tetrabutyl titanate, five nitric hydrate bismuths, europium nitrate, EDTA and an ammonium nitrate 6H 8O 7In the solution, 100 ℃ of following heated and stirred obtain aqueous precursor gel;
(3) with aqueous precursor gel burning 5～60min under 500～750 ℃, obtain Bi 3-3xNbTiO 9: xEu 3+Precursor powder;
(4) with Bi 3-3xNbTiO 9: xEu 3+Precursor powder promptly obtains Bi at 600～900 ℃ of following thermal anneal process 0.5～12h 3-3xNbTiO 9: xEu 3+Red-light fluorescent powder.
In the aforesaid method, in the step (1), the mol ratio of Hydrocerol A and Niobium Pentxoxide is 8～16: 1.
In the aforesaid method, the massfraction of hydrofluoric acid is 40%.
In the aforesaid method, in the step (1), the concentration of aqueous citric acid solution is 84.5g/L.
The present invention also provides the application of this fluorescent material, because this red-light fluorescent powder luminous intensity is big, therefore can be applicable in white light LEDs s illumination and the demonstration field.
The present invention at first utilizes the collosol and gel combustion method to prepare to form and reaches the mixed uniformly precursor powder of molecular level level, after handling through suitable thermal anneal process, obtains the Bi of Aurivillius structure 3-3xNbTiO 9: xEu 3+Red-light fluorescent powder.This technological process safety, simple, need not complex apparatus, be easy to control.
Not only chemicalstability is good, nontoxic, radiationless for novel red-light fluorescent powder of the present invention, narrow particle size distribution, active ions are evenly distributed in the matrix; And luminosity is high; Excite to descend all can obtain the bigger red emission peak of luminous intensity at AlGaN (350～360 nm) and GaN (390～400 nm) purple LED, can be applicable in white light LEDs s illumination and the demonstration field.
Description of drawings
Fig. 1 is embodiment 1 gained Bi 2.85NbTiO 9: 0.05Eu 3+The XRD figure spectrum of red-light fluorescent powder.
Fig. 2 is embodiment 1 gained Bi 2.85NbTiO 9: 0.05Eu 3+The ESEM of red-light fluorescent powder (SEM) photo.
Fig. 3 is embodiment 1 gained Bi 2.85NbTiO 9: 0.05Eu 3+The excitation spectrum of red-light fluorescent powder.
Fig. 4 is embodiment 1 gained Bi 2.85NbTiO 9: 0.05Eu 3+Emmission spectrum (the λ of red-light fluorescent powder Ex=355 nm).
Fig. 5 is embodiment 1 gained Bi 2.85NbTiO 9: 0.05Eu 3+Emmission spectrum (the λ of red-light fluorescent powder Ex=399 nm).
Embodiment
Through specific embodiment the present invention is further set forth below, should be understood that, following explanation only is in order to explain the present invention, its content not to be limited.Agents useful for same and reactant all can have been bought on market among the following embodiment, and used ammoniacal liquor is common commercially available ammoniacal liquor.
Embodiment 1
(1) with Nb 2O 5Under 80～90 ℃, be dissolved among 40% the HF, then to wherein splashing into NH 3H 2O solution to pH value is 8.5～9.5, forms white Nb (OH) 5Throw out, ageing is 12 hours under the room temperature, is dissolved in C after throw out is filtered, washs 6H 8O 7H 2In the O aqueous solution (84.5g/L), C 6H 8O 7H 2O and Nb 2O 5Mol ratio be 16: 1, form transparent Nb-C 6H 8O 7Solution;
(2) according to mol ratio Nb 5+: Ti 4+: Bi 3+: Eu 3+: EDTA=1: 1: 2.85: 0.15: 3.3 and NH 4NO 3: C 6H 8O 7H 2The ratio of O=4.5: 1 is with Ti (C 4H 9O) 4, Bi (NO 3) 35H 2O, Eu (NO 3) 3, EDTA and NH 4NO 3Join the Nb-C that step (1) is produced successively 6H 8O 7In the solution, form clear solution, 100 ℃ of following heated and stirred obtain lurid aqueous precursor gel;
(3) this aqueous precursor gel was burnt 15 minutes down at 550 ℃, obtain Bi 2.85NbTiO 9: 0.05Eu 3+Precursor powder;
(4) with the Bi that obtains 2.85NbTiO 9: 0.05Eu 3+Precursor powder promptly obtains Bi 700 ℃ of following anneal 2 hours 2.85NbTiO 9: 0.05Eu 3+Red-light fluorescent powder.
Fig. 1 is Bi 2.85NbTiO 9: 0.05Eu 3+The XRD figure spectrum of red-light fluorescent powder can find that the diffraction peak of fluorescent material can be preferably corresponding to Bi from figure 3NbTiO 9Standard diffraction card (JCPDS No. 39-0233) data, show that this red-light fluorescent powder has the Aurivillius structure.
Fig. 2 is Bi 2.85NbTiO 9: 0.05Eu 3+The SEM photo of red-light fluorescent powder shows that particle size distribution is narrower, mostly is between 80～120 nm.
Fig. 3 is Bi 2.85NbTiO 9: 0.05Eu 3+The excitation spectrum of red-light fluorescent powder, the stronger excitation peak of ultraviolet region lays respectively at 355 and 399 nm, with AlGaN and GaN purple LED coupling.
Fig. 4 is Bi 2.85NbTiO 9: 0.05Eu 3+Emmission spectrum (the λ of red-light fluorescent powder Ex=355 nm), show that emmission spectrum mainly is in the ruddiness zone, the highest peak value is positioned at 616 nm.
Fig. 5 is Bi 2.85NbTiO 9: 0.05Eu 3+Emmission spectrum (the λ of red-light fluorescent powder Ex=399 nm), show that emmission spectrum mainly is in the ruddiness zone, the highest peak value is positioned at 616 nm.
Embodiment 2
(1) with Nb 2O 5Under 80～90 ℃, be dissolved among 40% the HF, then to wherein splashing into NH 3H 2O solution to pH value is 8.5～9.5, forms white Nb (OH) 5Throw out, ageing is 14 hours under the room temperature, is dissolved in C after throw out is filtered, washs 6H 8O 7H 2In the O aqueous solution (84.5g/L), C 6H 8O 7H 2O and Nb 2O 5Mol ratio be 10: 1, form transparent Nb-C 6H 8O 7Solution;
(2) according to mol ratio Nb 5+: Ti 4+: Bi 3+: Eu 3+: EDTA=1: 1: 2.97: 0.03: 3.75 and NH 4NO 3: C 6H 8O 7H 2The ratio of O=4.25: 1 is with Ti (C 4H 9O) 4, Bi (NO 3) 35H 2O, Eu (NO 3) 3, EDTA and NH 4NO 3Join the Nb-C that step (1) is produced successively 6H 8O 7In the solution, form clear solution, 100 ℃ of following heated and stirred obtain lurid aqueous precursor gel;
(3) this aqueous precursor gel was burnt 35 minutes down at 575 ℃, obtain Bi 2.97NbTiO 9: 0.01Eu 3+Precursor powder;
(4) with the Bi that obtains 2.97NbTiO 9: 0.01Eu 3+Precursor powder promptly obtains Bi 675 ℃ of following anneal 7 hours 2.97NbTiO 9: 0.01Eu 3+Red-light fluorescent powder.
Embodiment 3
(1) with Nb 2O 5Under 80～90 ℃, be dissolved among 40% the HF, then to wherein splashing into NH 3H 2O solution to pH value is 8.5～9.5, forms white Nb (OH) 5Throw out, ageing is 10 hours under the room temperature, is dissolved in C after throw out is filtered, washs 6H 8O 7H 2In O (Hydrocerol A) aqueous solution (84.5g/L), C 6H 8O 7H 2O and Nb 2O 5Mol ratio be 8: 1, form transparent Nb-C 6H 8O 7Solution;
(2) according to mol ratio: Nb 5+: Ti 4+: Bi 3+: Eu 3+: EDTA=1: 1: 2.991: 0.009: 3.5 and NH 4NO 3: C 6H 8O 7H 2The ratio of O=4: 1 is with Ti (C 4H 9O) 4, Bi (NO 3) 35H 2O, Eu (NO 3) 3, EDTA and NH 4NO 3Join the Nb-C that step (1) is produced successively 6H 8O 7In the solution, form clear solution, 100 ℃ of following heated and stirred obtain lurid aqueous precursor gel;
(3) this aqueous precursor gel was burnt 55 minutes down at 525 ℃, obtain Bi 2.991NbTiO 9: 0.003Eu 3+Precursor powder;
(4) with the Bi that obtains 2.991NbTiO 9: 0.003Eu 3+Precursor powder promptly obtains Bi 650 ℃ of following anneal 10 hours 2.991NbTiO 9: 0.003Eu 3+Red-light fluorescent powder.
Embodiment 4
(1) with Nb 2O 5Under 80～90 ℃, be dissolved among 40% the HF, then to wherein splashing into NH 3H 2O solution to pH value is 8.5～9.5, forms white Nb (OH) 5Throw out, ageing is 15 hours under the room temperature, is dissolved in C after throw out is filtered, washs 6H 8O 7H 2The O aqueous solution (among the 84.5g/L 0, C 6H 8O 7H 2O and Nb 2O 5Mol ratio be 14: 1, form transparent Nb-C 6H 8O 7Solution;
(2) according to mol ratio Nb 5+: Ti 4+: Bi 3+: Eu 3+: EDTA=1: 1: 2.76: 0.24: 4 and NH 4NO 3: C 6H 8O 7H 2The ratio of O=5: 1 is with Ti (C 4H 9O) 4, Bi (NO 3) 35H 2O, Eu (NO 3) 3, EDTA and NH 4NO 3Join the Nb-C that step (1) is produced successively 6H 8O 7In the solution, form clear solution, 100 ℃ of following heated and stirred obtain lurid aqueous precursor gel;
(3) this aqueous precursor gel was burnt 30 minutes down at 625 ℃, obtain Bi 2.76NbTiO 9: 0.08Eu 3+Precursor powder;
(4) with the Bi that obtains 2.76NbTiO 9: 0.08Eu 3+Precursor powder promptly obtains Bi 800 ℃ of following anneal 5 hours 2. 76NbTiO 9: 0.08Eu 3+Red-light fluorescent powder.
Embodiment 5
(1) with Nb 2O 5Under 80～90 ℃, be dissolved among 40% the HF, then to wherein splashing into NH 3H 2O solution to pH value is 8.5～9.5, forms white Nb (OH) 5Throw out, ageing is 13 hours under the room temperature, is dissolved in C after throw out is filtered, washs 6H 8O 7H 2In the O aqueous solution (84.5g/L), C 6H 8O 7H 2O and Nb 2O 5Mol ratio be 9: 1, form transparent Nb-C 6H 8O 7Solution;
(2) according to mol ratio Nb 5+: Ti 4+: Bi 3+: Eu 3+: EDTA=1: 1: 2.64: 0.36: 4.5 and NH 4NO 3: C 6H 8O 7H 2The ratio of O=5.5: 1 is with Ti (C 4H 9O) 4, Bi (NO 3) 35H 2O, Eu (NO 3) 3, EDTA and NH 4NO 3Join the Nb-C that step (1) is produced successively 6H 8O 7In the solution, form clear solution, 100 ℃ of following heated and stirred obtain lurid aqueous precursor gel;
(3) this aqueous precursor gel was burnt 20 minutes down at 700 ℃, obtain Bi 2.64NbTiO 9: 0.12Eu 3+Precursor powder;
(4) with the Bi that obtains 2.64NbTiO 9: 0.12Eu 3+Precursor powder promptly obtains Bi 875 ℃ of following anneal 3 hours 2.64NbTiO 9: 0.12Eu 3+Red-light fluorescent powder.
Embodiment 6
(1) with Nb 2O 5Under 80～90 ℃, be dissolved among 40% the HF, then to wherein splashing into NH 3H 2O solution to pH value is 8.5～9.5, forms white Nb (OH) 5Throw out, ageing is 16 hours under the room temperature, is dissolved in C after throw out is filtered, washs 6H 8O 7H 2In the O aqueous solution (84.5g/L), C 6H 8O 7H 2O and Nb 2O 5Mol ratio be 14: 1, form transparent Nb-C 6H 8O 7Solution;
(2) according to mol ratio Nb 5+: Ti 4+: Bi 3+: Eu 3+: EDTA=1: 1: 2.55: 0.45: 4 and NH 4NO 3: C 6H 8O 7H 2The ratio of O=6: 1 is with Ti (C 4H 9O) 4, Bi (NO 3) 35H 2O, Eu (NO 3) 3, EDTA and NH 4NO 3Join the Nb-C that step (1) is produced successively 6H 8O 7In the solution, form clear solution, 100 ℃ of following heated and stirred obtain lurid aqueous precursor gel;
(3) this aqueous precursor gel was burnt 10 minutes down at 725 ℃, obtain Bi 2.55NbTiO 9: 0.15Eu 3+Precursor powder;
(4) with the Bi that obtains 2.55NbTiO 9: 0.15Eu 3+Precursor powder promptly obtains Bi 825 ℃ of following anneal 4 hours 2.55NbTiO 9: 0.15Eu 3+Red-light fluorescent powder.

Claims (6)

1. a bismuth laminated red-light fluorescent powder is characterized in that, chemical general formula is: Bi 3-3xNbTiO 9: xEu 3+, 0.001≤x≤0.15.
2. the preparation method of the described bismuth laminated red-light fluorescent powder of claim 1 is characterized in that may further comprise the steps:
(1) Niobium Pentxoxide is dissolved in the hydrofluoric acid under 80～90 ℃, adds ammoniacal liquor then and regulate pH to 8.5～9.5, form the niobium hydroxide deposition; Reaction solution room temperature ageing 10～16h refilters, washs, and obtains niobium hydroxide; Niobium hydroxide is dissolved in the aqueous citric acid solution, obtains Nb-C 6H 8O 7Solution;
(2) Nb in molar ratio 5+: Ti 4+: Bi 3+: Eu 3+: EDTA=1:1:3～3x:3x:3～4.5 and mol ratio an ammonium nitrate: the ratio of Hydrocerol A=3～6:1 joins the Nb-C that step (1) makes successively with tetrabutyl titanate, five nitric hydrate bismuths, europium nitrate, EDTA and an ammonium nitrate 6H 8O 7In the solution, 100 ℃ of following heated and stirred obtain aqueous precursor gel;
(3) with aqueous precursor gel burning 5～60min under 500～750 ℃, obtain Bi 3-3xNbTiO 9: xEu 3+Precursor powder;
(4) with Bi 3-3xNbTiO 9: xEu 3+Precursor powder promptly obtains Bi at 600～900 ℃ of following thermal anneal process 0.5～12h 3-3xNbTiO 9: xEu 3+Red-light fluorescent powder.
3. preparation method according to claim 2 is characterized in that: in the step (1), the mol ratio of Hydrocerol A and Niobium Pentxoxide is 8～16: 1.
4. preparation method according to claim 2 is characterized in that: in the step (1), the massfraction of hydrofluoric acid is 40%.
5. preparation method according to claim 2 is characterized in that: in the step (1), the concentration of aqueous citric acid solution is 84.5g/L.
6. the application of the described bismuth laminated red-light fluorescent powder of claim 1.
CN201110295380.2A 2011-09-28 2011-09-28 Bismuth-layer-structured red light emitting phosphor, preparation method thereof, and application thereof Expired - Fee Related CN102424751B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106905969A (en) * 2017-03-29 2017-06-30 江苏师范大学 In fluorescent material, the preparation method and application of near ultraviolet excitated lower transmitting gold-tinted
CN109772294A (en) * 2019-03-18 2019-05-21 济南大学 The preparation method and products obtained therefrom of a kind of tetragonal phase BiVO4 film with p-type conductivity and application

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
QIAN MA ET AL.: "Synthesis and luminescence of pure and Eu3+-activated Aurivillius-type Bi3TiNbO9 nanophosphors", 《MATERIALS CHEMISTRY AND PHYSICS》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106905969A (en) * 2017-03-29 2017-06-30 江苏师范大学 In fluorescent material, the preparation method and application of near ultraviolet excitated lower transmitting gold-tinted
CN106905969B (en) * 2017-03-29 2019-04-16 江苏师范大学 Fluorescent material, preparation method and application near ultraviolet excitated lower transmitting yellow light
CN109772294A (en) * 2019-03-18 2019-05-21 济南大学 The preparation method and products obtained therefrom of a kind of tetragonal phase BiVO4 film with p-type conductivity and application
CN109772294B (en) * 2019-03-18 2021-12-07 济南大学 Preparation method of tetragonal phase BiVO4 film with p-type conductivity, obtained product and application

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