CN106350068A - Cerium-europium-terbium codoped nanocrystal fluorescent powder and preparation method thereof - Google Patents
Cerium-europium-terbium codoped nanocrystal fluorescent powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses cerium-europium-terbium codoped nanocrystal fluorescent powder which has a chemical general formula of CexEunTb1-x-nF3 (x+n is greater than 0 and less than or equal to 1), wherein x represents a molar concentration of Ce3+, and n represents a molar concentration of Eu3+. A preparation method of the powder comprises the following steps: (1) weighing Ce(NO3)3.6H2O, Eu(NO3)3.6H2O and Tb(NO3)3.6H2O, adding [Bmim]NO3, stirring for 30-45min at 55-65 DEG C to prepare mixed liquid, (2) adding the mixed liquid into [Bmim]PF6, performing ultrasonic dispersion for 1-3h at 10-30Hz, and (3) cooling ultrasonic dispersion liquid to the room temperature, sucking liquid on a lower layer after liquid layering, washing with acetone, and then performing centrifugation and drying. The preparation method is simple, low in energy consumption and low in corrosion, and the prepared nanocrystal fluorescent powder has a good luminescent property.
Description
Technical field
The present invention relates to rare earth luminescent material technical field and in particular to a kind of cerium europium terbium co-doped nano crystalline substance fluorescent material and
Its preparation method.
Background technology
The own method through developing multiple synthetic rare earth doped nano-particle at present, including high temperature solid-state method, hydro-thermal/hot melt
Agent method, sol-gal process, microwave method, supercritical ultrasonics technology etc..Solid reaction process synthesizing rare-earth luminescent material, is to apply earliest and
Many traditional methods, are also the currently the only method realizing industrialized production, and its main process is to be up to the former of purity requirement
Material weigh according to a certain percentage, add a certain amount of flux be sufficiently mixed after grind even, then certain temperature atmosphere when
Between under the conditions of carry out calcination.Although high temperature solid-state method is through people's years of researches, technics comparing is ripe, the method itself
There is intrinsic defect: calcination temperature is high, and majority will be more than 1300 DEG C；Response time is long, is typically necessary 6 8h；
Production die is big, and density is high, and hardness is big.But it is dusty material it is therefore necessary to by high temperature solid-state due to what reagent application needed
Product is through ball-milling technology process, and grinds the crystal structure being easy to destroy luminescent material, thus leading to luminescent properties significantly
Degree declines.
The product that existing majority fluorescent RE powder manufacturing enterprise produces is still single rare earth inorganic powder materials, and technique sets
For seriously falling behind, product function is single, and purity is relatively low, of low quality, the production method also high temperature solid-state adopting energy consumption higher more
Method, and prepare rare-earth fluorescent solid material by means of the effect of toxic and volatile organic solvent or highly corrosive soda acid, this just makes
Become in production process to the waste of the energy and the destruction of environment, reduced production security, virtually also increase and produce into
This.
Minority fluorescent RE powder is rear-earth-doped to be obtained, when cerium and europium are doped, but micro gently dilute for two or three
The presence of native cerium can have a strong impact on the luminescent properties containing europium Hydrargyri Oxydum Rubrum, therefore cerium europium be co-doped with fluorescent material often poor performance it is impossible to reach
To using standard.
Content of the invention
For above-mentioned deficiency of the prior art, the present invention provides a kind of cerium europium terbium co-doped nano crystalline substance fluorescent material and its system
Preparation Method, can effectively solving preparation time long, power consumption is high, and the presence of highly corrosive and cerium can affect the photism containing europium Hydrargyri Oxydum Rubrum
The problem of energy.
For achieving the above object, the technical solution adopted for the present invention to solve the technical problems is:
A kind of cerium europium terbium co-doped nano crystalline substance fluorescent material, its chemical general formula is cexeuntb1-x-nf3(0 ＜ x+n≤1)；Wherein
X represents rare earth ion ce3+Molar concentration；N represents rare earth ion eu3+Molar concentration.
Further, a kind of cerium europium terbium co-doped nano crystalline substance fluorescent material, its chemical formula is ce0.3eu0.5tb0.2f3.
Further, a kind of cerium europium terbium co-doped nano crystalline substance fluorescent material, its chemical formula is ce0.3eu0.2tb0.5f3.
The preparation method of above-mentioned cerium europium terbium co-doped nano crystalline substance fluorescent material, comprises the following steps:
(1) weigh rare earths material ce (no respectively3)3·6h2o、eu(no3)3·6h2O and tb (no3)3·6h2O, mixing, plus
Enter ionic liquid [bmim] no3, stir 30-45min in 55-65 DEG C, obtain mixed liquor；Wherein each rare earths material and ionic liquid
[bmim]no3Mol ratio is 1:1-3；
(2) step (1) gained mixed liquor microsyringe is expelled to ionic liquid [bmim] pf6In, in 95-105
DEG C, ultrasonic disperse 1-3h under the conditions of 10-30hz；Wherein ionic liquid [bmim] pf6Mol ratio and each rare earths material between is equal
For 1-3:1；
(3) step (2) gained ultrasonic disperse liquid is cooled to room temperature, after liquid layered, draws lower floor's liquid, washed with acetone
Wash, then centrifugation under 8000-10000r/min rotating speed, obtain white solid, be finally placed in 90-100 DEG C of vacuum drying 2-
3h, obtains cerium europium terbium co-doped nano crystalline substance fluorescent material, reclaims supernatant liquid, available water extracts excessive from supernatant liquid simultaneously
Ionic liquid [bmim] no3Rare earth nitrate with residual.
Further, each rare earths material and ionic liquid [bmim] no in step (1)3Mol ratio is 1:3.
Further, in step (1), whipping temp is 60 DEG C, and mixing time is 30min.
Further, step (2) intermediate ion liquid [bmim] pf6Mol ratio and each rare earths material between is 1:1.
Further, in step (2), mixed liquor injection flow velocity is 1-5 μ l/s.
Further, in step (3), centrifugal rotational speed is 8000r/min.
Further, in step (3), vacuum drying temperature is 90 DEG C, and drying time is 2h.
Cerium europium terbium co-doped nano crystalline substance fluorescent material that the present invention provides and preparation method thereof, has the advantages that
(1) the ultrasonic wave added synthetic method with ionic liquid as substrate for the present invention, in conjunction with auto injection equipment and ionic liquid
The research and development of recovery process, overcome the high energy consumption of high temperature solid-state method and the shortcoming of agglutinating nature yeast preparation time length, realize mental retardation
Consumption, high yield, high-quality rare-earth nano-crystal material is prepared in environmental protection.
(2) present invention adopts good stability, and nonvolatile ionic liquid can achieve recovery and the circulation of solvent as solvent
Use, compared with the volatile organic solvent that traditional handicraft is used, there is lower toxicity, have with respect to strong acid and strong base lower
Corrosivity, can reduce reaction solution to the corrosion of instrument and loss.
(3) present invention utilizes ionic liquid [bmim] no3As to cerous coordination protective capability, and using ultrasonic auxiliary
Help the low temperature preparation technique of synthesis, the oxidation of trivalent cerium ion can be effectively prevented from, thus avoiding quadrivalent cerium sudden to the fluorescence of europium
The effect of going out, improves the luminous intensity of prepared fluorescent RE powder.
(4) the cerium europium terbium co-doped nano crystalline substance fluorescent material of present invention preparation has uniform particle sizes, and specific surface is big, and light efficiency is high,
Heat stability is good, the adjustable advantage of spectrum.
Brief description
Fig. 1 is the preparation method flow chart of cerium europium terbium co-doped nano crystalline substance fluorescent material of the present invention.
Fig. 2 is the projection transmission electron microscope picture of the cerium europium terbium co-doped nano crystalline substance fluorescent material of embodiment 3 gained.
Fig. 3 is the grain size distribution of the cerium europium terbium co-doped nano crystalline substance fluorescent material of embodiment 3 gained.
Fig. 4 is the ce of embodiment 1 gained0.2eu0.8f3The launching light spectrogram of nano-crystal fluorescent powder.
Fig. 5 is the launching light spectrogram of the cerium europium terbium co-doped nano crystalline substance fluorescent material of embodiment 2 gained.
Fig. 6 is the launching light spectrogram of the cerium europium terbium co-doped nano crystalline substance fluorescent material of embodiment 3 gained.
Fig. 7 is the ce of embodiment 4 gained0.7tb0.3f3The launching light spectrogram of nano-crystal fluorescent powder.
Fig. 8 is the chromaticity coordinates schematic diagram of the rare earth co-doped nano crystalline substance fluorescent material of embodiment 1-4 gained.
Specific embodiment
The preparation method of cerium europium terbium co-doped nano crystalline substance fluorescent material, its flow chart is shown in Fig. 1.
Embodiment 1
A kind of cerium europium terbium co-doped nano crystalline substance fluorescent material, its chemical formula is ce0.2eu0.8f3.
The preparation method of above-mentioned cerium europium terbium co-doped nano crystalline substance fluorescent material, comprises the following steps:
(1) press ce3+And eu3+Mol ratio be 0.2:0.8, weigh rare earths material ce (no respectively3)3·6h2O and eu
(no3)3·6h2O, mixing, add ionic liquid [bmim] no3, stir 30min in 60 DEG C, obtain mixed liquor；Wherein each rare earth is former
Material and ionic liquid [bmim] no3Mol ratio is 1:3；
(2) step (1) gained mixed liquor microsyringe is expelled to ionic liquid [bmim] pf6In, 100 DEG C,
Ultrasonic disperse 1h under the conditions of 20hz；Wherein mixed liquor injection flow velocity is 4 μ l/s；Wherein ionic liquid [bmim] pf6With each rare earth
Mol ratio between raw material is 1:1；
(3) step (2) gained ultrasonic disperse liquid is cooled to room temperature, after liquid layered, draws lower floor's liquid, washed with acetone
Wash, then centrifugation 10min under 8500r/min rotating speed, obtains white solid, be finally placed in 90 DEG C of vacuum drying 2h, obtain cerium
Europium terbium co-doped nano crystalline substance fluorescent material, reclaims supernatant liquid simultaneously, and supernatant liquid is ionic liquid [bmim] no3Dilute with remain
Potassium nitrate hydrochlorate, available water extracts excessive ionic liquid [bmim] no from supernatant liquid3With residual rare earth nitrate, right
It is circulated utilization.
The cerium europium terbium co-doped nano crystalline substance fluorescent material that said method is obtained, launches main peak under the ultraviolet excitation of 250nm
HONGGUANG for 612nm, as shown in figure 8, its chromaticity coordinate (x, y)=(0.5929,0.3872).
Embodiment 2
A kind of cerium europium terbium co-doped nano crystalline substance fluorescent material, its chemical formula is ce0.3eu0.5tb0.2f3.
The preparation method of above-mentioned cerium europium terbium co-doped nano crystalline substance fluorescent material, comprises the following steps:
(1) press ce3+、eu3+And tb3+Mol ratio be 0.3:0.5:0.2, weigh rare earths material ce (no respectively3)3·
6h2o、eu(no3)3·6h2O and tb (no3)3·6h2O, mixing, add ionic liquid [bmim] no3, stir 30min in 60 DEG C,
Obtain mixed liquor；Wherein each rare earths material and ionic liquid [bmim] no3Mol ratio is 1:3；
(2) step (1) gained mixed liquor microsyringe is expelled to ionic liquid [bmim] pf6In, 100 DEG C,
Ultrasonic disperse 1h under the conditions of 20hz；Wherein mixed liquor injection flow velocity is 4 μ l/s；Wherein ionic liquid [bmim] pf6With each rare earth
Mol ratio between raw material is 1:1.
(3) step (2) gained ultrasonic disperse liquid is cooled to room temperature, after liquid layered, draws lower floor's liquid, washed with acetone
Wash, then centrifugation 10min under 8500r/min rotating speed, obtains white solid, be finally placed in 90 DEG C of vacuum drying 2h, obtain cerium
Europium terbium co-doped nano crystalline substance fluorescent material, reclaims supernatant liquid simultaneously, and supernatant liquid is ionic liquid [bmim] no3Dilute with remain
Potassium nitrate hydrochlorate, available water extracts excessive ionic liquid [bmim] no from supernatant liquid3With residual rare earth nitrate, right
It is circulated utilization.
As shown in figure 5, the cerium europium terbium co-doped nano crystalline substance fluorescent material that said method is obtained, in the ultraviolet excitation of 250nm
Lower transmitting main peak is the orange light of 612nm, as shown in figure 8, its chromaticity coordinate (x, y)=(0.4961,0.4421).
Embodiment 3
A kind of cerium europium terbium co-doped nano crystalline substance fluorescent material, its chemical formula is ce0.3eu0.2tb0.5f3.
The preparation method of above-mentioned cerium europium terbium co-doped nano crystalline substance fluorescent material, comprises the following steps:
(1) press ce3+、eu3+And tb3+Mol ratio be 0.3:0.2:0.5, weigh rare earths material ce (no respectively3)3·
6h2o、eu(no3)3·6h2O and tb (no3)3·6h2O, mixing, add ionic liquid [bmim] no3, stir 30min in 60 DEG C,
Obtain mixed liquor；Wherein each rare earths material and ionic liquid [bmim] no3Mol ratio is 1:3；
(2) step (1) gained mixed liquor microsyringe is expelled to ionic liquid [bmim] pf6In, 100 DEG C,
Ultrasonic disperse 1h under the conditions of 20hz；Wherein mixed liquor injection flow velocity is 4 μ l/s；Wherein ionic liquid [bmim] pf6With each rare earth
Mol ratio between raw material is 1:1；
(3) step (2) gained ultrasonic disperse liquid is cooled to room temperature, after liquid layered, draws lower floor's liquid, washed with acetone
Wash, then centrifugation 10min under 8500r/min rotating speed, obtains white solid, be finally placed in 90 DEG C of vacuum drying 2h, obtain cerium
Europium terbium co-doped nano crystalline substance fluorescent material, reclaims supernatant liquid simultaneously, and supernatant liquid is ionic liquid [bmim] no3Dilute with remain
Potassium nitrate hydrochlorate, available water extracts excessive ionic liquid [bmim] no from supernatant liquid3With residual rare earth nitrate, right
It is circulated utilization.
The projection transmission electron microscope picture of cerium europium terbium co-doped nano crystalline substance fluorescent material that said method is obtained and grain size distribution divide
Do not see Fig. 2 and Fig. 3.
From Fig. 2 and Fig. 3, cerium europium terbium co-doped nano crystalline substance fluorescent material size and form is more uniform, and size is many points
Cloth is in 10-20nm.
As shown in fig. 6, the cerium europium terbium co-doped nano crystalline substance fluorescent material that said method is obtained, in the ultraviolet excitation of 250nm
Lower transmitting main peak is the gold-tinted of 543nm, as shown in figure 8, its chromaticity coordinate (x, y)=(0.3704,0.5390).
Embodiment 4
A kind of cerium europium terbium co-doped nano crystalline substance fluorescent material, its chemical formula is ce0.7tb0.3f3.
The preparation method of above-mentioned cerium europium terbium co-doped nano crystalline substance fluorescent material, comprises the following steps:
(1) press ce3+And tb3+Mol ratio be 0.7:0.3, weigh rare earths material ce (no respectively3)3·6h2O and tb
(no3)3·6h2O, mixing, add ionic liquid [bmim] no3, stir 30min in 60 DEG C, obtain mixed liquor；Wherein each rare earth is former
Material and ionic liquid [bmim] no3Mol ratio is 1:3；
(2) step (1) gained mixed liquor microsyringe is expelled to ionic liquid [bmim] pf6In, 100 DEG C,
Ultrasonic disperse 1h under the conditions of 20hz；Wherein mixed liquor injection flow velocity is 4 μ l/s；Wherein ionic liquid [bmim] pf6With each rare earth
Mol ratio between raw material is 1:1；
(3) step (2) gained ultrasonic disperse liquid is cooled to room temperature, after liquid layered, draws lower floor's liquid, washed with acetone
Wash, then centrifugation 10min under 8500r/min rotating speed, obtains white solid, be finally placed in 90 DEG C of vacuum drying 2h, obtain cerium
Europium terbium co-doped nano crystalline substance fluorescent material, reclaims supernatant liquid simultaneously, and supernatant liquid is ionic liquid [bmim] no3Dilute with remain
Potassium nitrate hydrochlorate, available water extracts excessive ionic liquid [bmim] no from supernatant liquid3With residual rare earth nitrate, right
It is circulated utilization.
As shown in fig. 7, the cerium europium terbium co-doped nano crystalline substance fluorescent material that said method is obtained, in the ultraviolet excitation of 250nm
Lower transmitting main peak is the green glow of 543nm, as shown in figure 8, its chromaticity coordinate (x, y)=(0.2664,0.6405).
Embodiment 2 and 3 prepares rare-earth nano-crystal fluorescent material using the codope of cerium europium terbium, by allocating rare-earth europium and terbium
Energy transfer process between doping ratio and cerium terbium europium (ce → tb → eu), can realize rare-earth europium in same material
Red fluorescence and the mixing of rare earth terbium green fluorescence, realize the fine setting of fluorescence colourity, more individually contain europium (embodiment 1) and individually
Nano-crystal fluorescent powder containing terbium (embodiment 4), its colour gamut is wider, has the adjustable advantage of colourity.
Claims (10)
1. a kind of cerium europium terbium co-doped nano crystalline substance fluorescent material is it is characterised in that chemical general formula is cexeuntb1-x-nf3(0 ＜ x+n≤
1)；Wherein x represents ce3+Molar concentration；N represents eu3+Molar concentration.
2. cerium europium terbium co-doped nano crystalline substance fluorescent material according to claim 1 is it is characterised in that chemical formula is
ce0.3eu0.5tb0.2f3.
3. cerium europium terbium co-doped nano crystalline substance fluorescent material according to claim 1 is it is characterised in that chemical formula is
ce0.3eu0.2tb0.5f3.
4. as described in any one of claim 1-3 cerium europium terbium co-doped nano crystalline substance fluorescent material preparation method it is characterised in that
Comprise the following steps:
(1) weigh rare earths material ce (no respectively3)3·6h2o、eu(no3)3·6h2O and tb (no3)3·6h2O, mixing, add
[bmim]no3, stir 30-45min in 55-65 DEG C, obtain mixed liquor；Wherein each rare earths material and [bmim] no3Mol ratio is 1:
1-3；
(2) step (1) gained mixed liquor microsyringe is expelled to [bmim] pf6In, in 95-105 DEG C, 10-30hz condition
Lower ultrasonic disperse 1-3h；Wherein [bmim] pf6Mol ratio and each rare earths material between is 1-3:1；
(3) step (2) gained ultrasonic disperse liquid is cooled to room temperature, after liquid layered, draws lower floor liquid, with washing with acetone,
Then centrifugation under 8000-10000r/min rotating speed, obtains white solid, is finally placed in 90-100 DEG C of vacuum drying 2-3h,
Obtain cerium europium terbium co-doped nano crystalline substance fluorescent material.
5. the preparation method of cerium europium terbium co-doped nano according to claim 4 crystalline substance fluorescent material is it is characterised in that step
(1) each rare earths material and [bmim] no in3Mol ratio is 1:3.
6. the preparation method of cerium europium terbium co-doped nano according to claim 4 crystalline substance fluorescent material is it is characterised in that step
(1) in, whipping temp is 60 DEG C, and mixing time is 30min.
7. the preparation method of cerium europium terbium co-doped nano according to claim 4 crystalline substance fluorescent material is it is characterised in that step
(2) [bmim] pf in6Mol ratio and each rare earths material between is 1:1.
8. the preparation method of cerium europium terbium co-doped nano according to claim 4 crystalline substance fluorescent material is it is characterised in that step
(2) in, mixed liquor injection flow velocity is 1-5 μ l/s.
9. the preparation method of cerium europium terbium co-doped nano according to claim 4 crystalline substance fluorescent material is it is characterised in that step
(3) in, centrifugal rotational speed is 8000r/min.
10. the preparation method of cerium europium terbium co-doped nano according to claim 4 crystalline substance fluorescent material is it is characterised in that step
(3) in, vacuum drying temperature is 90 DEG C, and drying time is 2h.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007082663A1 (en) * | 2006-01-11 | 2007-07-26 | Universität Karlsruhe | Process for the synthesis of nanocrystalline phosphor particles and nanocrystalline phosphor particles obtainable by this process |
| CN101157473A (en) * | 2007-09-20 | 2008-04-09 | 东华大学 | Preparation method of rare-earth doping fluoride nano luminescent particles |
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- 2016-08-30 CN CN201610769093.3A patent/CN106350068B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007082663A1 (en) * | 2006-01-11 | 2007-07-26 | Universität Karlsruhe | Process for the synthesis of nanocrystalline phosphor particles and nanocrystalline phosphor particles obtainable by this process |
| CN101157473A (en) * | 2007-09-20 | 2008-04-09 | 东华大学 | Preparation method of rare-earth doping fluoride nano luminescent particles |
Non-Patent Citations (1)
| Title |
|---|
| FARHEEN N. SAYED,等: "Solid state white light emitting systems based on CeF3: RE3+ nanoparticles and their composites with polymers", 《JOURNAL OF COLLOID AND INTERFACE SCIENCE》 * |
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