CN109504381A - The method of microwave and the double outfield auxiliary liquid phase synthesis bismuth europium codope molybdate red phosphors of ultrasonic wave - Google Patents
The method of microwave and the double outfield auxiliary liquid phase synthesis bismuth europium codope molybdate red phosphors of ultrasonic wave Download PDFInfo
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Abstract
The invention belongs to fluorescent powder technical field of powdered material preparation, more particularly to a kind of method of microwave and the double outfield auxiliary liquid phase synthesis bismuth europium codope molybdate red phosphor body materials of ultrasonic wave, (1) is using sodium molybdate, calcium nitrate, bismuth nitrate, europium nitrate solution as raw material；Using urea as precipitating reagent, certain stoichiometric is subjected to ingredient；(2) feed liquid is placed in microwave cooperates with auxiliary liquid phase coprecipitation to prepare fluorescent powder presoma with the double outfields of ultrasonic wave；(3) presoma sediment is washed and is filtered；(4) dry and thermal decomposition, obtains 2~4 μm of bismuth europium codope molybdate red phosphor products C a of Monodispersed1‑x‑yMoO4:(Eu3+ y,Bi3+ x).Due to the synergistic effect of " cavitation effect " of " the interior heating " and ultrasonic wave of microwave, obtained product near-spherical, regular appearance, crystallization degree are high, and the obtained fluorescent phosphor service life is long, and luminous intensity is higher than single europium and adulterates molybdate Ca1‑xMoO4:Eu3+ xFluorescent powder；Its chromaticity coordinates is the red fluorescence powder raw material that (0.6598,0.3398) is suitable as white light LEDs.
Description
Technical field
The invention belongs to the preparation technical fields of luminescent powder material, and in particular to one kind is with sodium molybdate, calcium nitrate feed liquid
For primary raw material, using urea as precipitating reagent, and liquid phase synthesis bismuth europium codope molybdic acid is assisted using microwave and the double outfields of ultrasonic wave
The method of salt red fluorescence powder.
Technical background
Currently, White LED has become forth generation lighting source, and white light LEDs in the market are mostly by fluorescent powder and core
Piece composition light transformation approach and obtain, one of them is that yellow fluorescent powder is equipped with by blue LED die to realize, but it lacks
Red light, thus color developing is not good enough；Another kind is to be equipped with what three primary colors fluorescent powder was realized by UV LED chip, this
Although LED white light color is Well-recovered, the commercial Y that generallys use at present2O2S:Eu3+Red light emitting phosphor low efficiency, surely
It is qualitative not good enough.
In red fluorescence powder, another rear-earth-doped molybdate red phosphor has (1) good chemistry because of it
Stability, thermal stability and hydrolytic stability；(2) wide and strong charge transfer absorption band, can cooperate Eu3+F-f transition；(3)
Cost of material is cheap, and production cost is low；(4) emission spectrum of excitation spectrum and existing ultraviolet light and blue-light LED chip coincide
Very well, many advantages, such as can directly being excited by existing chip, launch pure feux rouges and the weight for increasingly causing people
Depending on.However, at present focusing mostly on the preparation method research of molybdate substrate in traditional high temperature solid-state method, followed by colloidal sol one is solidifying
Glue method, microemulsion method and hydro-thermal method, and rarely have public affairs for the research of liquid-phase precipitation method especially outfield auxiliary liquid-phase precipitation rule
Open report.
Summary of the invention
1. technical problems to be solved
It is molybdate red glimmering to overcome existing high temperature solid-state method, sol-gel method, microemulsion method and hydro-thermal method etc. to prepare
The deficiencies of complex technical process existing for light powder method, operating condition are not easy to control place, the present invention provide a kind of microwave and super
The method of the double outfield collaboration auxiliary molybdate red fluorescence of liquid phase synthesis bismuth europium codope of sound wave.
2. technical solution
In order to solve the above technical problems, the present invention provides a kind of microwave and the double outfields auxiliary liquid phase synthesis bismuth europiums of ultrasonic wave are double
The method for adulterating molybdate red phosphor comprising the steps of:
(1) with sodium molybdate (Na2MoO4), calcium nitrate (Ca (NO3)2), bismuth nitrate (Bi (NO3)3), europium nitrate (Eu (NO3)3)
Solution is raw material, with urea (CO (NH2)2) it is precipitating reagent；Stoichiometrically measure a certain amount of Ca (NO3)2、CO(NH2)2、
Bi(NO3)3、Eu(NO3)3It is mixed into feed liquid A, measures a certain concentration Na2MoO4Form feed liquid B；
(2) first uniformly mixed A feed liquid is placed in microwave and ultrasonic synergistic Liquid-phase reactor, then B feed liquid is slow
Ground is counter to be added in solution A, control ultrasonic wave/microwave cooperating mode be 1:2 or 2:1,80~95 DEG C of reaction temperature, the reaction time
1.5~2.5h obtains sediment；
(3) heat filtering, washing are carried out to sediment, obtains the presoma of subject matter；
(4) it after presoma is dry at 80~120 DEG C, is thermally decomposed at 800~1000 DEG C of Yu Wendu, heat preservation 3~
4h obtains subject matter bismuth europium codope molybdate Ca1-x-yMoO4:(Eu3+ y,Bi3+ x) fluorescent powder, wherein x=0.0~0.04, y=
0.06~0.08.
Further, the method, it is sodium molybdate, equal with calcium nitrate feed concentration in step (1), it is dense to control its
Degree is c (Na2MoO4)=c (Ca (NO3)2)=1~2molL-1；c(CO(NH2)2)=3~5molL-1。
The method, in step (1), CO (NH2)2With CaMoO4Molar ratio be 2~5.
The method, in step (2), the frequency of the ultrasonic wave is 20~25kHz.
The method, in step (2), ultrasonic wave/microwave Cooperative Mode is 1:2, i.e. microwave outfield is made
With being continuous, and ultrasonic wave outfield is then interval 2s after pulse 1s, and as the period, cycle operation is until reaction terminates.
3. working principle
(1) biradical matter calcium molybdate forerunner's body technique is adulterated using microwave and the double outfield auxiliary liquid phase synthesis europiums of ultrasonic wave, filled
Divide " synergistic effect " using ultrasonic wave " cavitation " and microwave " interior heating ", promotes feed liquid Na2MoO4·2H2O、Ca
(NO3)2·4H2O and Bi3+·6H2O、Eu3+·6H2H is crystallized or is coordinated in O2CO in the removing of O, precipitating reagent3 2-With OH-Cracking
And the generation of hydroxyl radical free radical；Make CO in system3 2-、OH-Activity increases rapidly, and then accelerates the shape of molybdate presoma nucleus
At, the rearrangement of lattice, removing, the refinement of crystal grain and the raising of crystallization degree of hydration shell and the crystallization water；It is thermally decomposed in presoma
In the process, subject matter can inherit the Monodispersed of its presoma, near-spherical feature.
(2) due to Bi3+Ion and Ca2+Ionic radius is close, in addition under microwave and the double outfield synergistic effects of ultrasonic wave,
So that Bi3+Ion, which enters, replaces part Ca in the lattice of matrix2+Ion, and do not cause substantially changeing for matrix structure, but Bi3 +Ion can transfer energy to neighbouring activator Eu3+Ion plays the role of sensitizer, so as to cause molybdate fluorescence
The luminous intensity of powder is significantly improved.
4. beneficial effect
(1) simple, the manageable liquid-phase precipitation method of operating condition of the invention using technical process, with high temperature solid-state method phase
Than, low 300 DEG C of synthesis temperature or more and it is energy saving, product pattern is more regular, particle diameter distribution is narrow and after ball milling and classification can be saved
Treatment process；Compared with sol-gel method and microemulsion method, operation of the present invention is simpler, without adding any activating agent, dividing
The coating materials such as powder and template both can get high-purity molybdate fluorescent material, while in turn avoid drawing for dressing agent
Enter and the luminescent properties of product are impacted；Compared with hydro-thermal method, reaction rate of the present invention is high, the high―temperature nuclei mistake without pressurization
Journey；
(2) the bismuth europium codope molybdate red phosphor product granularity that is prepared of the present invention is controllably between 1~4 μm
Polyhedron near-spherical, regular appearance, particle diameter distribution is narrow, and the heap density of unit volume is big and light scattering loss is small；Product
Crystallization degree is high, and fluorescence lifetime is greater than 0.398ms, and excitation spectrum, can be by the black light of 395nm and 465nm without miscellaneous peak
Blue light effectively excites, the maximum intensity of emission peak at 616nm, and is significantly higher than the molybdate fluorescent powder of single europium doping.Its
Chromaticity coordinates is (0.6598,0.3398), very close with the chromaticity coordinates (0.67,0.33) of international feux rouges, and red more glimmering than commercial
Light powder Y2O2S:Eu3+(0.622,0.351) feux rouges is purer, is suitable as the red fluorescence powder raw material of white light LEDs.
Detailed description of the invention
Fig. 1 is techniqueflow chart of the invention.
Fig. 2 is respectively molybdate fluorescence prepared by (a) of the invention and external heat liquid-phase coprecipitation (b) and high temperature solid-state method
Powder (c) scanning electron microscope picture (SEM) compares figure, shows that the pattern of product of the present invention is more regular, particle diameter distribution is narrower.
Fig. 3 is bismuth europium codope molybdate Ca prepared by the present invention1-x-yMoO4:(Eu3+ y,Bi3+ x) X-ray of fluorescent powder spreads out
(XRD) map is penetrated, shows that the substance is still the white tungsten of undoped tetragonal crystal system when bismuth ion adulterates molar ratio x < 0.2
Mine (CaWO4) structure, the Bi of doping3+、Eu3+Completely into lattice, Ca is substituted2+Coordination.Do not occur impurity peaks in figure, and
Each main diffraction peak peak type is sharp, this shows that the sample purity of preparation is high, free from admixture phase, and crystallization degree is high.When bismuth doping is big
It will appear Bi when 20% molar ratio3+WO4Impurity phase, thus doping x should be less than 0.2.
When Fig. 4 is bismuth doping x=0.01, Ca0.92MO4:(Eu3+ 0.07,Bi3+ 0.01) adulterated with single europium
Ca0.93MoO4:Eu3+ 0.07The spectrum comparison diagram of fluorescent powder shows that the excitation peak intensity of bismuth europium codope molybdate is apparently higher than list
One europium adulterates molybdate fluorescent powder.
When Fig. 5 is bismuth doping x=0.01~0.05, Ca0.93-xMO4:(Eu3+ 0.07,Bi3+ x) fluorescent powder emission spectrum
Comparison diagram shows best when bismuth doping molar fraction is 0.02~0.04.
Fig. 6 is Ca under different thermal decomposition temperatures0.9MO4:(Eu3+ 0.07,Bi3+ 0.03) fluorescent powder exciting light spectrogram, show it
Best thermal decomposition temperature is 900~1000 DEG C, 300 DEG C lower than the synthesis temperature of high temperature solid-state method or more.
Fig. 7 show Ca0.92MO4:(Eu3+ 0.07,Bi3+ 0.01) fluorescent powder in excitation wavelength is 395nm, launch wavelength is
Fluorescence lifetime attenuation curve figure under 616nm, the fluorescence lifetime for calculating its fluorescent powder is 0.398ms.
Fig. 8 show Ca0.92MO4:(Eu3+ 0.07,Bi3+ 0.01) fluorescent powder chromaticity coordinates figure.Its chromaticity coordinates can be calculated from figure
It is very close with the chromaticity coordinates (0.67,0.33) of international feux rouges for (0.6598,0.3398), and than commercial red fluorescence powder
Y2O2S:Eu3+The feux rouges of (0.622,0.351) is purer, can be used as the red fluorescence powder raw material of white light LEDs.
Specific embodiment
The present invention is further illustrated with case study on implementation with reference to the accompanying drawing.
The model XH-300A and XO-SM50 of microwave and ultrasonic wave liquid phase are used in the embodiment of the present invention, microwave is maximum
Power 1000 and 700W, can stepless time adjustment non-pulse continuous work, ultrasonic wave maximum power 1500 and 900W, frequency 25kHz.
It is involved in the present invention to product average grain diameter be combine its SEM scheme, by Image Tool software measuring and calculating
It arrives.
Embodiment 1
(1) 2molL is configured-1Sodium molybdate (Na2MoO4), bismuth nitrate (Bi (NO3)3), europium nitrate (Eu (NO3)3), calcium nitrate
(Ca(NO3)2) solution be raw material, 4molL-1Urea (CO (NH2)2) it is precipitating reagent；Stoichiometrically measure Ca (NO3)2、
Bi(NO3)3、Eu(NO3)3、CO(NH2)2Solution is each 91,3,6,200mL be mixed into feed liquid A, take Na2MoO4Solution 100mL composition material
Liquid B；
(2) first uniformly mixed solution A is placed in microwave and ultrasonic synergistic Liquid-phase reactor, then B solution is slow
Ground is counter to be added in solution A, and control ultrasonic wave/microwave cooperating mode is 1:2, ultrasonic power 700W, microwave power 500W, reaction
90 DEG C of temperature, reaction time 2h obtains sediment；
(3) heat filtering, washing are carried out to sediment, obtains the presoma of subject matter；
(4) presoma after dry 4h, is thermally decomposed at 1000 DEG C of Yu Wendu at 100 DEG C, keeps the temperature 3.5h, obtains bismuth
Europium codope molybdate Ca0.91MO4:(Eu3+ 0.06,Bi3+ 0.03) fluorescent powder.
The fluorescent powder being prepared SEM figure as Fig. 2 (on) shown in, average grain diameter is about 2 μm, luminescent properties as scheme
It shown in 3~8, can effectively be excited by the blue light of the black light of 395nm and 465nm, the intensity of emission peak is most at 616nm
Greatly, and it is apparently higher than single europium doping calcium molybdate fluorescent powder.Pass through fluorescence lifetime decay formula: I=I0e-t/τCalculate its fluorescence longevity
Order (wherein I0And ItThe luminous intensity of zero moment and t moment sample is respectively indicated, τ represents Decay), obtain its fluorescence lifetime
For 0.398ms, chromaticity coordinates is located in red light region, and calculating its chromaticity coordinates using CIE software is X=0.6598, Y=
0.3398, it is very close with the chromaticity coordinates (0.67,0.33) of international feux rouges, and than commercial red fluorescence powder Y2O2S:Eu3+
(0.622,0.351) feux rouges is purer, suitable for the red fluorescence powder raw material as white light LEDs.
Embodiment 2
(1) 1molL is configured-1Sodium molybdate (Na2MoO4), bismuth nitrate (Bi (NO3)3), europium nitrate (Eu (NO3)3), calcium nitrate
(Ca(NO3)2) solution be raw material, 3molL-1Urea (CO (NH2)2) it is precipitating reagent；Stoichiometrically measure Ca (NO3)2、
Bi(NO3)3、Eu(NO3)3、CO(NH2)2Solution is each 90,3,7,200mL be mixed into feed liquid A, take Na2MoO4Solution 100mL composition material
Liquid B；
(2) first uniformly mixed solution A is placed in microwave and ultrasonic synergistic Liquid-phase reactor, then B solution is slow
Ground is counter to be added in solution A, and control ultrasonic wave/microwave cooperating mode is 1:2, ultrasonic power 700W, microwave power 500W, reaction
90 DEG C of temperature, reaction time 2h obtains sediment；
(3) heat filtering, washing are carried out to sediment, obtains the presoma of subject matter；
(4) presoma after dry 4h, is thermally decomposed at 900 DEG C of Yu Wendu at 80 DEG C, keeps the temperature 4h, it is double to obtain bismuth europium
Adulterate molybdate Ca0.9MoO4:(Eu3+ 0.07,Bi3+ 0.03) fluorescent powder.
The fluorescent powder average grain diameter being prepared is about 2.5 μm, and luminescent properties and embodiment 1 are substantially similar, but such as Fig. 6
It is shown, show that sensitizer bismuth ion adds molar ratio x=0.03, i.e., 3% or so when is best, luminous strength ratio embodiment 1
In 1% it is stronger, be particularly suited for the red fluorescence powder raw material as white light LEDs.
In conclusion the present invention assists liquid using the microwave and ultrasonic wave outfield that technical process is simple, operating condition is controllable
Polyhedron of the bismuth europium codope molybdate red phosphor product granularity that the method for co-precipitation is prepared between 2~4 μm
Near-spherical, regular appearance, particle diameter distribution is narrow, and the heap density of unit volume is big and light scattering loss is small；Product crystallization degree
Height, fluorescence lifetime are greater than 0.398ms, and fluorescent powder is in feux rouges under the excitation of 395~465nm wavelength, and excitation spectrum shines without miscellaneous peak
Intensity is significantly higher than single europium doping molybdate fluorescent powder, can effectively be excited by ultraviolet light and blue light, than commercial Y2O2S:
Eu3+Feux rouges is purer, can meet the requirement for making White LED red fluorescence powder raw material.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
It, for those skilled in the art, still can be with although describing the invention in detail with reference to the foregoing embodiments
It modifies the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features.It is all
Under the premise of design of the invention, made any modification, improvement etc. be should all be included in the protection scope of the present invention.
Claims (5)
1. the method for microwave and the double outfield auxiliary liquid phase synthesis bismuth europium codope molybdate red phosphors of ultrasonic wave, feature exist
In by following steps:
(1) with sodium molybdate (Na2MoO4), calcium nitrate (Ca (NO3)2), bismuth nitrate (Bi (NO3)3), europium nitrate (Eu (NO3)3) solution
For raw material, with urea (CO (NH2)2) it is precipitating reagent；Stoichiometrically measure a certain amount of Ca (NO3)2、CO(NH2)2、Bi
(NO3)3、Eu(NO3)3It is mixed into feed liquid A, measures a certain amount of Na2MoO4Solution composition feed liquid B；
(2) first uniformly mixed A feed liquid is placed in microwave and ultrasonic synergistic Liquid-phase reactor, then B feed liquid is slowly anti-
Be added solution A in, control ultrasonic wave/microwave cooperating mode be 1:2 or 2:1,80~95 DEG C of reaction temperature, the reaction time 1.5~
2.5h obtains sediment；
(3) heat filtering, washing are carried out to sediment, obtains the presoma of subject matter；
(4) it after presoma is dry at 80~120 DEG C, is thermally decomposed at 800~1000 DEG C of Yu Wendu, keeps the temperature 3~4h, obtain
To subject matter bismuth europium codope molybdate Ca1-x-yMoO4:(Eu3+ y,Bi3+ x) fluorescent powder, wherein x=0.0~0.04, y=0.06
~0.08.
2. according to claim 1, the method, it is characterised in that: sodium molybdate, dense with calcium nitrate feed liquid in step (1)
Spend it is equal, control its concentration be c (Na2MoO4)=c (Ca (NO3)2)=1~2molL-1；c(CO(NH2)2)=3~5mol
L-1。
3. according to claim 1, the method, it is characterised in that: in step (1), CO (NH2)2With CaMoO4Mole
Than being 2~5.
4. according to claim 1, the method, it is characterised in that: in step (2), the frequency of the ultrasonic wave is
20~25kHz.
5. method according to claim 1, it is characterised in that: in step (2), ultrasonic wave/microwave association
It is 1:2 with mode, i.e., microwave outer field action is continuous, and ultrasonic wave outfield is then interval 2s after pulse 1s, as the period,
Cycle operation is until reaction terminates.
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Cited By (3)
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| CN110437834A (en) * | 2019-10-10 | 2019-11-12 | 佛山市钜亮光学材料有限公司 | A kind of method of the preparation method of the high fluorescent powder of thermal stability and production Ceramic Tiles |
| CN113909485A (en) * | 2021-10-11 | 2022-01-11 | 先导薄膜材料（广东）有限公司 | Preparation method of superfine cobalt powder |
| CN116120933A (en) * | 2022-11-25 | 2023-05-16 | 南京信息工程大学 | Rare earth doped yttrium molybdate fluorescent powder with hollow core-shell structure and preparation method thereof |
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| CN103113889A (en) * | 2013-03-12 | 2013-05-22 | 关荣锋 | Molybdate red phosphor and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110437834A (en) * | 2019-10-10 | 2019-11-12 | 佛山市钜亮光学材料有限公司 | A kind of method of the preparation method of the high fluorescent powder of thermal stability and production Ceramic Tiles |
| CN113909485A (en) * | 2021-10-11 | 2022-01-11 | 先导薄膜材料（广东）有限公司 | Preparation method of superfine cobalt powder |
| CN113909485B (en) * | 2021-10-11 | 2023-11-17 | 先导薄膜材料（广东）有限公司 | Preparation method of superfine cobalt powder |
| CN116120933A (en) * | 2022-11-25 | 2023-05-16 | 南京信息工程大学 | Rare earth doped yttrium molybdate fluorescent powder with hollow core-shell structure and preparation method thereof |
| CN116120933B (en) * | 2022-11-25 | 2024-02-23 | 南京信息工程大学 | Rare earth doped yttrium molybdate fluorescent powder with hollow core-shell structure and preparation method thereof |
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Application publication date: 20190322 |
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