CN108753299A - A kind of Y1-x-yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body - Google Patents
A kind of Y1-x-yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
- C09K11/7772—Halogenides
Abstract
A kind of Y1‑x‑yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body, which is characterized in that it is with Y (NO3)3.6H2O、Tb4O7、Ce(NO3)3.6H2O, 1- butyl -3- methyl imidazolium tetrafluoroborates, surfactant, dust technology be raw material, respectively pass through solution preparation steps, with liquid whipping step, hydro-thermal reaction step, centrifuge washing drying and etc. be made.The present invention is successfully realized the doping of Ce, Tb, and preparation process does not have the generation of the poisonous and harmful substances such as HF, environmentally friendly, it does not pollute the environment, product luminous intensity obtained is high, and stable luminescence, finished product is at stub form, aggregation extent is high, and be uniformly dispersed, shine plane of refraction light, and illumination effect is good, finished product purity is high, high income, up to 98.3% or more, stability of photoluminescence are good, after placing 3 months, luminous intensity with comparing for 0 day, and almost unchanged, it is simple and easy to get that the present invention prepares raw material, it is cheap, it is worth marketing application.
Description
Technical field
The present invention relates to a kind of Y1-x-yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body.
Background technology
In three primary colors fluorescent powder, Tb3+、Ce3+The rare-earth salts of activation is green emitting phosphor, green powder to the luminous flux of lamp most
Greatly.In Ce3+And Tb3+The YF of codope3In, due to from Ce3+To Tb3+Between there are energy transmission, Ce3+It can be shown as sensitizer
Write enhancing Tb3+In the green emitted of 545nm, therefore crystallite Y1-x-yF3:xCe3+,yTb3+Luminescent color can by change mix
Miscellaneous Tb3+Concentration be adjusted, may be implemented from it is orange to yellow again to green luminescent color change.The green powder of three-basic-colour lamp
With Tb3+As activator, Tb3+Maximum emission peak be located at 545nm, belong to Tb3+'s5D4→7F5Transition.Ce3+In 254nm
Nearby there is strong absorption, there is strong transmitting, Ce in the long wave ultraviolet area of 330~400nm3+Radiationless energy transmission can be passed through
Energy is effectively transferred to Tb3+。
And most widely used aluminate green powder is because firing temperature is high at present, synthesis cycle is long, and the powder after firing is hard,
The disadvantages such as processing is difficult, and yield is low.
Rare earth fluoride has low phonon energy, high heat and environmental stability, has become in luminescent material at present
Good host material.So causing great attention, YF by the research of the nano luminescent material of matrix of fluoride3It is
A kind of very important metal fluoride, about pencil YF3Preparation report it is also seldom, such as Wang is with Y (NO3)3.6H2O
It is that raw material has synthesized a diameter of 100nm by the simple precipitation method with HF, length is the YF of 500nm3Nanometer bundle, the nanometer bundle by
Many nano wire aggregation compositions.Zhang etc. uses a kind of simple microwave irradiation, has synthesized YF3:The nanometer bundle of Yb, Tm, receive
Meter Shu is made of nanobelt, and has studied their optical property.At present apparently, the preparation side of rear-earth-doped luminous nano granule
Method is unfavorable to human and environment because there are preparation process will produce the poisonous and harmful substances such as HF for it, while there is also complicated for operation, lifes
Produce of high cost, low yield, product purity is low, and product luminous intensity obtained is not ideal enough, surrounds and watches aggregation extent defective tightness simultaneously
And dispersion is not uniform enough, and the development in nano-particle fluorescence body field is restrict so as to cause technical problems such as illumination effect differences.
Rear-earth-doped luminous nano granule with unique luminescent properties because making it in fields such as biomedicines with extensively
Application prospect, thus cause more and more to pay close attention to.When rare earth nanometer particle is as biological fluorescent labeling and when practical application,
It may interact with large biological molecules such as protein in organism and DNA, and then influence their structure and function,
Unknown physiological effect is generated, so the interaction of research rare-earth fluorescent nano particle and protein is to nano biological medicine
Development and the evaluation of rare earth nanometer particle safety in utilization have important practical significance.And it is glimmering with changes such as surfactants
Light powder it is also possible to certain specific sites with gene are combined, with this marker gene, probes into gene choosing to the compatibility of organism
The applications such as the principle of selecting property expression.Therefore the research of fluorescent powder is for genetic engineering, protein engineering, the biology neck such as cell engineering
The marker research in domain has certain complementary potential value.Currently, in relation to rare earth nanometer particle and protein interaction
Research it is seldom, according to the literature, people have found that rare-earth compounds have that some are special in the sixties in last century
Pharmacological action, such as blood coagulation resisting function, anti-inflammatory and bactericidal effect, anti arteriosclerosis effect and antitumaous effect etc..And there is research
Show that the toxicity of rare earth compounding is also lower than the toxicity of some transient metal complexes and the drug of part organic synthesis.
YF3Crystal has low phonon energy, high heat and environmental stability, is widely used in luminous host material, and
YF3:Ce3+, Tb3+It is the important green luminescent material used in three primary colors fluorescent powder.The preparation of fluorescent powder is mainly high temperature solid-state
Method, although method is simple, due to the limitation of the conventional method so that the centre of luminescence disperses uneven, influence in matrix
Its luminous efficiency.For this purpose, people have been devoted to, research low temperature, particle size is small, purity is high and need not be sintered and grind
Synthetic method, such as hydro-thermal method, microemulsion method and microwave method.
Invention content
Present invention aims at provide a kind of Y1-x-yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body.
The object of the invention is achieved through the following technical solutions：
A kind of Y1-x-yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body, which is characterized in that it is with Y
(NO3)3.6H2O、Tb4O7、Ce(NO3)3.6H2O, 1- butyl -3- methyl imidazolium tetrafluoroborates, surfactant, dust technology are
Raw material, respectively pass through solution preparation steps, with liquid whipping step, hydro-thermal reaction step, centrifuge washing drying and etc. be made；Its
Described in x, y value be 0.02,0.13 or 0.05,0.05.
Further, a kind of Y1-x-yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body, which is characterized in that described
Surfactant be octadecyl sodium thiophosphate, polyvinylpyrrolidone, polyethyleneimine, enuatrol, polyethylene glycol 400,
It is one or more in Macrogol 6000, polyethylene glycol 2000, lauryl sodium sulfate, neopelex.
Further, a kind of Y1-x-yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body, which is characterized in that described
Surfactant is preferably neopelex.
Further, a kind of Y1-x-yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body, which is characterized in that described
Solution allocation step is to take Y (NO3)3.6H2Y (the NO that deionized water is configured to 0.25mol/L are added in appropriate vessel in O3)3It is molten
Liquid, it is spare；Separately take Tb4O7, the dilute nitric acid dissolution of 2.5mol/L is first added, is subsequently placed in water-bath in 70~80 DEG C of temperature
3~4h of lower heating evaporates extra dust technology, adds the Tb (NO that deionized water is configured to 0.25mol/L3)3Solution, it is standby
With；The wherein described Tb4O7Mass volume ratio with dust technology is 1:10；Separately take Ce (NO3)3.6H2O is added deionized water and is configured to
Ce (the NO of 0.25mol/L3)3Solution, it is spare.
Further, a kind of Y1-x-yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body, which is characterized in that described
It is the Y (NO for taking above-mentioned configuration with liquid whipping step3)3Solution, Tb (NO3)3Solution, Ce (NO3)3Solution is placed in appropriate vessel,
Neopelex is added, 50~55min is stirred at 20~25 DEG C, after the completion of stirring, 1- butyl -3- methyl miaows are added
Azoles tetrafluoroborate controls 20~25 DEG C of temperature, and closed stirring 3~4h, 100~120r/min of rotating speed obtain mixed liquor, spare.
Further, a kind of Y1-x-yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body, which is characterized in that the Y
(NO3)3Solution, Tb (NO3)3Solution, Ce (NO3)3The volume ratio of solution is 18:1:1 or 17:0.4:2.6, the Ce3+、Tb3+With
Y3+The amount ratio of the sum of amount of substance and neopelex substance is 1:2, the Ce3+、Tb3+And Y3+The amount of substance
The sum of with the ratio between the amount of 1- butyl -3- methyl imidazolium tetrafluoroborate substances be 1:1~3.
Further, a kind of Y1-x-yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body, which is characterized in that described
Hydro-thermal reaction step is that first mixed liquor is placed in tetrafluoroethene reaction kettle, and then reaction kettle is placed in baking oven, and temperature is arranged
170~180 DEG C, 19~21h is reacted, after reaction, cooled to room temperature is to get precipitation crude product 1.
Further, a kind of Y1-x-yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body, which is characterized in that described
Centrifuge washing baking step is will to precipitate crude product 1 to be transferred in centrifuge tube, and ethyl alcohol is added, is washed, and washing every time terminates to need
Centrifugal treating, 5000~7000r/min of centrifuge speed, 3~4min of centrifugation time are carried out with centrifuge, centrifugation terminates, topples over
Supernatant liquor obtains crude product 2, and crude product 2 is placed in baking oven, setting 55~65 DEG C of drying temperature be dried 5~8h to get at
Product.
Further, a kind of Y1-x-yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body, which is characterized in that centrifugation
Ethyl alcohol described in washing and drying step is absolute ethyl alcohol, and addition is precipitate 1 volume of crude product 7~10 times, the washing times
It is 2~3 times.
The present invention has following advantageous effect：
A kind of Y of the present invention1-x-yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body is successfully realized Ce, Tb
Doping, preparation process does not have the generation of the poisonous and harmful substances such as HF, environmentally friendly, does not pollute the environment, product hair obtained
Luminous intensity is high, stable luminescence, and for finished product at stub form, aggregation extent is high, and is uniformly dispersed, and shine plane of refraction light, illumination effect
Good, finished product purity is high, and high income, up to 98.3% or more, stability of photoluminescence is good, and after placing 3 months, luminous intensity was the same as 0 day
Compare, almost unchanged, it is simple and easy to get that the present invention prepares raw material, cheap, is worth marketing application.
Description of the drawings
Fig. 1 is Y of the present invention0.9F3:0.05Ce3+,0.05Tb3+The XRD diffraction patterns of nano particle.
Fig. 2 is Y of the present invention0.9F3:0.05Ce3+,0.05Tb3+The SEM of nano particle schemes.
Fig. 3 is Y of the present invention0.9F3:0.05Ce3+,0.05Tb3+The exciting light spectrogram of nano particle.
Fig. 4 is Y of the present invention0.9F3:0.05Ce3+,0.05Tb3+The launching light spectrogram of nano particle.
Fig. 5 is Y of the present invention0.85F3:0.02Ce3+,0.13Tb3+The XRD diffraction patterns of nano particle.
Fig. 6 is Y of the present invention0.85F3:0.02Ce3+,0.13Tb3+The SEM of nano particle schemes.
Fig. 7 is Y of the present invention0.85F3:0.02Ce3+,0.13Tb3+The exciting light spectrogram of nano particle.
Fig. 8 is Y of the present invention0.85F3:0.02Ce3+,0.13Tb3+The launching light spectrogram of nano particle.
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：A kind of Y0.9F3:0.05Ce3+,0.05Tb3+The preparation of nano-particle fluorescence body
Accurately weigh 47.8825gY (NO3)3.6H2O deionized water dissolvings and being diluted in 500ml volumetric flasks are made into
Y (the NO of 0.25mol/L3)3Solution, it is spare.By 2.3365g Tb4O7With the dilute nitric acid dissolution of 2.5mol/L, then evaporate
After extra nitric acid, addition deionized water, which is diluted in 50ml volumetric flasks, is made into 0.25mol/L Tb (NO3)3Solution, it is spare.
By 5.4265g Ce (NO3)3.6H2O deionized water dissolvings are simultaneously diluted in 50ml volumetric flasks, are made into 0.25mol/L Ce
(NO3)3Solution, it is spare.18ml 0.25mol/L Y (NO are accurately pipetted with liquid-transfering gun3)3, 1000 μ l 0.25mol/L Ce
(NO3)3, 1000 μ l 0.25mol/L Tb (NO3)3, in addition 3.4848g (control RE3+:SDBS=1:2, wherein RE3+For trivalent
Rare earth ion Ce3+、Tb3+And Y3+The sum of) neopelex (SDBS) is in the small glue beakers of 100ml, then addition stirring
Son stirs 52min on magnetic stirring apparatus, and 2.800g (2314 μ l) 1- butyl -3- methyl imidazolium tetrafluoroborates, control is added
22 DEG C of temperature, covers preservative film (closed), and setting rotating speed 100r/min stirs 3h.Mixed liquor is transferred to 100ml polytetrafluoroethyl-nes
In the reaction kettle of alkene.Reaction kettle is placed in baking oven, 20h is kept at 175 DEG C.It waits for that it is cooled to room temperature, 3 is precipitated with ethanol wash
It is secondary.Each washing centrifuge topples over supernatant liquor after keeping 4min, obtains crude product 2 in centrifuge speed 6000r/min.It will
Crude product 2 is placed in baking oven, is dried 7h in 60 DEG C of air atmospheres, is obtained finished product.After measured, this product finished product yield is 98.3%.
Experiment one：Product made from embodiment 1 is done into following measurement
Product made from embodiment 1 is subjected to XRD tests：
Radiation source is Cu cakes, and wavelength 1.54060m, scanning angle is 20 °~80 °, voltage 30kV, electric current 20mA,
Sweep speed is as shown in Figure 1 for the XRD diffraction patterns of its X-ray nano particle of 2.4 °/min..As seen from the figure, XRD angle of diffraction
2 θ 24.208 ± 0.2 °, 25.610 ± 0.2 °, 27.481 ± 0.2 °, 30.597 ± 0.2 °, 35.740 ± 0.2 °, 40.623 ±
0.2°、43.532±0.2°、45.247±0.2°、46.597±0.2°、47.169±0.2°、48.727±0.2°、50.909
± 0.2 °, 51.844 ± 0.2 °, 52.987 ± 0.2 °, 54.597 ± 0.2 ° etc. has rank to penetrate peak.
To the product obtained by embodiment 1 be subjected to electron-microscope scanning, scanning result is shown in Fig. 2.
Y as seen from Figure 20.9F3:0.05Ce3+,0.05Tb3+Product is the nano material of stub state of aggregation, aggregation extent
Height, and be uniformly dispersed.
Product obtained by embodiment 1 is done into excitation spectrum experiment, experimental result is shown in Fig. 3.From the figure 3, it may be seen that Y0.9F3:
0.05Ce3+,0.05Tb3+Under 544.6nm monitorings, the excitation spectrum highest peak of sample appears in 261.0nm.
By the Y obtained by embodiment 10.9F3:0.05Ce3+,0.005Tb3+Nano-particle fluorescence body nano-particle fluorescence body
Emission spectrum experiment is done, experimental result is shown in Fig. 4.As shown in Figure 4, Y0.9F3:0.05Ce3+,0.05Tb3+In 261nm ultraviolet excitations
It measures, is clearly visible in 486.2nm, 491.2nm, 496.4nm, 544.8nm, 552.6nm, 585.2nm, 589.8nm,
622.2nm has apparent diffraction maximum, wherein most strong at the peak that 544.8nm occurs.
Experiment two：Stability experiment：Y made from Example 10.9F3:0.05Ce3+,0.005Tb3+Nano-particle fluorescence
Body finished product is placed in conventional seals polybag place 3 months, 3 months after take out, carry out XRD tests, the experimental results showed that,
Significant change does not occur for XRD diffraction patterns, you can thinks that product component does not change, compared with 0 day, the degree of approximation reaches fluorescence intensity
To 99% or more, luminous intensity does not change, therefore, it can be said that this product good light stability.
Embodiment 2：A kind of Y0.85F3:0.02Ce3+,0.13Tb3+The preparation of nano-particle fluorescence body
Accurately weigh 47.8825gY (NO3)3.6H2Deionized water is added in 500ml volumetric flasks and is made into for O dissolved dilutions
0.25mol/LY(NO3)3Solution for standby.By 2.3365g Tb4O7With the dilute nitric acid dissolution of 2.5mol/L, then evaporate more
After remaining nitric acid, with deionized water dissolving and it is diluted in 50ml volumetric flasks and is made into 0.25mol/L Tb (NO3)3Solution for standby.
By 5.4265g Ce (NO3)3.6H2O dissolved dilutions are made into 0.25mol/L Ce (NO in 50ml volumetric flasks3)3Solution for standby.
17ml 0.25mol/L Y (NO are accurately pipetted with liquid-transfering gun3)3, 400 μ l 0.25mol/L Ce (NO3)3, 2600 μ l
0.25mol/L Tb(NO3)3, in addition 3.4848g (control RE3+:SDBS=1:2, wherein RE3+ are the rare earth ion Ce of trivalent3 +、Tb3+And Y3+The sum of) neopelex (SDBS) is in the small glue beakers of 100ml, then addition stirrer is stirred in magnetic force
It mixes and stirs 55min on device, 2.800g (2314 μ l) 1- butyl -3- methyl imidazolium tetrafluoroborates are added, controlled at 25 DEG C
Preservative film (closed) is covered, setting rotating speed 120r/min stirs 3h.Mixed liquor is transferred to the reaction kettle of 100ml polytetrafluoroethylene (PTFE)
In.Reaction kettle is placed in baking oven, 21h is kept at 180 DEG C.It waits for that it is cooled to room temperature, is precipitated 3 times with ethanol wash.It washes every time
It washs with centrifuge in centrifuge speed 6000r/min, topples over supernatant liquor after keeping 4min, obtain crude product 2.Crude product 2 is placed in
In baking oven, is dried in 60 DEG C of air atmospheres, obtain finished product.After measured, this product finished product yield is 98.8%.
Experiment one：Product made from embodiment 2 is done into following measurement
Product made from embodiment 1 is subjected to XRD tests：
Radiation source is Cu cakes, and wavelength 1.54060m, scanning angle is 20 °~80 °, voltage 30kV, electric current 20mA,
Sweep speed is as shown in Figure 1 for the XRD diffraction patterns of its X-ray nano particle of 2.4 °/min..As seen from the figure, XRD angle of diffraction
2 θ 24.208 ± 0.2 °, 25.610 ± 0.2 °, 27.532 ± 0.2 °, 30.649 ± 0.2 °, 35.688 ± 0.2 °, 40.675 ±
0.2°、43.584±0.2°、45.143±0.2°、46.649±0.2°、47.221±0.2°、48.675±0.2°、50.909
± 0.2 °, 51.844 ± 0.2 °, 52.987 ± 0.2 °, 54.597 ± 0.2 ° etc. has rank to penetrate peak.
To the product obtained by embodiment 1 be subjected to electron-microscope scanning, scanning result is shown in Fig. 2.
Y as seen from Figure 20.85F3:0.02Ce3+,0.13Tb3+Product is the nano material of stub state of aggregation, assembles journey
Degree is high, and is uniformly dispersed.
Product obtained by embodiment 1 is done into excitation spectrum experiment, experimental result is shown in Fig. 3.From the figure 3, it may be seen that Y0.85F3:
0.02Ce3+,0.13Tb3+Under 545.0nm monitorings, the excitation spectrum highest peak of sample appears in 262.0nm.
By the Y obtained by embodiment 20.85F3:0.02Ce3+,0.13Tb3+Nano-particle fluorescence body nano-particle fluorescence body is done
Emission spectrum is tested, and experimental result is shown in Fig. 4.As shown in Figure 4, Y0.85F3:0.02Ce3+,0.13Tb3+Swash in 261.0nm ultraviolet lights
Hair measures, and is clearly visible in 486.2nm, 491.2nm, 496.4nm, 544.8nm, 552.6nm, 585.2nm, 589.8nm,
622.2nm has apparent diffraction maximum, wherein most strong at the peak that 544.8nm occurs.
Experiment two：Stability experiment：Y made from Example 20.85F3:0.02Ce3+,0.13Tb3+Nano-particle fluorescence body
Finished product is placed in conventional seals polybag place 3 months, 3 months after take out, carry out XRD tests, the experimental results showed that, X spreads out
It penetrates figure and significant change does not occur, you can think that product component does not change, compared with 0 day, the degree of approximation reaches fluorescence intensity
99% or more, luminous intensity does not change substantially, therefore, it can be said that this product good light stability.
Claims (9)
1. a kind of Y1-x-yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body, which is characterized in that it is with Y (NO3)3.6H2O、Tb4O7、Ce(NO3)3.6H2O, 1- butyl -3- methyl imidazolium tetrafluoroborates, surfactant, dust technology are raw material,
Respectively pass through solution preparation steps, with liquid whipping step, hydro-thermal reaction step, centrifuge washing drying and etc. be made；Wherein institute
The value for stating x, y is 0.02,0.13 or 0.05,0.05.
2. a kind of Y as described in claim 11-x-yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body, feature exist
In the surfactant is octadecyl sodium thiophosphate, polyvinylpyrrolidone, polyethyleneimine, enuatrol, poly- second two
One kind or more in alcohol 400, Macrogol 6000, polyethylene glycol 2000, lauryl sodium sulfate, neopelex
Kind.
3. a kind of Y as claimed in claim 21-x-yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body, feature exist
In the surfactant is preferably neopelex.
4. a kind of Y as claimed in claim 31-x-yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body, feature exist
In the solution allocation step is to take Y (NO3)3.6H2The Y that deionized water is configured to 0.25mol/L is added in appropriate vessel in O
(NO3)3Solution, it is spare；Separately take Tb4O7, the dilute nitric acid dissolution of 2.5mol/L is first added, is subsequently placed in water-bath in 70 ~ 80 DEG C
At a temperature of heat 3 ~ 4h evaporate extra dust technology, add the Tb (NO that deionized water is configured to 0.25mol/L3)3It is molten
Liquid, it is spare；The wherein described Tb4O7Mass volume ratio with dust technology is 1:10；Separately take Ce (NO3)3.6H2Deionized water is added in O
It is configured to the Ce (NO of 0.25mol/L3)3Solution, it is spare.
5. a kind of Y as claimed in claim 41-x-yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body, feature exist
In the liquid whipping step of matching is the Y (NO for taking above-mentioned configuration3)3Solution, Tb (NO3)3Solution, Ce (NO3)3Solution is placed in suitable
In container, neopelex is added, 50 ~ 55min is stirred at 20 ~ 25 DEG C, after the completion of stirring, 1- butyl -3- is added
Methyl imidazolium tetrafluoroborate controls 20 ~ 25 DEG C of temperature, and closed stirring 3 ~ 4h, 100 ~ 120r/min of rotating speed obtain mixed liquor, standby
With.
6. a kind of Y as claimed in claim 51-x-yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body, feature exist
In the Y (NO3)3Solution, Tb (NO3)3Solution, Ce (NO3)3The volume ratio of solution is 18:1:1 or 17:0.4:2.6, it is described
Ce3+、Tb3+And Y3+The amount ratio of the sum of amount of substance and neopelex substance is 1:2, the Ce3+、Tb3+And Y3 +The ratio between the sum of amount of substance and the amount of 1- butyl -3- methyl imidazolium tetrafluoroborate substances are 1:1~3.
7. a kind of Y as claimed in claim 61-x-yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body, feature exist
In, the hydro-thermal reaction step is that first mixed liquor is placed in tetrafluoroethene reaction kettle, and then reaction kettle is placed in baking oven, if
170 ~ 180 DEG C of temperature is set, 19 ~ 21h is reacted, after reaction, cooled to room temperature is to get precipitation crude product 1.
8. a kind of Y as claimed in claim 71-x-yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body, feature exist
In the centrifuge washing baking step is will to precipitate crude product 1 to be transferred in centrifuge tube, and ethyl alcohol is added, is washed, and is washed every time
End need to carry out centrifugal treating, 5000 ~ 7000r/min of centrifuge speed, 3 ~ 4min of centrifugation time with centrifuge, and centrifugation terminates,
Topple over supernatant liquor, obtain crude product 2, crude product 2 is placed in baking oven, setting 55 ~ 65 DEG C of drying temperature be dried 5 ~ 8h to get
Finished product.
9. a kind of Y as claimed in claim 81-x-yF3:xCe3+,yTb3+The preparation method of nano-particle fluorescence body, feature exist
In ethyl alcohol described in centrifuge washing baking step is absolute ethyl alcohol, and addition is precipitate 1 volume of crude product 7 ~ 10 times, described to wash
It is 2 ~ 3 times to wash number.
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| CN111748346B (en) * | 2020-06-19 | 2021-06-15 | 浙江大学 | Up-conversion nanowire and preparation method and application thereof |
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