CN103275720B - Sodium lanthanum vanadate-based luminous material as well as preparation method and application thereof - Google Patents

Sodium lanthanum vanadate-based luminous material as well as preparation method and application thereof Download PDF

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CN103275720B
CN103275720B CN201310177006.1A CN201310177006A CN103275720B CN 103275720 B CN103275720 B CN 103275720B CN 201310177006 A CN201310177006 A CN 201310177006A CN 103275720 B CN103275720 B CN 103275720B
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sodium
ion
lanthanum
luminescent material
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CN103275720A (en
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黄彦林
徐传艳
李亚东
袁蓓玲
关莹
秦琳
陶正旭
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Chongqing Golute New Material Technology Co Ltd
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Suzhou University
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Abstract

The invention relates to a sodium lanthanum vanadate-based luminous material as well as a preparation method and application thereof and belongs to the technical field of inorganic luminous materials. The luminous material is activated by rare earth europium ion Eu<3+> and has the chemical formula of Na3La8-xEuxV3O21, wherein x is the molar percent of Eu<3+> doping, and x is more than or equal to 0.0001 and less than or equal to 0.25. The pure-phase red fluorescent powder with excellent luminous performance is prepared by respectively employing a high-temperature solid state method and a hydrothermal method. The luminous material has strong stimulation in the range from 300nm to 450nm, is meshed with the transmitting wavelength of the near ultraviolet light-emitting diode (LED) chip, and the transmitting light is mainly the red light with the wavelength of 621nm. The prepared powder is high in purity, high in crystallinity and high in luminous strength; and the luminous material is simple in preparation process and low in equipment requirement and production cost and has wide application prospect.

Description

A kind of sodium lanthanum vanadate based luminescent material, preparation method and application thereof
Technical field
The present invention relates to a kind of europium ion Eu 3+the vanadate based luminescent material activated, preparation method and application, belong to inorganic fluorescent material technical field.
Background technology
Rare-earth vanadate luminescent powder is a kind of important luminous host.The luminescent material chemistry and the thermal stability that take rare-earth vanadate as matrix are high, are widely used in high-pressure mercury lamp, plasma flat-plate display and Field Emission Display.The sixties in last century, emitting red light powder YVO 4: Eu is developed successfully, in order to replace non-rare earth red fluorescent powder, and makes brightness improve 40%.But along with the expansion of modern science and technology and fluorescent material application, YVO 4: Eu red fluorescence powder more and more can not meet the needs of development.Such as, YVO 4: Eu near ultraviolet and blue region launching efficiency low.
Chinese invention patent CN 101591540A " a kind of rare-earth vanadate LaVO 4: the preparation method of Eu red fluorescence powder " disclose the fluorescent material that a kind of vanadic acid lanthanum mixes europium, utilize microwave-hydrothermal method to prepare, there is reaction temperature low, the advantage that the reaction time is short.Chinese invention patent CN 102191060A " a kind of vanadate phosphor and preparation method thereof " discloses a kind of fluorescent material of rear-earth-doped vanadic acid yttrium, and prepared fluorescent material, under the exciting light of 314 nm, launches the ruddiness that centre wavelength is 615 nanometers.In Chinese invention patent CN 102399558A " a kind of vanadate red phosphor, preparation method and application ", disclose vanadate red phosphor, its molecular formula is NaM iIla1 -x-y(VO 4) 2: Eu x, RI iI y, wherein M iIfor alkaline-earth metal magnesium ion Mg 2+, calcium ion Ca 2+, strontium ion Sr 2+, barium ions Ba 2+with zinc ion Zn 2+in one, or two or more combination, R iIIfor rare earth samarium ion Sm 3+, gadolinium ion Gd 3+, terbium ion Tb 3+, dysprosium ion Dy 3+, lutetium ion Lu 3+and ruthenium ion Y 3+in at least one, x is europium ion Eu 3+the molar percentage coefficient of doping, 0.0001≤x≤0.6; Y is rare earth ion R iIIreplace lanthanum ion La 3+molar percentage coefficient, 0.0001≤y≤0.6.In technique scheme, Eu 3+the red fluorescence powder of the vanadate matrix activated absorbs weak near ultraviolet and blue region.
The result of study of existing document shows, Eu 3+the rare-earth vanadate based luminescent material Na activated 3la 8-xeu xv 3o 21have no report.
Summary of the invention
The present invention seeks to overcome Eu in prior art 3+the vanadate red phosphor activated absorbs weak weak point near ultraviolet and blue region, provides that a kind of degree of crystallinity is high, luminous efficiency is remarkable, preparation method is simple, the sodium lanthanum vanadate based luminescent material of environmental protection, preparation method and application thereof.
For reaching above goal of the invention, the technical solution used in the present invention is to provide a kind of sodium lanthanum vanadate based luminescent material, and its chemical formula is Na 3la 8-xeu xv 3o 21, wherein, x is Eu 3+doping, 0.0001≤x≤0.25; Described luminescent material has strong exciting light in 300 nanometers and 450 nm, and its utilizing emitted light is the red luminescence of 621 nm.
The method preparing sodium lanthanum vanadate based luminescent material of the present invention adopts a high temperature solid-state method, comprises the following steps:
1. with containing the compound of sodium ion, the compound containing lanthanum ion, the compound containing europium ion and containing the compound of vanadium ion for raw material, by general formula Na 3la 8-xeu xv 3o 21, in 0.0001≤x≤0.25, the stoichiometric proportion of corresponding element takes each raw material, mixes after grinding;
2. by the raw material mixed temperature be 300 ~ 600 DEG C, precalcining 1 ~ 2 time under air atmosphere, insulation 3 ~ 6 h, Temperature fall is to room temperature;
fully ground by powder after precalcining, in air atmosphere, with the temperature calcination of 1000 ~ 1200 DEG C, insulation 6 ~ 10h, obtains a kind of europium ion Eu after cooling naturally 3+the sodium lanthanum vanadate based luminescent material Na activated 3la 8-xeu xv 3o 21, wherein x is Eu 3+doping, 0.0001≤x≤0.25.
Prepare in the technical scheme of sodium lanthanum vanadate based luminescent material at employing high temperature solid-state method of the present invention, the described compound containing sodium ion is one or more the combination in sodium carbonate, sodium acid carbonate, sodium nitrate, sodium oxide molybdena.The described compound containing europium ion is the one in europium oxide, europium nitrate, or the combination of two kinds.The described compound containing vanadium ion is the one in vanadic oxide, vanadium trioxide, or the combination of two kinds.The described compound containing lanthanum ion is the one in lanthana, lanthanum nitrate, or the combination of two kinds.
The method of another kind of preparation sodium lanthanum vanadate based luminescent material of the present invention adopts hydro thermal method, comprises the following steps:
1. general formula Na is pressed 3la 8-xeu xv 3o 21the stoichiometric proportion of middle corresponding element, takes the oxide containing lanthanum ion and europium ion, is that two kinds of compounds are dissolved as rare earth nitrate solution by the red fuming nitric acid (RFNA) of 3 ~ 5 times of lanthanum atoms and europium atom, dilutes with the deionized water of 5 ~ 10 times of volumes with molal quantity;
2. general formula Na is pressed 3la 8-xeu xv 3o 21the stoichiometric proportion of middle corresponding element, takes NaNO 3and NH 4vO 3, be dissolved in the water respectively under the condition of 50 ~ 70 DEG C in temperature, be configured to NaNO 3and NH 4vO 3solution;
3. under magnetic agitation condition, by NaNO 3solution and NH 4vO 3solution joins in the rare earth nitrate solution that 1. step obtain, then to add molal quantity be the citric acid of 1 ~ 3 times of rare earth atom is complexing agent, obtains mixed solution; Regulate the pH value of mixed solution to be 5 ~ 8 with ammoniacal liquor and nitric acid, stir 1 ~ 2 h;
4. the solution that 3. step obtains is poured in reactor, add deionized water and make liquor capacity reach 70 ~ 80% of reactor volume, be incubated 4 ~ 8h under the condition of 170 ~ 200 DEG C at oven temperature after sealing, after cooling, be precipitated thing through centrifugal treating; After sediment being spent deionized water, oven dry, obtain a kind of europium ion Eu 3+the sodium lanthanum vanadate based luminescent material Na activated 3la 8-xeu xv 3o 21, wherein x is Eu 3+doping, 0.0001≤x≤0.25.
Technical solution of the present invention also comprises a kind of application of described sodium lanthanum vanadate based luminescent material, described luminescent material is coordinated with appropriate blueness and green emitting phosphor, apply and be packaged in outside ultraviolet and blue-ray LED diode chip for backlight unit, preparing white light LEDs illuminating device.
Compared with prior art, technical solution of the present invention advantage is:
1, with existing red vanadate phosphor as YVO 4: Eu 3+, LaVO 4: Eu 3+compare, the red fluorescence powder prepared by technical solution of the present invention has stronger exciting near ultraviolet (300 nm) and blue region (450 nm), it is coordinated with appropriate blueness and green emitting phosphor, apply and be packaged in outside ultraviolet and blue-ray LED diode chip for backlight unit, preparing white light LEDs illuminating device.
2, with other sulfide Y 2o 2s:Eu 3+, halide etc. is host material red fluorescence powder is compared, the preparation process of host material of the present invention is pollution-free, safety, environmental protection.
3, prepared powder degree of crystallinity is high, and chemistry and Heat stability is good, luminous efficiency significantly improves.
Accompanying drawing explanation
The Na of Fig. 1 obtained by the embodiment of the present invention 1 3la 7.99eu 0.01v 3o 21the X-ray powder diffraction spectrogram of material sample;
The Na of Fig. 2 obtained by the embodiment of the present invention 1 3la 7.99eu 0.01v 3o 21the utilizing emitted light spectrogram that material sample monitors at ambient temperature;
The Na of Fig. 3 obtained by the embodiment of the present invention 2 3la 7.9eu 0.1v 3o 21the X-ray powder diffraction spectrogram of material sample and the contrast of standard spectrogram;
The Na of Fig. 4 obtained by the embodiment of the present invention 2 3la 7.9eu 0.1v 3o 21the excitation and emission spectra figure that material sample monitors at ambient temperature;
The Na of Fig. 5 obtained by the embodiment of the present invention 2 3la 7.9eu 0.1v 3o 21the decay of luminescence curve chart that material sample monitors at ambient temperature.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment, technical solution of the present invention is described further.
Embodiment 1
According to chemical formula Na 3la 7.99eu 0.01v 3o 21in the stoichiometric proportion of each element, take Na respectively 2cO 30.795 gram, La 2o 36.512 gram, Eu 2o 30.009 gram, V 2o 51.365 gram.Grind in agate mortar, and fully mix.The powder mixed is carried out in air atmosphere first time calcining, temperature is 300 DEG C, is incubated 3 h, takes out sample after Temperature fall to room temperature.Again fully ground in agate mortar by powder after first time calcining, under air atmosphere, carry out second time sintering, temperature is 600 DEG C, is incubated 6 h, takes out sample and again grind after Temperature fall to room temperature.Uniform powder will be ground calcine at 1000 DEG C, be incubated 6 h, naturally finally obtain Na after cooling 3la 7.99eu 0.01v 3o 21red luminescent phosphor.
See accompanying drawing 1, its Na obtained by the present embodiment 3la 7.99eu 0.01v 3o 21the X-ray powder diffraction pattern of material sample.As seen from Figure 1, the Na obtained by the present embodiment 3la 7.99eu 0.01v 3o 21material is pure phase and degree of crystallinity is more complete.
See accompanying drawing 2, its Na obtained by the present embodiment 3la 7.99eu 0.01v 3o 21the utilizing emitted light spectrogram that material sample monitors at ambient temperature.As shown in Figure 2, the Na obtained by the present embodiment 3la 7.99eu 0.01v 3o 21material is main based on the red luminescence of 621 nm wavelength, and luminous intensity is higher.
Embodiment 2
According to chemical formula Na 3la 7.9eu 0.1v 3o 21in the stoichiometric proportion of each element, take 1.275 grams of NaNO 3be dissolved in 30 ml water, take 1.755 g NH 4vO 3dissolving is gone in 40 ml water, and 50 DEG C of water-baths are configured to solution respectively; Take 6.439 grams of La again 2o 3with 0.09 gram of Eu 2o 3being dissolved in 24 ml concentration is in the red fuming nitric acid (RFNA) of 2.5 mol/ml, and dilutes with deionized water; By NaNO 3and NH 4vO 3solution slowly joins in the rare earth nitrate solution under magnetic agitation, then adds 0.04mol citric acid as complexing agent; Solution PH is regulated to be 6 by dust technology and ammoniacal liquor, abundant stirring is again after deionized water dilution, the solution getting reactor capacity 80 % is poured in hydrothermal reaction kettle, 6 h are incubated in 180 DEG C of baking ovens, by the solution centrifugal taking precipitate obtained, and spend deionized water post-drying and obtain red fluorescence powder Na 3la 7.9eu 0.1v 3o 21.
See accompanying drawing 3, its Na obtained by the present embodiment 3la 7.9eu 0.1v 3o 21the X-ray powder diffraction pattern of material sample and the comparison diagram of standard spectrum.As seen from Figure 3, the Na obtained by the present embodiment 3la 7.9,eu 0.1v 3o 21material is pure phase and degree of crystallinity is more complete.
See accompanying drawing 4, its Na obtained by the present embodiment 3la 7.9eu 0.1v 3o 21the excitation and emission spectra figure that material sample monitors at ambient temperature.As shown in Figure 4, the Na obtained by the present embodiment 3la 7.9eu 0.1v 3o 21material is under 333 nanometer excitation wavelengths, produce stronger luminescence, main based on the red luminescence of 621 nano wave lengths, it and near ultraviolet LED chip emission wavelength are very identical, it is coordinated appropriate blueness and green emitting phosphor, and apply and be packaged in outside ultraviolet and blue-ray LED diode chip for backlight unit, can be applicable to prepare White-light LED illumination device.
See accompanying drawing 5, its Na obtained by the present embodiment 3la 7.9eu 0.1v 3o 21material sample decay of luminescence curve chart, as can be seen from Figure 5, the Na obtained by the present embodiment 3la 7.9eu 0.1v 3o 21in the luminescent material illumination that the Decay of material emission can be applied to display device, three-color fluorescent lamp and Field Emission Display completely and display device.
Embodiment 3
According to chemical formula Na 3la 7.75eu 0.25v 3o 21in the stoichiometric proportion of each element, take NaNO respectively 31.275 gram, La 2o 36.316 gram, Eu 2o 30.22 gram, V 2o 31.125 gram.Grind in agate mortar, and fully mix.Calcined in air atmosphere by the powder mixed, temperature is 500 DEG C, is incubated 5 h, takes out sample after Temperature fall to room temperature.Again grind, uniform powder will be ground and calcine at 1200 DEG C, and be incubated 10 h, naturally finally obtain Na after cooling 3la 7.75eu 0.25v 3o 21red luminescent phosphor.
Na obtained by the present embodiment 3la 7.75eu 0.25v 3o 21material sample architectural feature, emission spectrum information, similar to embodiment 1.
Embodiment 4
According to chemical formula Na 3la 7.8eu 0.2v 3o 21in the stoichiometric proportion of each element, take 1.275 grams of NaNO 3be dissolved in 30 ml water, take 1.755 grams of NH 4vO 3dissolving is gone in 40 ml water, and 70 DEG C of water-baths are configured to solution respectively; Take 6.357 grams of La again 2o 3with 0.18 gram of Eu 2o 3being dissolved in 24 ml concentration is in the red fuming nitric acid (RFNA) of 2.5 mol/ml, and dilutes with deionized water; By NaNO 3and NH 4vO 3solution slowly joins in the rare earth nitrate solution under magnetic agitation, then adds 0.06 mol citric acid as complexing agent; Solution PH is regulated to be 6 by dust technology and ammoniacal liquor, abundant stirring is again after deionized water dilution, and the solution getting reactor capacity 80% is poured in hydrothermal reaction kettle, is incubated 5 h in 200 DEG C of baking ovens, by the solution centrifugal taking precipitate obtained, and spend deionized water post-drying and obtain red fluorescence powder Na 3la 7.8eu 0.2v 3o 21.
Na obtained by the present embodiment 3la 7.8eu 0.2v 3o 21material sample architectural feature, excitation and emission spectra information, similar to embodiment 2.
Embodiment 5
According to chemical formula Na 3la 7.85eu 0.15v 3o 21in the stoichiometric proportion of each element, take NaHCO respectively 30.84 gram, NaNO 30.425 gram, La 2o 36.398 grams, Eu (NO 3) 36H 2o 335 grams, V 2o 31.125 gram.Grind in agate mortar, and fully mix.The powder mixed is carried out in air atmosphere first time calcining, temperature is 400 DEG C, is incubated 5 h, takes out sample after Temperature fall to room temperature.By first time, the powder of calcining again fully grinds in agate mortar, and under air atmosphere, carry out second time sintering, temperature is 500 DEG C, is incubated 4 h, takes out sample and again grind after Temperature fall to room temperature.Uniform powder will be ground calcine at 1100 DEG C, be incubated 8 h, naturally finally obtain Na after cooling 3la 7.85eu 0.15v 3o 21red luminescent phosphor.
Na obtained by the present embodiment 3la 7.85eu 0.15v 3o 21material sample architectural feature and emission spectrum information similar to Example 1.

Claims (4)

1. a sodium lanthanum vanadate based luminescent material, is characterized in that: its chemical formula is Na 3la 8-xeu xv 3o 21, wherein, x is Eu 3+doping, 0.0001≤x≤0.25; Described luminescent material has strong exciting light in 300 nanometers and 450 nanometers, and its utilizing emitted light is the red luminescence of 621 nanometers.
2. a preparation method for sodium lanthanum vanadate based luminescent material as claimed in claim 1, is characterized in that adopting high temperature solid-state method, comprises the following steps:
1. with containing the compound of sodium ion, the compound containing lanthanum ion, the compound containing europium ion and containing the compound of vanadium ion for raw material, by general formula Na 3la 8-xeu xv 3o 21, in 0.0001≤x≤0.25, the stoichiometric proportion of corresponding element takes each raw material, mixes after grinding;
2. by the raw material mixed temperature be 300 ~ 600 DEG C, precalcining 1 ~ 2 time under air atmosphere, insulation 3 ~ 6 h, Temperature fall is to room temperature;
fully ground by powder after precalcining, in air atmosphere, with the temperature calcination of 1000 ~ 1200 DEG C, insulation 6 ~ 10h, obtains a kind of europium ion Eu after cooling naturally 3+the sodium lanthanum vanadate based luminescent material Na activated 3la 8-xeu xv 3o 21, wherein x is Eu 3+doping, 0.0001≤x≤0.25;
The described compound containing sodium ion is one or more the combination in sodium carbonate, sodium acid carbonate, sodium nitrate, sodium oxide molybdena; The described compound containing europium ion is the one in europium oxide, europium nitrate, or the combination of two kinds; The described compound containing vanadium ion is the one in vanadic oxide, vanadium trioxide, or the combination of two kinds; The described compound containing lanthanum ion is the one in lanthana, lanthanum nitrate, or the combination of two kinds.
3. a preparation method for sodium lanthanum vanadate based luminescent material as claimed in claim 1, is characterized in that adopting hydro thermal method, comprises the following steps:
1. general formula Na is pressed 3la 8-xeu xv 3o 21the stoichiometric proportion of middle corresponding element, takes the oxide containing lanthanum ion and europium ion, is that two kinds of compounds are dissolved as rare earth nitrate solution by the red fuming nitric acid (RFNA) of 3 ~ 5 times of lanthanum atoms and europium atom, dilutes with the deionized water of 5 ~ 10 times of volumes with molal quantity;
2. general formula Na is pressed 3la 8-xeu xv 3o 21the stoichiometric proportion of middle corresponding element, takes NaNO 3and NH 4vO 3, be dissolved in the water respectively under the condition of 50 ~ 70 DEG C in temperature, be configured to NaNO 3and NH 4vO 3solution;
3. under magnetic agitation condition, by NaNO 3solution and NH 4vO 3solution joins in the rare earth nitrate solution that 1. step obtain, then to add molal quantity be the citric acid of 1 ~ 3 times of rare earth atom is complexing agent, obtains mixed solution; Regulate the pH value of mixed solution to be 5 ~ 8 with ammoniacal liquor and nitric acid, stir 1 ~ 2 h;
4. the solution that 3. step obtains is poured in reactor, add deionized water and make liquor capacity reach 70 ~ 80% of reactor volume, be incubated 4 ~ 8h under the condition of 170 ~ 200 DEG C at oven temperature after sealing, after cooling, be precipitated thing through centrifugal treating; After sediment being spent deionized water, oven dry, obtain a kind of europium ion Eu 3+the sodium lanthanum vanadate based luminescent material Na activated 3la 8-xeu xv 3o 21, wherein x is Eu 3+doping, 0.0001≤x≤0.25.
4. an application for sodium lanthanum vanadate based luminescent material as claimed in claim 1, coordinates described luminescent material with appropriate blueness and green emitting phosphor, applies and be packaged in outside ultraviolet and blue-ray LED diode chip for backlight unit, prepare white light LEDs illuminating device.
CN201310177006.1A 2013-05-14 2013-05-14 Sodium lanthanum vanadate-based luminous material as well as preparation method and application thereof Expired - Fee Related CN103275720B (en)

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CN104673314B (en) * 2015-01-28 2017-03-01 江苏师范大学 Vanadate-based down-conversion luminescent material and preparation method thereof
CN104910914B (en) * 2015-05-08 2017-05-24 江苏师范大学 Lanthanum boron vanadate-based red fluorescent material and preparation method thereof
CN107201228A (en) * 2017-07-21 2017-09-26 江苏师范大学 A kind of Eu3+Ion-activated vanadium silicate material and preparation method and application
CN109321250A (en) * 2018-10-25 2019-02-12 惠州学院 A kind of nanoscale lanthanum orthophosphate yttrium base red fluorescent powder and preparation method thereof
CN109777421B (en) * 2019-03-15 2021-04-20 常州工程职业技术学院 Europium ion Eu3+Activated red fluorescent powder, preparation method and application
CN109988575B (en) * 2019-04-28 2021-02-26 常州工程职业技术学院 Eu (Eu)3+Ion-activated vanadium-phosphorus niobate red fluorescent powder, preparation method and application thereof

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