CN106433642A - Self-activated titanoniobate-based fluorescent powder and preparation method thereof - Google Patents

Self-activated titanoniobate-based fluorescent powder and preparation method thereof Download PDF

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CN106433642A
CN106433642A CN201610845827.1A CN201610845827A CN106433642A CN 106433642 A CN106433642 A CN 106433642A CN 201610845827 A CN201610845827 A CN 201610845827A CN 106433642 A CN106433642 A CN 106433642A
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fluorescent material
preparation
nbtio
gdnbtio
stage sintering
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司家勇
刘娜
宋思远
蔡格梅
钟利萍
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Central South University of Forestry and Technology
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Central South University of Forestry and Technology
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    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
    • C09K11/7767—Chalcogenides

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  • Inorganic Chemistry (AREA)
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  • Luminescent Compositions (AREA)

Abstract

The invention discloses a self-activated titanoniobate-based fluorescent material and a preparation method thereof. The series of fluorescent powder is prepared by the following steps: taking GdNbTiO6 as a matrix, doping rare earth ions Eu3<+> and Dy<3+>, thereby obtaining a red fluorescent material Gd<1-x>NbTiO6:xEu3<+> and yellow green fluorescent powder Gd<1-y>NbTiO6:yDy3<+>, wherein x is equal to 0.01-0.05, and y is equal to 0.01-0.05. The process flow disclosed by the invention is safe, simple and easy to control. The prepared fluorescent material has the advantages of high chemical stability, non-toxicity, zero radiation, high brightness, high color purity, high conversion efficiency and the like.

Description

A kind of self-activation niobate-titanate base fluorescent powder and preparation method thereof
Technical field
The present invention relates to rare earth luminescent material field, especially relate to can apply to a kind of red of three-color fluorescent lamp Or yellow green self-activating niobate-titanate base fluorescent material and preparation method thereof.
Background technology
Current commercial light source major part needs to make light conversion, the fluorescence prepared by rare-earth trichromatic fluorescent powder using fluorescent material Lamp is very energy-efficient new type light source, is the prior development direction of world's lighting source, is increased with 15% speed every year, Corresponding three primary colors fluorescent powder is in great demand, and is substantially at the state that supply falls short of demand.Because rare-earth trichromatic fluorescent lamp has Specular removal, low light attenuation, long-life feature, are therefore generally satisfactory under the overall situation vigorously advocating energy-saving and emission-reduction at present And fast-developing, the research and development of rare earth luminescent material and application will be one of focuses in international competition, explore new rare earth Luminescence system is also one of focus of current illumination field.
Fluorescence host material, as the bearer of the centre of luminescence, has large effect to the luminous of the centre of luminescence, for Specific activator ion, its absorption band not only relies on the energy level of itself, also puts to death in residing lattice environment.
In recent years, lot of domestic and international units is devoted to finding and is suitable to rear-earth-doped base Quality Research, to rare earth niobium titanium Hydrochlorate is that the exploration of the fluorescent material of substrate is also constantly being carried out, and is prepared for a series of rare earth niobate-titanates that can be used for different field Fluorescent material (LaNbTiO6:Eu3+、YNbTiO6:Eu3+/Dy3+), but contrast with business-like fluorescent material at present, this line fluorescent Also there is segmental defect in powder, such as luminous efficiency is not high, and light decay is big, and colourity is impure etc..In recent years, numerous studies personnel were right GdNbTiO6Microwave dielectric property carried out detailed probing into, and its optical property has no report always.In addition, prior art Personnel are additionally considered that Gd and La, Y are all rare earth element, have similar chemical property, there is also certain phase on luminescent properties Like property, and due to exciting the part electron-hole pair of formation may be by Gd3+Captured, excitation energy is in Gd3+Upper move Move, therefore, those skilled in the art will be considered that this kind of situation can be so that the luminous efficiency of fluorescent material reduces (can be found in document1K.Mori,M.Nakayama and H.Nishimura,Role of the core excitons formed by 4f-4f transitions of Gd3+on Ce3+scintillation in Gd2SiO5:Ce3+,Physical Review B,2003, 67.
Content of the invention
But in the discovery GdNbTiO that inventor is unexpected and pleasantly surprised under study for action6There is more excellent optical property；This is Inventor does not expect.Therefore, the present invention provides a kind of red or yellow green rare earth niobate-titanate fluorescent material, has Luminous efficiency is high, and light decay is little, the good optical property of the pure grade of colourity, and can be very good to meet the requirement of three primary colors fluorescent powder.
A kind of self-activation niobate-titanate base fluorescent powder of the present invention, is with GdNbTiO6For matrix, by mixing 0.01～ 0.05at.%Eu3+Enter Gd3+Position, obtaining chemical formula is Gd(1‐x)NbTiO6:xEu3+Single-phase red fluorescence powder；By mixing 0.01～0.05at.%Dy3+Enter GdNbTiO6Gd in matrix3+Position, obtains Gd(1‐y)NbTiO6:yDy3+Single-phase yellow green is glimmering Light powder.
Using the X-ray powder diffraction data of the host material of the present invention, carried out using Fullprof software Rietveld refine, shows described GdNbTiO6Matrix belongs to Pbcn (No.60) space group, and cell parameter isZ=4.
The preparation method of this niobate-titanate base fluorescent powder is：It is Gd according to chemical formula(1‐x)NbTiO6:xEu3+Or Gd(1‐y) NbTiO6:yDy3+Required nonstoichiometric molar ratio weighs Gd2O3、Nb2O5And TiO2, and Eu2O3Or Dy2O3, it is fully ground, Then carry out two-step sintering to obtain, first stage sintering temperature is 1000～1200 DEG C, is cooled to room temperature after sintering, grind, so Carry out second stage sintering under conditions of 1250～1350 DEG C of temperature afterwards, cooling, grind, obtain final product.
The heating rate of first stage sintering step is preferably 3～5 DEG C/min.
The heating rate of second stage sintering step is preferably 3～5 DEG C/min.
The temperature retention time of first stage sintering step is preferably 10～15 hours.
The temperature retention time of second stage sintering step is preferably 10～15 hours.
Preferred by above-mentioned condition, can obtain further performance more preferably luminous intensity height, warm tones, fast decay, Persistence is short, heat stability is good, be easy to preserve for a long time, the niobate-titanate base fluorescent powder of the present invention of applied range.
The present inventor passes through research and finds Gd(1‐x)NbTiO6:xEu3+Effective excitation wavelength of series phosphor powder be located at 200～ In the range of 320nm, show the feature of wide band absorption, can be used for red fluorescence powder.Gd(1‐y)NbTiO6:yDy3+Series phosphor powder Effective excitation wavelength be located at 200～320nm in the range of, show the feature of wide band absorption, for yellowish green fluorescent powder.
Beneficial effects of the present invention
Such as luminous efficiency existing for existing fluorescent RE powder for the present invention is not high, light decay is big, colourity is impure etc. Defect, successfully explores a kind of new rare earth niobium titanate compound as the redness of phosphor host and yellow-green fluorescence Powder；The fluorescent material that the present invention provides has in ultra-violet (UV) band Absorber Bandwidth (200 320nm wave-length coverage) it is seen that light area high transmission, Luminous intensity height, warm tones, the features such as persistence is short, heat stability is good, preparation technology is simpler.
The present invention is by adopting GdNbTiO6Grope for matrix and in substantial amounts of experiment, obtain passing through respectively singly mixing 0.01～ 0.05at.%Eu3+Or 0.01～0.05at.%Dy3+Enter Gd3+Position, and control reactions steps, each step by strict The combination of response parameter etc., with GdNbTiO6The position consistency of diffraction maximum, and do not have miscellaneous peak to occur, product is single-phase lighting by force Degree height, warm tones, persistence is short, heat stability is good, be easy to the rare earth niobate-titanate base Hydrargyri Oxydum Rubrum that preserves for a long time and yellowish green powder.
The rare earth niobate-titanate Hydrargyri Oxydum Rubrum excitation wavelength that the present invention prepares is located in the range of the 320nm of broadband 200, Peak value is reached, the strongest launch wavelength is located at 614nm, meets the condition of electricity-saving lamp red fluorescence powder well at 273nm；Right Such fluorescent material carries out attenuation curve test and finds its fluorescence lifetime in 0.056ms.The yellowish green powder of rare earth niobate-titanate excites Wavelength is located in the range of 200 320nm, reaches peak value at 273nm, and the strongest launch wavelength is located at 577nm, to such fluorescent material Carrying out attenuation curve test finds its fluorescence lifetime in 0.045ms.The fluorescent material of the present invention is not only suitable for for three primary colours In fluorescent lamp, and can be good at meeting the short requirement of PDP twilight sunset, can be widely used in during plasma flat-plate shows.This After substantial amounts of experimental exploring, the single-phase RE niobate-titanate base fluorescent powder having finally given the present invention produces the inventor of invention Thing, it is keeping GdNbTiO6The excellent properties being obtained in that on the premise of the phase structure of matrix are for those skilled in the art For be difficult to expect.
In sum, the fluorescent material obtained by the present invention has that chemical stability is good, nontoxic, radiationless, high brightness, height The advantages of excitation, high conversion efficiency.And technical process is safe, simple, easily controllable.
Brief description
Fig. 1 is embodiment 1, comparative example 1, and 12 3 sample XRD spectrums of embodiment compare；
It can be seen that the fluorescent material obtained by embodiment 1 and GdNbTiO6Structure is consistent, as shown in Figure 1, implements The diffraction maximum of the product obtained by example 1 and GdNbTiO6The position consistency of diffraction maximum, and do not have miscellaneous peak to occur it is known that embodiment 1 Obtained product is single-phase, and the product that comparative example 1 obtains is multiphase, from figure this it appears that it comprises a small amount of TiO2With GdNbO4, the product that embodiment 12 obtains also is single-phase.
Fig. 2 is embodiment 1, embodiment 2, embodiment 4, and 6 four sample XRD spectrums of embodiment compare；
It can be seen that embodiment 2, embodiment 4, the sample XRD spectrum that embodiment 6 is obtained and embodiment 1 sample XRD spectrum is completely the same, does not have miscellaneous peak to occur, is all GdNbTiO in the present invention6The single composition sample of phosphor host Product.
Fig. 3 is embodiment 1, embodiment 7, embodiment 9, and 11 4 sample XRD spectrums of embodiment compare；
Product obtained by embodiment 1 is single-phase, and in its XRD spectrum, all diffraction maximums belong to GdNbTiO6.Can by Fig. 3 Know, embodiment 7, embodiment, 9, the position consistency of the diffraction maximum of the sample obtained by embodiment 11 and embodiment 1 diffraction maximum, and Miscellaneous peak is not had to occur it is known that embodiment 7, embodiment, 9, the product obtained by embodiment 11 is all single-phase.
Fig. 4 is the exciting light spectrogram of fluorescent material and launching light spectrogram that embodiment 1 is obtained；
It is 509nm by fixing excitation wavelength, the excitation spectrum of the fluorescent material that measurement embodiment 1 is obtained.Its excitation spectrum It is predominantly located at the Broad excitation band of ultraviolet region 200～320nm, excite the most by force peak value to be located near 273nm.
It is 273nm by fixing excitation wavelength, the emission spectrum of the fluorescent material that measurement embodiment 1 is obtained, permissible from figure Find out, the emission spectrum of embodiment 1 is predominantly located at the broad emission band of 400～650nm scope, it is attached that its strongest is located at 509nm Closely, corresponding fluorescent material sends bright blue green light.It follows that embodiment 1 is a kind of self-activating fluorescent material.
Fig. 5 is the exciting light spectrogram of the fluorescent material that embodiment 2～6 is obtained；
It is 614nm by fixing excitation wavelength, the excitation spectrum of the fluorescent material that measurement embodiment 2～6 is obtained, can from figure To find out, occur at 200～320nm, 361nm, 382nm, 393nm, 416nm and 464nm in the range of 200～500 Excitation peak, is wherein located at the Broad excitation band intensity in the range of ultraviolet region 200～320nm and is significantly stronger than other excitation peaks；And And the intensity of the prepared excitation spectrum of fluorescent material of embodiment 6 is higher than the excitation spectrum of the fluorescent material that embodiment 2～5 is obtained.
Fig. 6 is the emission spectrum comparison diagram of the fluorescent material that embodiment 2～6 is obtained；
According to embodiment in Fig. 5 2～6 excitation peak feature, it is 273nm by fixing excitation wavelength, measures embodiment 2～6 The emission spectrum of prepared fluorescent material, it can be seen that the position of emission peak is not changed in, the launching light of embodiment 2～6 Spectrum is all located at emission peak near 594nm, 614nm, 656nm and 705nm in the range of 500～725nm, its strongest Near 614nm, increase with doping content, the transmitting peak intensity at 614nm improves constantly；It is obvious that embodiment 6 is made The intensity of the emission spectrum of fluorescent material obtaining is higher than the fluorescent material that embodiment 2～5 is obtained.
Fig. 7 is the excitation spectrum comparison diagram of the fluorescent material that embodiment 7～11 is obtained；
It is 577nm by fixing excitation wavelength, the excitation spectrum of the fluorescent material that measurement embodiment 7～11 is obtained, from figure As can be seen that going out at 200～320nm, 353nm, 387nm, 427nm, 451nm and 477nm in the range of 200～500 Show excitation peak, be wherein located at the Broad excitation band intensity in the range of ultraviolet region 200～320nm and be significantly stronger than other excitation peaks； And the intensity of the excitation spectrum of fluorescent material that embodiment 11 is obtained is higher than the exciting light of the fluorescent material that embodiment 7～10 is obtained Spectrum.
Fig. 8 is the emission spectrum comparison diagram of the fluorescent material that embodiment 7～11 is obtained；
According to embodiment in Fig. 7 7～11 excitation peak feature, it is 273nm by fixing excitation wavelength, measurement embodiment 7～ 11 be obtained fluorescent material emission spectrum, it can be seen that the position of emission peak is not changed in, embodiment 7～11 send out Penetrate spectrum and be all located at, near 482nm, 577nm and 660nm, emission peak occurs in the range of 500～725nm, its strongest Near 577nm, increase with doping content, the transmitting peak intensity at 577nm improves constantly；It is obvious that embodiment 11 The intensity of the emission spectrum of prepared fluorescent material is higher than the fluorescent material that embodiment 7～10 is obtained.
Fig. 9 is embodiment 1, the chromaticity coordinate figure of the fluorescent material that embodiment 6 and embodiment 11 are obtained；
Chromaticity coordinate analysis is carried out to this fluorescent material using CIE chromaticity diagram, determines that the chromaticity coordinate of embodiment 1 is (0.228,0.318), shows that it sends blue green light on chromaticity coordinate figure；Determine embodiment 6 chromaticity coordinate be (0.594, 0.379), chromaticity coordinate figure shows it sends warm HONGGUANG；Determine embodiment 11 chromaticity coordinate be (0.343,0.449), Chromaticity coordinate figure shows that it sends green-yellow light.
Figure 10 is the fluorescence lifetime curve of the fluorescent material that embodiment 6 is obtained；
By this fluorescent material is carried out with fluorescence lifetime test, in figure circle represents experiment value, and solid line is origin matching number According to fitting data coincidence formula I=I0+A1*exp(-t/t1)+A2*exp(-t/t2), the fluorescence lifetime calculating fluorescent material is 0.056ms.
Figure 11 is the fluorescence lifetime curve of the fluorescent material that embodiment 11 is obtained；
By this fluorescent material is carried out with fluorescence lifetime test, in figure five-pointed star represents experiment value, and solid line is origin matching Data, fitting data coincidence formula I=I0+A1*exp(-t/t1)+A2*exp(-t/t2), the fluorescence lifetime calculating fluorescent material is 0.045ms.
Figure 12 is embodiment 1 and the excitation spectrum of comparative example 2 and emission spectrum comparison diagram.
Specific embodiment
It is intended to further illustrate the present invention with reference to embodiments, and the unrestricted present invention.
Embodiment 1：GdNbTiO6The preparation of fluorescent material substrate
Weigh 0.7820gNb2O5、1.0059g Gd2O3With 0.4447g TiO2Put in agate mortar and grind 30 minutes, make Raw material mix homogeneously.Raw material is put into be placed in crucible in Muffle furnace carry out two-step sintering (1200 DEG C of first stage sintering temperature, Insulation was cooled to room temperature with stove after 12 hours, ground 20 minutes；1250 DEG C of second stage sintering temperature, cold with stove after being incubated 12 hours But to room temperature, two-step sintering heating rate is 5 DEG C/min.Burned sample is taken out and grinds, you can prepared GdNbTiO6Glimmering Light powder substrate.
Comparative example 1：GdNbTiO6The preparation of fluorescent material substrate
Weigh 0.7820gNb2O5、1.0059g Gd2O3With 0.4447g TiO2Put in agate mortar and grind 30 minutes, make Raw material mix homogeneously.Raw material is put into be placed in crucible in Muffle furnace carry out two-step sintering (1000 DEG C of first stage sintering temperature, Insulation was cooled to room temperature with stove after 12 hours, ground 20 minutes；1100 DEG C of second stage sintering temperature, cold with stove after being incubated 12 hours But to room temperature, two-step sintering heating rate is 5 DEG C/min.Burned sample is taken out and grinds, you can prepared GdNbTiO6Glimmering Light powder substrate control sample 1.
Embodiment 2：(Gd0.99Eu0.01)NbTiO6The preparation of fluorescent material
Weigh 0.7820g Nb2O5、0.9959g Gd2O3、0.4447g TiO2With 0.0098g Eu2O3, remaining step with Embodiment 1 is identical.
Embodiment 3：(Gd0.98Eu0.02)NbTiO6The preparation of fluorescent material
Weigh 0.7820g Nb2O5、0.9858g Gd2O3、0.4447g TiO2With 0.0195g Eu2O3, remaining step with Embodiment 1 is identical.
Embodiment 4：(Gd0.97Eu0.03)NbTiO6The preparation of fluorescent material
Weigh 0.7820g Nb2O5、0.9758g Gd2O3、0.4447g TiO2With 0.0293g Eu2O3, remaining step with Embodiment 1 is identical.
Embodiment 5：(Gd0.96Eu0.04)NbTiO6The preparation of fluorescent material
Weigh 0.7820g Nb2O5、0.9657g Gd2O3、0.4447g TiO2With 0.0391g Eu2O3, remaining step with Embodiment 1 is identical.
Embodiment 6：(Gd0.95Eu0.05)NbTiO6The preparation of fluorescent material
Weigh 0.7820g Nb2O5、0.9556g Gd2O3、0.4447g TiO2With 0.0488g Eu2O3, remaining step with Embodiment 1 is identical.
Embodiment 7：(Gd0.99Dy0.01) NbTiO6 fluorescent material preparation
Weigh 0.7820g Nb2O5,0.9959g Gd2O3,0.4447g TiO2 and 0.0104g Dy2O3, remaining step Same as Example 1.
Embodiment 8：(Gd0.98Dy0.02)NbTiO6The preparation of fluorescent material
Weigh 0.7820g Nb2O5、0.9858g Gd2O3、0.4447g TiO2With 0.0207g Dy2O3, remaining step with Embodiment 1 is identical.
Embodiment 9：(Gd0.97Dy0.03)NbTiO6The preparation of fluorescent material
Weigh 0.7820g Nb2O5、0.9758g Gd2O3、0.4447g TiO2With 0.0311g Dy2O3, remaining step with Embodiment 1 is identical.
Embodiment 10：(Gd0.96Dy0.04)NbTiO6The preparation of fluorescent material
Weigh 0.7820g Nb2O5、0.9657g Gd2O3、0.4447g TiO2With 0.0414g Dy2O3, remaining step with Embodiment 1 is identical.
Embodiment 11：(Gd0.95Dy0.05)NbTiO6The preparation of fluorescent material
Weigh 0.7820g Nb2O5、0.9556g Gd2O3、0.4447g TiO2With 0.0518g Dy2O3, remaining step with Embodiment 1 is identical.
Embodiment 12：GdNbTiO6The preparation of fluorescent material substrate
Weigh 0.7820g Nb2O5、1.0059g Gd2O3With 0.4447g TiO2Put in agate mortar and grind 30 minutes, Make raw material mix homogeneously.Raw material is put into be placed in crucible in Muffle furnace and carry out two-step sintering.First stage sintering temperature 1200 DEG C, insulation was cooled to room temperature with stove after 12 hours, ground 20 minutes；1300 DEG C of second stage sintering temperature, insulation 12 hours after with Stove is cooled to room temperature, and two-step sintering heating rate is 5 DEG C/min.Burned sample is taken out and grinds, also can be obtained GdNbTiO6Fluorescent material substrate.
Comparative example 2：YNbTiO6Fluorescent material
Weigh 2.1347gNb2O5、1.7100g Gd2O3With 1.2109g TiO2Put in agate mortar and grind 30 minutes, make Raw material mix homogeneously.Raw material is put into be placed in crucible in Muffle furnace carry out two-step sintering (1000 DEG C of first stage sintering temperature, Insulation was cooled to room temperature with stove after 12 hours, ground 20 minutes；1250 DEG C of second stage sintering temperature, cold with stove after being incubated 12 hours But to room temperature, two-step sintering heating rate is 5 DEG C/min.Burned sample is taken out and grinds, that is, document YNbTiO is obtained6 Fluorescent material substrate.In order to preferably study the luminosity of fluorescent material of the present invention, select document YNbTiO6Fluorescent material is as ginseng Compare fluorescent material.Figure 12 gives excitation spectrum and the emission spectrum comparison diagram of embodiment 1 and comparative example 2.Can from figure Go out, when 274nm is as excitation wavelength, apparently higher than comparative example 2, the emissive porwer of embodiment 1 is about for the launching efficiency of embodiment 1 For comparative example 2 2.7 times.

Claims (7)

1. a kind of self-activation niobate-titanate base fluorescent powder it is characterised in that
This fluorescent material is with GdNbTiO6For matrix；Wherein, mix 0.01～0.05at.%Eu3+Enter Gd3+Position, obtains chemistry Formula is Gd(1‐x)NbTiO6:xEu3+Single-phase red fluorescence powder；Mix 0.01～0.05at.%Dy3+Enter GdNbTiO6In matrix Gd3+Position, obtaining chemical formula is Gd(1‐y)NbTiO6:yDy3+Single-phase yellowish green fluorescent powder；X or y be molal quantity 0.01～ 0.05.
2. fluorescent material according to claim 1 is it is characterised in that GdNbTiO6Matrix belongs to Pbcn (No.60) space group, Cell parameter isZ=4.
3. the preparation method of the self-activation niobate-titanate base fluorescent powder described in claim 1 is：It is Gd according to chemical formula(1‐x) NbTiO6:xEu3+Or Gd(1‐y)NbTiO6:yDy3+Required nonstoichiometric molar ratio weighs Gd2O3、Nb2O5And TiO2, and Eu2O3Or Dy2O3；It is fully ground, then carries out two-step sintering and obtain, first stage sintering temperature is 1000～1200 DEG C, sintering After be cooled to room temperature, grind；Then carry out second stage sintering under conditions of temperature is 1250 DEG C～1350 DEG C, cooling, grind Mill, obtains final product.
4. preparation method according to claim 3 it is characterised in that the first stage sintering heating rate be 3～5 DEG C/ min.
5. the preparation method according to claim 3 or 4 is it is characterised in that the heating rate of second stage sintering is 3～5 ℃/min.
6. preparation method according to claim 3 it is characterised in that the first stage sintering temperature retention time 10～15h.
7. preparation method according to claim 3 it is characterised in that second stage sintering temperature retention time 10～15h.
CN201610845827.1A 2016-09-23 2016-09-23 Self-activated titanoniobate-based fluorescent powder and preparation method thereof Pending CN106433642A (en)

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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
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CN107601553B (en) * 2017-09-12 2023-11-10 南京工业大学 Functional potassium magnesium titanate and preparation method thereof
CN109762564A (en) * 2019-03-13 2019-05-17 常州工程职业技术学院 A kind of europium ion Eu3+The titanate red fluorescence powder of activation, preparation method and applications

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