CN108456525A - A kind of preparation method of europium doping yttrium fluoride nano-particle fluorescence body - Google Patents
A kind of preparation method of europium doping yttrium fluoride nano-particle fluorescence body Download PDFInfo
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Abstract
A kind of Y1‑xF3:xEu3+The preparation method of nano-particle fluorescence body, it is with Y (NO3)3.6H2O、Eu2O3, surfactant, 1 butyl, 3 methyl imidazolium tetrafluoroborate be raw material, respectively by closed stirring, hydro-thermal reaction, centrifugation, washing, drying and etc. be made, the X value ranges be 0.01 ~ 0.2.The present invention may make Eu to be successfully doped in matrix, the product of each difference doping is near ultraviolet excitated, sends out fluorescent red-orange, it is good to all have higher luminous intensity, the uniformity that shines, it is evenly distributed, product purity obtained is high, no dissolved oxygen impurity, product cut size is smaller and uniform, the coating good photochromic difference of effect is small, and gas sensing property is good, especially has stronger gas sensing property to imflammable gas；Preparation method yield of the present invention is high, and yield may be up to 99.1% or more, and preparation method is simple, and production cost is low, and preparation process not will produce HF, to human and environment close friend, easily realizes and produces in enormous quantities, be worth marketing application.
Description
Technical field
The present invention relates to a kind of Y1-xF3:xEu3+The preparation method of nano-particle fluorescence body.
Background technology
Rare earth fluoride nano material has broad-band gap, low phonon vibration energy, high heat and environmental stability,
As the good host material in luminescent material, there is potential application prospect in optical field.Traditional organic fluorescence dye
Material photochemical stability is poor, absorb and transmitting band is wider, photobleaching and photodissociation are serious, photolytic product often has killing to organism
Effect, this greatly limits its application ranges.And the semiconductor fluorescence studied extensively in recent years is nanocrystalline due to chemical steady
Qualitative poor, bio-toxicity is difficult to avoid that, application nevertheless suffers from some limitations.In comparison, rare earth nano material has only
The physical properties such as special light, electricity, magnetic, and bio-toxicity is small, thus have broad application prospects in bio-imaging technology.
Rare earth fluoride nano material extends to middle infrared waves with son energy characteristic, light emitting region in a low voice near ultraviolet
Section, the matrix particularly suitable as laser crystal, up-conversion luminescent material.Product can be applied to display screen, energy-saving lamp, biology mark
The fields such as note, laser crystal and scintillation crystal.Y1-xF3:xEu3+Nanocrystal is in high-resolution display, electroluminescent device, light
The fields such as amplifier and fluorescence probe have potential application, and are expected in Flied emission, nanotube electric installation, display
The fields such as part, high temperature lubricating and friction, biomarker play an important role, and open up the frontier of material application.
Currently, the synthetic method of rare earth fluoride nano material mainly has synthesis in water, oil phase synthesis and synthesis in solid state etc..
Wherein, synthesis in water is most simple, to the of less demanding of instrument and equipment, still, it is generally the case that the nano-particle of synthesis in water is
Hydrophobic, the fluorescence intensity of particle solution is very weak, is not used to bioanalysis.
At present apparently, HF etc. is toxic to be had because it will produce there are preparation process for the preparation method of rare earth fluoride nano material
Evil substance, it is unfavorable to human and environment, while there is also complicated for operation, production cost is high, finished product is easier to doping dissolved oxygen impurity, purity
Low, grain size is larger, and particle size uniformity is poor, poor using process coating effect, and luminous intensity is strong, luminance nonuniformity one, photochromic difference
Etc. technical problems restrict the development in nano-particle fluorescence body field.
Invention content
Present invention aims at provide a kind of Y1-xF3:xEu3+The preparation method of nano-particle fluorescence body.
The object of the invention is achieved through the following technical solutions：
A kind of Y1-xF3:xEu3+The preparation method of nano-particle fluorescence body, which is characterized in that it is with Y (NO3)3.6H2O、
Eu2O3, surfactant, 1- butyl -3- methyl imidazolium tetrafluoroborates be raw material, respectively by closed stirring, hydro-thermal reaction,
Centrifugation, washing, drying and etc. be made, the X value ranges be 0.01~0.2.
Further, a kind of Y1-xF3:xEu3+The preparation method of nano-particle fluorescence body, which is characterized in that the surface-active
Agent is one kind in disodium EDTA or neopelex.
Further, a kind of Y1-xF3:xEu3+The preparation method of nano-particle fluorescence body, which is characterized in that the surface-active
Agent is preferably neopelex.
Further, a kind of Y1-xF3:xEu3+The preparation method of nano-particle fluorescence body, which is characterized in that the dodecyl
Benzene sulfonic acid sodium salt addition need to meet Eu in solution3+With Y3+The sum of with the molar ratio of neopelex be 1:2.
Specifically, a kind of Y1-xF3:xEu3+The preparation method of nano-particle fluorescence body, which is characterized in that it is under including
Carry out step to be made：
1. taking Y (NO3)3.6H2O is dissolved in appropriate vessel, and the Y (NO that deionized water is configured to 0.25mol/L are added3)3
Solution, it is spare；
2. taking Eu2O3It is first dissolved with dust technology, obtains Eu (NO3)3, be subsequently placed in water-bath in water-bath evaporate it is extra
Nitric acid adds the Eu (NO that deionized water is configured to 0.25mol/L3)3；A concentration of 1.5mol/L of the dust technology, it is described
Eu2O3Mass volume ratio with dust technology is 1:12；The bath temperature is 50~60 DEG C, and water bath time is 1~2h；
3. by Y (NO obtained in step 13)3Solution and Eu (NO3)3Solution is placed in appropriate vessel, and dodecyl is added
Benzene sulfonic acid sodium salt is subsequently placed in 30~40min of stirring in magnetic stirring apparatus, 1- butyl -3- methylimidazole tetrafluoro boric acids is then added
Salt, it is closed to continue 1~2h of stirring, mixed liquor is obtained, it is spare；Y (the NO3)3Solution, Eu (NO3)3Solution and 1- butyl -3- first
The molar ratio of base tetrafluoroborate is 0.99~0.80:0.1~0.2:1~3；
4. mixed liquor obtained in step 3 is placed in the reaction kettle of polytetrafluoroethylene (PTFE), it is subsequently placed in baking oven, setting temperature
180~190 DEG C of degree, keep 22~for 24 hours, it takes out, placement is cooled to 20~25 DEG C, spare；
5. taking mixed liquor after cooling in step 4, it is placed in a centrifuge and is centrifuged 4~6 minutes in 6000~8000r/min,
Liquid is discarded supernatant, centrifugation is collected, the absolute ethyl alcohol washing that 10 times of quality of precipitation are then added precipitates 3 times, has washed every time
Cheng Houyong centrifuges centrifuge 4~6 minutes in 6000~8000r/min of rotating speed, collect and precipitate to get crude product, spare；
6. crude product is placed in baking oven, dry, takes out to get Y1-xF3:xEu3+；78~82 DEG C of the drying temperature, drying
Time is 6~10 hours.
The present invention has following advantageous effect：
A kind of Y of the present invention1-xF3:xEu3+The preparation method of nano-particle fluorescence body may make Eu to be successfully doped in matrix,
It is each difference doping product be near ultraviolet excitated, send out fluorescent red-orange, all have higher luminous intensity, shine it is uniform
It spends, is evenly distributed, product purity obtained is high, and no dissolved oxygen impurity, product cut size is smaller and uniform, and coating effect is good, photochromic
Difference is small, and gas sensing property is good, especially has stronger gas sensing property to imflammable gas；Preparation method yield of the present invention is high, and yield can be high
Up to 99.1% or more, preparation method is simple, and production cost is low, and preparation process not will produce HF, to human and environment friend
It is good, it easily realizes and produces in enormous quantities, be worth marketing application.
Description of the drawings
Fig. 1 is the present inventionNano-particle fluorescence body X-ray diffractogram.
Fig. 2 is the present inventionNano-particle fluorescence body SEM figures.
Fig. 3 is the present inventionThe transmitting figure of nano-particle fluorescence body
Fig. 4 is the present inventionThe excitation figure of nano-particle fluorescence body
Fig. 5 is the present inventionNano-particle fluorescence body X-ray diffractogram.
Fig. 6 is the present inventionNano-particle fluorescence body SEM figures.
Fig. 7 is the present inventionThe transmitting figure of nano-particle fluorescence body
Fig. 8 is the present inventionThe excitation figure of nano-particle fluorescence body
Fig. 9 is the present inventionNano-particle fluorescence body X-ray diffractogram.
Figure 10 is the present inventionNano-particle fluorescence body SEM figures.
Figure 11 is the present inventionThe transmitting figure of nano-particle fluorescence body
Figure 12 is the present inventionThe excitation figure of nano-particle fluorescence body
Figure 13 is the present inventionNano-particle fluorescence body X-ray diffractogram.
Figure 14 is the present inventionNano-particle fluorescence body SEM figures.
Figure 15 is the present inventionThe transmitting figure of nano-particle fluorescence body
Figure 16 is the present inventionThe excitation figure of nano-particle fluorescence body
Figure 17 is the present inventionNano-particle fluorescence body X-ray diffractogram.
Figure 18 is the present inventionNano-particle fluorescence body SEM figures.
Figure 19 is the present inventionThe transmitting figure of nano-particle fluorescence body
Figure 20 is the present inventionThe excitation figure of nano-particle fluorescence body
Specific implementation mode
The present invention is specifically described below by embodiment, it is necessary to which indicated herein is that following embodiment is only used
In invention is further explained, it should not be understood as limiting the scope of the invention, person skilled in art can
To make some nonessential modifications and adaptations to the present invention according to aforementioned present invention content.
Embodiment 1：Preparation
1. taking the Y (NO of 0.25mol3)3.6H2O is dissolved in appropriate vessel, and deionized water 1000ml is added and is configured to
Y (the NO of 0.25mol/L3)3Solution, it is spare；
2. taking the Eu of 0.125mol2O3With the dust technology 528ml dissolvings of 1.5mol/L, Eu (NO are obtained3)3, it is subsequently placed in
1h is heated at a temperature of 60 DEG C in water-bath and evaporates extra nitric acid, add deionized water and complement to 1000ml so that
Eu(NO3)3A concentration of 0.25mol/L；
3. by Y (NO obtained in step 13)3Eu (NO obtained in solution 39.6ml and step 23)3Solution 0.4ml, sets
In appropriate vessel, the neopelex of 0.02mol is added, is subsequently placed in magnetic stirring apparatus and stirs 35min, then
1- butyl -3- methyl imidazolium tetrafluoroborates 4.65ml is added, it is closed to continue to stir 2h, mixed liquor is obtained, it is spare；
4. mixed liquor obtained in step 3 is placed in the reaction kettle of polytetrafluoroethylene (PTFE), it is subsequently placed in baking oven, setting temperature
190 DEG C of degree keeps 22h, takes out, and placement is cooled to 25 DEG C, spare；
5. taking mixed liquor after cooling in step 4, it is placed in a centrifuge and is centrifuged 4 minutes in 8000r/min, discarded supernatant
Liquid collects centrifugation, and the absolute ethyl alcohol washing precipitation 3 times for precipitating 10 times of quality is then added, every time after the completion of washing with from
Scheming centrifuges 4 minutes in rotating speed 8000r/min, collects and precipitates to get crude product, spare；
6. crude product is placed in baking oven, 60 DEG C of oven temperature is set, is dried 4 hours, take out to get
After measured, this product finished product yield is 99.3%, this product finished product purity 99.5%.Gas sensing property the experimental results showed that, this
Product have gas sensing property to imflammable gas.
Obtained by embodiment 1Nano-particle fluorescence body does XRD tests：
Radiation source is Cu cakes, and wavelength 1.54060m, scanning angle is 20 °~80 °, and voltage is 30 kV, and electric current is
20mA, sweep speed are 2.4 °/min, and the X diffraction patterns of X-ray nano particle are as shown in Figure 1.
Fig. 1 isThe X diffraction patterns of nano particle, 2 θ of X angle of diffraction 24.312 ± 0.2 °,
25.662±0.2°、27.636±0.2°、30.649±0.2°、 35.792±0.2°、40.779±0.2°、46.787±
0.2 °, 47.314 ± 0.2 °, 51.998 ± 0.2 °, 53.194 ± 0.2 °, 54.823 ± 0.2 °, 63.273 ± 0.2 ° etc. has
Diffraction maximum.
By will be obtained by embodiment 1Nano-particle fluorescence body carries out electron-microscope scanning, and scanning result is shown in
Fig. 2.
As seen from Figure 2The pattern of nano-particle fluorescence body is the form of grain of rice rod-shpaed particle aggregation
Nano particle.Grain of rice rod-shpaed particle grain size is grown between 170-240nm.
Embodiment 2Preparation
1. taking the Y (NO of 0.25mol3)3.6H2O is dissolved in appropriate vessel, and deionized water 1000ml is added and is configured to
Y (the NO of 0.25mol/L3)3Solution, it is spare；
2. taking the Eu of 0.125mol2O3With the dust technology 528ml dissolvings of 1.5mol/L, Eu (NO are obtained3)3, it is subsequently placed in
1h is heated at a temperature of 60 DEG C in water-bath and evaporates extra nitric acid, add deionized water and complement to 1000ml so that
Eu(NO3)3A concentration of 0.25mol/L；
3. by Y (NO obtained in step 13)3Eu (NO obtained in solution 38ml and step 23)3Solution 2ml is placed in suitable
In suitable container, the neopelex of 0.02mol is added, is subsequently placed in magnetic stirring apparatus and stirs 35min, is then added
1- butyl -3- methyl imidazolium tetrafluoroborates 4.65ml, it is closed to continue to stir 2h, mixed liquor is obtained, it is spare；
4. mixed liquor obtained in step 3 is placed in the reaction kettle of polytetrafluoroethylene (PTFE), it is subsequently placed in baking oven, setting temperature
190 DEG C of degree keeps 22h, takes out, and placement is cooled to 25 DEG C, spare；
5. taking mixed liquor after cooling in step 4, it is placed in a centrifuge and is centrifuged 4 minutes in 8000r/min, discarded supernatant
Liquid collects centrifugation, and the absolute ethyl alcohol washing precipitation 3 times for precipitating 10 times of quality is then added, every time after the completion of washing with from
Scheming centrifuges 4 minutes in rotating speed 8000r/min, collects and precipitates to get crude product, spare；
6. crude product is placed in baking oven, 60 DEG C of oven temperature is set, is dried 4 hours, take out to get
After measured, this product finished product yield is 99.2%, this product finished product purity 99.6%.Gas sensing property the experimental results showed that, this
Product have gas sensing property to imflammable gas.
Obtained by embodiment 2Nano-particle fluorescence body does XRD tests：
Radiation source is Cu cakes, and wavelength 1.54060m, scanning angle is 20 °~80 °, and voltage is 30 kV, and electric current is
20mA, sweep speed are 2.4 °/min, and the X diffraction patterns of X-ray nano particle are as shown in Figure 5.
Fig. 5 isThe X diffraction patterns of nano particle, 2 θ of X angle of diffraction 24.312 ± 0.2 °,
25.662±0.2°、27.481±0.2°、30.701±0.2°、 35.792±0.2°、40.727±0.2°、43.584±
0.2°、45.299±0.2°、 46.753±0.2°、47.169±0.2°、48.831±0.2°、50.961±0.2°、
51.896 ± 0.2 ° etc. have diffraction maximum.
Obtained by embodiment 3Nano-particle fluorescence body carries out electron-microscope scanning, and scanning result is shown in figure
6。
As seen from Figure 6The pattern of nano-particle fluorescence body is agglomerating by the aggregation of rice-shaped little particle
Shape.Rice-shaped little particle grain size is about 120-260nm.
Embodiment 3：Preparation
1. taking the Y (NO of 0.25mol3)3.6H2O is dissolved in appropriate vessel, and addition goes deionized water 1000ml to be configured to
Y (the NO of 0.25mol/L3)3Solution, it is spare；
2. taking the Eu of 0.125mol2O3With the dust technology 528ml dissolvings of 1.5mol/L, Eu (NO are obtained3)3, it is subsequently placed in
1h is heated at a temperature of 60 DEG C in water-bath and evaporates extra nitric acid, add deionized water and complement to 1000ml so that
Eu(NO3)3A concentration of 0.25mol/L；
3. by Y (NO obtained in step 13)3Eu (NO obtained in solution 36ml and step 23)3Solution 4ml is placed in suitable
In suitable container, the neopelex of 0.02mol is added, is subsequently placed in magnetic stirring apparatus and stirs 30min, is then added
1- butyl -3- methyl imidazolium tetrafluoroborates 4.65ml, it is closed to continue to stir 1h, mixed liquor is obtained, it is spare；
4. mixed liquor obtained in step 3 is placed in the reaction kettle of polytetrafluoroethylene (PTFE), it is subsequently placed in baking oven, setting temperature
180 DEG C of degree keeps for 24 hours, taking out, and placement is cooled to 20 DEG C, spare；
5. taking mixed liquor after cooling in step 4, it is placed in a centrifuge and is centrifuged 4 minutes in 6000r/min, discarded supernatant
Liquid collects centrifugation, and the absolute ethyl alcohol washing precipitation 3 times for precipitating 10 times of quality is then added, every time after the completion of washing with from
Scheming centrifuges 4 minutes in rotating speed 6000r/min, collects and precipitates to get crude product, spare；
6. crude product is placed in baking oven, 60 DEG C of oven temperature is set, is dried 4 hours, take out to get
After measured, this product finished product yield is 99.1%, this product finished product purity 99.8%.Gas sensing property the experimental results showed that, this
Product have gas sensing property to imflammable gas.
Obtained by embodiment 1Nano-particle fluorescence body does XRD tests：
Radiation source is Cu cakes, and wavelength 1.54060m, scanning angle is 20 °~80 °, voltage 30kV, electric current 20mA,
Sweep speed is 2.4 °/min.The X diffraction patterns of its X-ray nano particle are as shown in Figure 9.
YF2.9Eu0.12 θ of X angle of diffraction of nano particle 24.315 ± 0.2 °, 25.756 ± 0.2 °, 27.636 ±
0.2°、30.751±0.2°、35.847±0.2°、 40.812±0.2°、42.699±0.2°、45.314±0.2°、46.754
±0.2°、 47.333±0.2°、48.843±0.2°、51.125±0.2°、52.003±0.2°、 53.197±0.2°、
54.789 ± 0.2 °, 57.766 ± 0.2 ° etc. have diffraction maximum.
By will be obtained by embodiment 1Nano-particle fluorescence body carries out electron-microscope scanning, and scanning result is shown in figure
10。
As seen from Figure 6The pattern of nano-particle fluorescence body is gathered into greatly by rice-shaped little particle
It is spherical.Rice-shaped little particle grain size is about 120-260nm, and spherical grain size is about 0.8-1um
Embodiment 4：Preparation
1. taking the Y (NO of 0.25mol3)3.6H2O is dissolved in appropriate vessel, and deionized water 1000ml is added and is configured to
Y (the NO of 0.25mol/L3)3Solution, it is spare；
2. taking the Eu of 0.125mol2O3With the dust technology 528ml dissolvings of 1.5mol/L, Eu (NO are obtained3)3, it is subsequently placed in
1h is heated at a temperature of 60 DEG C in water-bath and evaporates extra nitric acid, add deionized water and complement to 1000ml so that
Eu(NO3)3A concentration of 0.25mol/L；
3. by Y (NO obtained in step 13)3Eu (NO obtained in solution 34ml and step 23)3Solution 6ml is placed in suitable
In suitable container, the neopelex of 0.02mol is added, is subsequently placed in magnetic stirring apparatus and stirs 35min, is then added
1- butyl -3- methyl imidazolium tetrafluoroborates 4.65ml, it is closed to continue to stir 2h, mixed liquor is obtained, it is spare；
4. mixed liquor obtained in step 3 is placed in the reaction kettle of polytetrafluoroethylene (PTFE), it is subsequently placed in baking oven, setting temperature
190 DEG C of degree keeps 22h, takes out, and placement is cooled to 25 DEG C, spare；
5. taking mixed liquor after cooling in step 4, it is placed in a centrifuge and is centrifuged 4 minutes in 8000r/min, discarded supernatant
Liquid collects centrifugation, and the absolute ethyl alcohol washing precipitation 3 times for precipitating 10 times of quality is then added, every time after the completion of washing with from
Scheming centrifuges 4 minutes in rotating speed 8000r/min, collects and precipitates to get crude product, spare；
6. crude product is placed in baking oven, 60 DEG C of oven temperature is set, is dried 4 hours, take out to get
After measured, this product finished product yield is 99.5%, this product finished product purity 99.2%.Gas sensing property the experimental results showed that, this
Product have gas sensing property to imflammable gas.
Obtained by embodiment 4Nano-particle fluorescence body does XRD tests：
Radiation source is Cu cakes, and wavelength 1.54060m, scanning angle is 20 °~80 °, and voltage is 30 kV, and electric current is
20mA, sweep speed are 2.4 °/min, and the X diffraction patterns of X-ray nano particle are as shown in figure 13.
Figure 13 isThe X diffraction patterns of nano particle, 2 θ of X angle of diffraction 24.208 ± 0.2 °,
25.714±0.2°、27.536±0.2°、30.597±0.2°、 35.792±0.2°、40.727±0.2°、43.532±
0.2°、45.299±0.2°、 46.701±0.2°、47.169±0.2°、48.675±0.2°、51.169±0.2°、
51.948 ± 0.2 °, 53.297 ± 0.2 °, 54.649 ± 0.2 ° etc. have diffraction maximum.
Obtained by embodiment 4Nano-particle fluorescence body carries out electron-microscope scanning, and scanning result is shown in figure
14。
As seen from Figure 14The pattern of particle fluorescence body is to be gathered into western orchid by rice-shaped little particle
It is flower-shaped.Rice-shaped little particle grain size is about 120-210nm, and broccoli shape grain size is about 0.4-0.8um, and is evenly distributed.
Embodiment 5：Preparation
1. taking the Y (NO of 0.25mol3)3.6H2O is dissolved in appropriate vessel, and deionized water 1000ml is added and is configured to
Y (the NO of 0.25mol/L3)3Solution, it is spare；
2. taking the Eu of 0.125mol2O3With the dust technology 528ml dissolvings of 1.5mol/L, Eu (NO are obtained3)3, it is subsequently placed in
1h is heated at a temperature of 60 DEG C in water-bath and evaporates extra nitric acid, add deionized water and complement to 1000ml so that
Eu(NO3)3A concentration of 0.25mol/L；
3. by Y (NO obtained in step 13)3Eu (NO obtained in solution 38ml and step 23)3Solution 4ml is placed in suitable
In suitable container, the neopelex of 0.02mol is added, is subsequently placed in magnetic stirring apparatus and stirs 35min, is then added
1- butyl -3- methyl imidazolium tetrafluoroborates 4.65ml, it is closed to continue to stir 2h, mixed liquor is obtained, it is spare；
4. mixed liquor obtained in step 3 is placed in the reaction kettle of polytetrafluoroethylene (PTFE), it is subsequently placed in baking oven, setting temperature
190 DEG C of degree keeps 22h, takes out, and placement is cooled to 25 DEG C, spare；
5. taking mixed liquor after cooling in step 4, it is placed in a centrifuge and is centrifuged 4 minutes in 8000r/min, discarded supernatant
Liquid collects centrifugation, and the absolute ethyl alcohol washing precipitation 3 times for precipitating 10 times of quality is then added, every time after the completion of washing with from
Scheming centrifuges 4 minutes in rotating speed 8000r/min, collects and precipitates to get crude product, spare；
6. crude product is placed in baking oven, 60 DEG C of oven temperature is set, is dried 4 hours, take out to get
After measured, this product finished product yield is 99.3%, this product finished product purity 99.5%.Gas sensing property the experimental results showed that, this
Product have gas sensing property to imflammable gas.
Obtained by embodiment 5Nano-particle fluorescence body does XRD tests：
Radiation source is Cu cakes, and wavelength 1.54060m, scanning angle is 20 °~80 °, voltage 30kV, electric current 20mA,
Sweep speed is 2.4 °/min, and the X diffraction patterns of X-ray nano particle are as shown in the figure.
Figure 17 isThe X diffraction patterns of nano particle, 2 θ of X angle of diffraction 24.260 ± 0.2 °,
25.949±0.2°、27.882±0.2°、30.6974±0.2°、35.536±0.2°、 41.003±0.2°、43.378±
0.2°、45.78±0.2°、46.547±0.2°、48.675±0.2°、50.757±0.2°、51.739±0.2°、52.673±
0.2 °, 54.381 ± 0.2 ° etc. etc. has diffraction maximum.
Obtained by embodiment 5Nano-particle fluorescence body carries out electron-microscope scanning, and scanning result is shown in figure
18。
As seen from Figure 18The pattern of particle fluorescence body is to be gathered into western orchid by rice-shaped little particle
It is flower-shaped.Rice-shaped little particle grain size is about 120-210nm, and broccoli shape grain size is about 0.4-0.8um.
Embodiment 6：Luminescent properties detect:
Obtained by Example 3The fluorescence property of nano-particle fluorescence body is tested, and experimental result is shown in figures
11.As shown in Figure 11,Under 394nm near ultraviolet excitations, it is clearly visible the fluorophor in 556.4nm,
588.6nm, 594.8nm, 616.8nm have apparent diffraction maximum, wherein most strong at the peak that 594.8nm occurs.
Claims (5)
1. a kind of Y1-xF3:xEu3+The preparation method of nano-particle fluorescence body, it is characterised in that：It is with Y (NO3)3.6H2O、
Eu2O3, surfactant, 1- butyl -3- methyl imidazolium tetrafluoroborates be raw material, respectively by closed stirring, hydro-thermal reaction,
Centrifugation, washing, drying and etc. be made, the X value ranges be 0.01~0.2.
2. a kind of Y as described in claim 11-xF3:xEu3+The preparation method of nano-particle fluorescence body, it is characterised in that：It is described
Surfactant is one kind in disodium EDTA or neopelex.
3. a kind of Y as claimed in claim 21-xF3:xEu3+The preparation method of nano-particle fluorescence body, it is characterised in that：It is described
Surfactant is preferably neopelex.
4. a kind of Y as claimed in claim 31-xF3:xEu3+The preparation method of nano-particle fluorescence body, it is characterised in that：It is described
Neopelex addition need to meet Eu in solution3+With Y3+The sum of with the molar ratio of neopelex be 1:
2。
5. a kind of Y as claimed in claim 41-xF3:xEu3+The preparation method of nano-particle fluorescence body, it is characterised in that：It is
Including getting off, step is made：
(1) takes Y (NO3)3.6H2O is dissolved in appropriate vessel, and the Y (NO that deionized water is configured to 0.25mol/L are added3)3It is molten
Liquid, it is spare；
(2) takes Eu2O3It is first dissolved with dust technology, obtains Eu (NO3)3, it is subsequently placed in water-bath in water-bath and evaporates extra nitre
Acid adds the Eu (NO that deionized water is configured to 0.25mol/L3)3；A concentration of 1.5mol/L of the dust technology, it is described
Eu2O3Mass volume ratio with dust technology is 1:12；The bath temperature is 50~60 DEG C, and water bath time is 1~2h；
(3) is by Y (NO obtained in step (1)3)3Solution and Eu (NO3)3Solution is placed in appropriate vessel, and detergent alkylate is added
Sodium sulfonate is subsequently placed in 30~40min of stirring in magnetic stirring apparatus, 1- butyl -3- methyl imidazolium tetrafluoroborates is then added,
It is closed to continue 1~2h of stirring, mixed liquor is obtained, it is spare；Y (the NO3)3Solution, Eu (NO3)3Solution and 1- butyl -3- methyl miaows
The molar ratio of azoles tetrafluoroborate is 0.99~0.80:0.1~0.2:1~3；
(4) mixed liquor obtained in step (3) is placed in the reaction kettle of polytetrafluoroethylene (PTFE) by, is subsequently placed in baking oven, setting temperature
180~190 DEG C of degree, keep 22~for 24 hours, it takes out, placement is cooled to 20~25 DEG C, spare；
(5) takes mixed liquor after cooling in step (4), is placed in a centrifuge and is centrifuged 4~6 minutes in 6000~8000r/min,
Liquid is discarded supernatant, centrifugation is collected, the absolute ethyl alcohol washing that 10 times of quality of precipitation are then added precipitates 3 times, has washed every time
Cheng Houyong centrifuges centrifuge 4~6 minutes in 6000~8000r/min of rotating speed, collect and precipitate to get crude product, spare；
(6) crude product is placed in baking oven by, and drying is taken out to get Y1-xF3:xEu3+；78~82 DEG C of the drying temperature, when drying
Between be 6~10 hours.
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| CN101476151A (en) * | 2009-03-17 | 2009-07-08 | 中国科学院长春光学精密机械与物理研究所 | Ion thermal growth method of near infrared light upper conversion fluoride nano crystal |
| CN101786649A (en) * | 2010-03-04 | 2010-07-28 | 上海大学 | Method for preparing rare-earth fluoride nanometer mesoporous spheres |
| CN105778902A (en) * | 2016-01-12 | 2016-07-20 | 佛山科学技术学院 | Preparation method of rare earth hollow nanocrystal |
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| CN101476151A (en) * | 2009-03-17 | 2009-07-08 | 中国科学院长春光学精密机械与物理研究所 | Ion thermal growth method of near infrared light upper conversion fluoride nano crystal |
| CN101786649A (en) * | 2010-03-04 | 2010-07-28 | 上海大学 | Method for preparing rare-earth fluoride nanometer mesoporous spheres |
| CN105778902A (en) * | 2016-01-12 | 2016-07-20 | 佛山科学技术学院 | Preparation method of rare earth hollow nanocrystal |
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