CN105838373A - Beta-NaYF4:Yb<3+>/Er<3+> micron crystal with red light directional emission performance - Google Patents
Beta-NaYF4:Yb<3+>/Er<3+> micron crystal with red light directional emission performance Download PDFInfo
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Abstract
The invention discloses a beta-NaYF4:Yb<3+>/Er<3+> micron crystal with red light directional emission performance. The crystal is synthesized in an alkaline environment by adopting sodium fluoride as a fluorine source, the synthetic method is simple and controllable, the reaction condition is mild and does not need modification in comparison with a pyrolytic process, and the prepared beta-NaYF4:Yb<3+>/Er<3+> micron crystal is good in crystallinity and dispersity, uniform in size and easy to be dissolved in water, and has a peculiar light emission characteristic: when exciting light is excited from top to bottom along any corner, or a middle position of an arc-shaped edge or the central axis of a single micron crystal, and the central axis or an adjacent corner of any crystal in multiple micron crystals, directional emission of red light can be realized; and the type of peculiar light emission characteristic ensures that the light emitting material can be applied to a laser, and the directional emission of monochromatic light can be realized without a wave limiting filter; the light emitting material also can be applied to biological imaging and has the advantage of accurately controlling the position of the exciting light; and the light emitting material also can be used as a waveguide modulator applied to research and development of a novel photoelectric device.
Description
Technical field
The invention belongs to luminescent material technical field, be specifically related to a kind of there is HONGGUANG directional transmissions performance
β-NaYF4:Yb3+/Er3+Micro-crystal.
Background technology
In trivalent rare earth ions doping upconverting fluorescent material has attracted world wide due to its exclusive physical characteristic
Scientist pay close attention to, especially in terms of optics, the electronic configuration of its uniqueness and abundant level structure impart its tool
Have that spectral line is sharp keen, launch that band is abundant, background fluorescence is low and the plurality of advantages such as fluorescence lifetime length.Along with science and technology
Development, rare earth luminescent material is widely applied to solaode, solid state laser, biomedicine, 3D imaging
The various fields such as false proof with infrared ray, has started the research boom in global range.At present, researchers have become
Prepared to merit the rare earth luminescent material of various pattern, as cylindricality, spherical, hexagonal dish type, dumb-bell shape with
And core-shell nucleocapsid structure etc..The preparation method reaction condition of these different-shape luminescent materials is violent, more
It is important that experimentation is loaded down with trivial details, it is impossible to the rare earth luminescent material of pattern required for one-step synthesis.Hydrothermal synthesis method
It is a kind of relatively simple, gentle, method efficiently by contrast, such as: Gao Dangli et al. uses ammonium fluoride conduct
Fluorine source uses the β-NaYF of water heat transfer4:Yb3+/Er3+Bar-shaped micro-crystal (Dangli Gao, Xiangyu Zhang,
And Wei Gao, ACS Appl.MatTm.IntTmfaces, 2013,5,9732-9739), Zhang Hong et al. use water
Full-boiled process has synthesized β-NaYF in the environment of weak acid4:Yb3+/Er3+Hexagonal plate-like micro-crystal (Junwei Zhao,
Yajuan Sun,Xianggui Kong,Lijin Tian,Yu Wang,Langping Tu,Jialong Zhao,and Hong
Zhang, J.Phys.Chem.B, 2008,112,15666-15672), the β-NaYF of both patterns4:Yb3+/Er3+
Micro-crystal is respectively provided with good fluorescent characteristic, can apply in fields such as sensing, solaode, bio-imagings,
But both micro-crystals all can not realize the directional transmissions of one-color fluorescence, and fluorescent emission image will not be with exciting light
The change of position and significantly change, therefore greatly limit its application and development further, such as: owing to it can not be real
Existing monochromatic directional transmissions, so limiting its application in the laser, and in the application aspect of bio-imaging,
It can not be precisely controlled exciting light position.
Summary of the invention
The technical problem to be solved is to provide a kind of and has HONGGUANG directional transmissions performance
β-NaYF4:Yb3+/Er3+Micro-crystal.
Solve above-mentioned technical problem and be employed technical scheme comprise that this crystal is prepared from by following method:
Sodium citrate is dissolved in deionized water, is then sequentially added into 0.2mol/LY (NO3)3Aqueous solution, 0.2mol/L
Yb(NO3)3Aqueous solution and 0.2mol/L Er (NO3)3Aqueous solution, is stirred at room temperature 20～40 minutes, then drips
The sodium fluoride aqueous solution of 1mol/L, continues stirring 15～30 minutes, with ammonia regulation pH value to 9～11, and gained
Mixed liquor proceeds in teflon-lined autoclave, and at 180～220 DEG C, hydro-thermal reaction 18～24 is little
Time, it is cooled to room temperature, is centrifuged, washs, is dried, obtain the β-NaYF with HONGGUANG directional transmissions performance4:Yb3+/Er3+
Micro-crystal, wherein Er (NO3)3、Yb(NO3)3、Y(NO3)3, sodium citrate, the mol ratio of sodium fluoride be 1:9～
11:37～40:73～95:900～1100.
The present invention has the β-NaYF of HONGGUANG directional transmissions performance4:Yb3+/Er3+Micro-crystal is preferably by following method system
For forming:
Sodium citrate is dissolved in deionized water, is then sequentially added into 0.2mol/L Y (NO3)3Aqueous solution, 0.2mol/L
Yb(NO3)3Aqueous solution and 0.2mol/L Er (NO3)3Aqueous solution, is stirred at room temperature 30 minutes, then drips 1mol/L
Sodium fluoride aqueous solution, continue stirring 20 minutes, with ammonia regulation pH value to 10, gained mixed liquor proceeds to gather
In the autoclave of tetrafluoroethene liner, at 200 DEG C, hydro-thermal reaction 24 hours, are cooled to room temperature, centrifugal,
Wash, be dried, obtain the β-NaYF with HONGGUANG directional transmissions performance4:Yb3+/Er3+Micro-crystal.
Above-mentioned Er (NO3)3、Yb(NO3)3、Y(NO3)3, sodium citrate, sodium fluoride mol ratio most preferably
1:10:39:83:1000。
The present invention uses sodium fluoride as fluorine source, has synthesized β-NaYF under alkaline environment4:Yb3+/Er3+Micro-crystal
Luminescent material, this β-NaYF4:Yb3+/Er3+Micro-crystal luminescent material has uniqueness compared with other micro-crystals
The characteristics of luminescence:
1, excite from top to bottom along the centre position at any one angle of single micro-crystal or an arc-shaped side when exciting light
Time, at β-NaYF4:Yb3+/Er3+Microcrystalline particles excite angle diagonal angle or excite limit to edge emitting HONGGUANG, real
Having showed the directional transmissions of HONGGUANG, the characteristics of luminescence of this uniqueness makes this luminescent material can apply on laser instrument, nothing
Notch filter plate is needed to can be achieved with monochromatic directional transmissions.
2, when exciting light is along the center of any one crystal in single micro-crystal central shaft or multiple micro-crystal
When axle excites from top to bottom, the luminescence process of micro-crystal seems flower process from blooming to withering, and passes through
Launch photo and be assured that the position of excitation, such that it is able to applied in bio-imaging field.
3, when exciting light along any one angle of single micro-crystal or the centre position of an arc-shaped side, multiple adjacent micro-
The central shaft of any one crystal or adjacent one jiao when exciting from top to bottom in meter Jing Ti, launch light along crystal grain
Six faces around oblate spheroid are propagated, therefore can be as waveguide modulator, for the research and development of Novel Optoelectronic Device.
Accompanying drawing explanation
Fig. 1 is the β-NaYF of embodiment 14:Yb3+/Er3+The XRD figure of micro-crystal.
Fig. 2 is the β-NaYF of embodiment 14:Yb3+/Er3+The SEM figure of micro-crystal.
Fig. 3 is the β-NaYF of embodiment 24:Yb3+/Er3+The SEM figure of micro-crystal.
Fig. 4 is the β-NaYF of embodiment 34:Yb3+/Er3+The SEM figure of micro-crystal.
Fig. 5 is the 980nm laser single β-NaYF along embodiment 14:Yb3+/Er3+Micro-crystal central shaft is from upper
Fluorescent emission photo when exciting under to.
Fig. 6 is the 980nm laser single β-NaYF along embodiment 14:Yb3+/Er3+Micro-crystal central shaft is from upper
Fluorescence emission spectrum when exciting under to.
Fig. 7 is the 980nm laser adjacent five β-NaYF along embodiment 14:Yb3+/Er3+In micro-crystal arbitrarily
Fluorescent emission photo when the central shaft of one crystal excites from top to bottom.
Fig. 8 is the 980nm laser single β-NaYF along embodiment 14:Yb3+/Er3+Any one angle of micro-crystal from
Fluorescent emission photo when exciting down.
Fig. 9 is the 980nm laser single β-NaYF along embodiment 14:Yb3+/Er3+Any one angle of micro-crystal from
Emission spectrum when exciting down.
Figure 10 is the 980nm laser single β-NaYF along embodiment 14:Yb3+/Er3+Any one arc of micro-crystal
Fluorescent emission photo when the centre position on shape limit excites from top to bottom.
Figure 11 is the 980nm laser single β-NaYF along embodiment 14:Yb3+/Er3+Any one arc of micro-crystal
The emission spectrum when centre position on shape limit excites from top to bottom.
Detailed description of the invention
The present invention is described in more detail with embodiment below in conjunction with the accompanying drawings, but protection scope of the present invention not only limits
In these embodiments.
Embodiment 1
Being joined by 0.1485g (0.5mmol) sodium citrate in the beaker filling 21mL deionized water, stirring is extremely
Sodium citrate is completely dissolved, and is then sequentially added into the Y (NO of 1.17mL 0.2mol/L in beaker3)3Aqueous solution,
Yb (the NO of 0.3mL 0.2mol/L3)3Er (the NO of aqueous solution and 0.03mL 0.2mol/L3)3Aqueous solution, room temperature
It is sufficiently stirred for 30 minutes, then in beaker, drips the sodium fluoride aqueous solution of 6mL 1mol/L, continue after dripping to stir
Mix 20 minutes, after the pH value of mixed liquor in ammonia regulation beaker to 10, mixed liquor is proceeded to 40mL poly-four
In the autoclave of fluorothene liner, at 200 DEG C, hydro-thermal reaction 24 hours, are cooled to room temperature, centrifugal, use
The alternately washing of deionized water and dehydrated alcohol, is dried 8 hours at 60 DEG C, obtains having HONGGUANG directional transmissions performance
β-NaYF4:Yb3+/Er3+Micro-crystal.
Products therefrom uses RagukuD/Max2550 (Japan) type X-ray diffractometer and Nova NanoSEM
450 (FEI) type scanning electron microscope characterizes, and result is shown in Fig. 1 and Fig. 2.As seen from Figure 1, gained produces
The X-ray diffractogram of thing and β-NaYF4Standard card (JCPDS card number: 16-0334) is consistent, shows products therefrom
For hexagonal crystal phase NaYF4:Yb3+/Er3+Micro-crystal.From Figure 2 it can be seen that gained β-NaYF4:Yb3+/Er3+Micron is brilliant
Bodily form looks are to be that the facing (being similar to the face that playground is run-track shaped) of arc is around one by about six both sides
Oblate spheroid combines, and micro-crystal size uniformity, dispersibility is the best.
Embodiment 2
Being joined by 0.1606g (0.5mmol) sodium citrate in the beaker filling 21mL deionized water, stirring is extremely
Sodium citrate is completely dissolved, and is then sequentially added into the Y (NO of 1.2mL0.2mol/L in beaker3)3Aqueous solution, 0.27
Yb (the NO of mL 0.2mol/L3)3Er (the NO of aqueous solution and 0.03mL 0.2mol/L3)3Aqueous solution, room temperature is abundant
Stir 30 minutes, then in beaker, drip the sodium fluoride aqueous solution of 6.6mL 1mol/L, after dripping, continue stirring
20 minutes, after the pH value of mixed liquor in ammonia regulation beaker to 10, mixed liquor is proceeded to 40mL polytetrafluoro
In the autoclave of ethylene liner, at 180 DEG C, hydro-thermal reaction 24 hours, are cooled to room temperature, centrifugal, spend
The alternately washing of ionized water and dehydrated alcohol, is dried 8 hours at 60 DEG C, obtains having HONGGUANG directional transmissions performance
β-NaYF4:Yb3+/Er3+Micro-crystal (see Fig. 3).
Embodiment 3
Being joined by 0.1341g (0.5mmol) sodium citrate in the beaker filling 21mL deionized water, stirring is extremely
Sodium citrate is completely dissolved, and is then sequentially added into the Y (NO of 1.1mL 0.2mol/L in beaker3)3Aqueous solution, 0.33
Yb (the NO of mL 0.2mol/L3)3Er (the NO of aqueous solution and 0.03mL 0.2mol/L3)3Aqueous solution, room temperature is abundant
Stir 30 minutes, then in beaker, drip the sodium fluoride aqueous solution of 5.7mL 1mol/L, after dripping, continue stirring
20 minutes, after the pH value of mixed liquor in ammonia regulation beaker to 10, mixed liquor is proceeded to 40mL polytetrafluoro
In the autoclave of ethylene liner, at 220 DEG C, hydro-thermal reaction 12 hours, are cooled to room temperature, centrifugal, spend
The alternately washing of ionized water and dehydrated alcohol, is dried 8 hours at 60 DEG C, obtains having HONGGUANG directional transmissions performance
β-NaYF4:Yb3+/Er3+Micro-crystal (see Fig. 4).
In order to prove beneficial effect of the present invention, the shape β-NaYF that embodiment 1 is prepared by inventor4:Yb3+/Er3+Micron
The fluorescent emission performance of crystal is studied, and specific experiment situation is as follows:
Take 10mg β-NaYF4:Yb3+/Er3+Micro-crystal adds in 4mL deionized water, ultrasonic disperse 30 minutes,
Sol evenning machine is used to be spin-coated on microscope slide by gained dispersion liquid, at exciting power, ambient temperature, light path (light path warp
Cross microscope), slit width, spectrum integral time the most constant in the case of, use Laser Scanning Confocal Microscope
(OLYMPUS-BX51) single β-NaYF on microscope slide is found in observation4:Yb3+/Er3+Microcrystalline particles, adopts
With LAB 170 type Nd:YAG (Spectra-Physics) pulse laser and Mira 900-F type femto-second laser
(CohErent) output 980nm laser, by finely tuning the position of laser focusing so that it is along single crystal grain
Central shaft excite from top to bottom, it is thus achieved that fluorescent emission photo as shown in Figure 5, the emission spectrum of its correspondence is shown in figure
6.As can be seen from Figure 5, during excitation position from top to bottom changes, β-NaYF4:Yb3+/Er3+
The luminescence process of microcrystalline particles is like process from blooming to withering of flower, and wherein a-e is what The flowers bloom luxuriantly
Process, f-l is the process that flower withers.As seen from Figure 6, the process from top to bottom changed in excitation position
In, β-NaYF4:Yb3+/Er3+The luminous intensity first increases and then decreases of microcrystalline particles, the most first increases and subtracts afterwards
Little, and green intensity is apparently higher than red light intensity.
According to the method described above, with 980nm laser along adjacent five β-NaYF4:Yb3+/Er3+In micro-crystal arbitrarily
The central shaft of one crystal excites from top to bottom, obtains fluorescent emission photo as shown in Figure 7.Can from Fig. 7
Go out, along with the position of excitation from top to bottom changes, β-NaYF4:Yb3+/Er3+The luminescence of microcrystalline particles
Not only like flower process from blooming to withering, (wherein a-e is the process that The flowers bloom luxuriantly to process, and f-i is that flower withers
Process), and not by the crystal grain of laser excitation, relative with the micro-crystal adjacent surface excited
The luminous intensity in individual face is the strongest, illustrates to launch just along crystal grain around the six of oblate spheroid face propagation.
According to the method described above, with 980nm laser along single β-NaYF4:Yb3+/Er+Any one angle in micro-crystal
Exciting from top to bottom, obtain fluorescent emission photo as shown in Figure 8, the emission spectrum of its correspondence is shown in Fig. 9.From figure
Can be seen that in 8, along with the position of excitation from top to bottom changes, at β-NaYF4:Yb3+/Er3+Micro-crystal
HONGGUANG is launched at the diagonal angle at particle excitation angle.Halfwidth according to the luminous intensity in Fig. 9 and emission peak is visible,
β-NaYF4:Yb3+/Er3+The HONGGUANG that microcrystalline particles is launched is better than green glow.As can be seen here, swash with 980nm laser
Bill β-NaYF4:Yb3+/Er3+Any one angle of microcrystalline particles is capable of the directional transmissions of HONGGUANG.
According to the method described above, with 980nm laser along single β-NaYF4:Yb3+/Er3+Any one arc in micro-crystal
The centre position on shape limit excites from top to bottom, obtains fluorescent emission photo as shown in Figure 10, the transmitting of its correspondence
Spectrum is shown in Figure 11.As can be seen from Figure 10, along with the position of excitation from top to bottom changes, at β-NaYF4:
Yb3+/Er3+Microcrystalline particles excite limit to edge emitting HONGGUANG.According to the luminous intensity in Figure 11 and emission peak
Halfwidth is visible, β-NaYF4:Yb3+/Er3+The HONGGUANG that microcrystalline particles is launched is better than green glow.As can be seen here, use
980nm laser excitation single β-NaYF4:Yb3+/Er3+The centre position energy of any one arc-shaped side of microcrystalline particles
Enough realize the directional transmissions of HONGGUANG.
Claims (3)
1. a β-NaYF with HONGGUANG directional transmissions performance4:Yb3+/Er3+Micro-crystal, it is characterised in that should
Micro-crystal is prepared from by following method: be dissolved in deionized water by sodium citrate, is then sequentially added into 0.2mol/L
Y(NO3)3Aqueous solution, 0.2mol/L Yb (NO3)3Aqueous solution and 0.2mol/L Er (NO3)3Aqueous solution, is stirred at room temperature
20～40 minutes, then drip the sodium fluoride aqueous solution of 1mol/L, continue stirring 15～30 minutes, adjust with ammonia
Joint pH value is to 9～11, and gained mixed liquor proceeds in teflon-lined autoclave, at 180～220 DEG C
Lower hydro-thermal reaction 18～24 hours, be cooled to room temperature, is centrifuged, washs, is dried, and obtains having HONGGUANG orientation and sends out
Penetrate the β-NaYF of performance4:Yb3+/Er3+Micro-crystal, wherein Er (NO3)3、Yb(NO3)3、Y(NO3)3, Fructus Citri Limoniae
Acid sodium, the mol ratio of sodium fluoride are 1:9～11:37～40:73～95:900～1100.
β-the NaYF with HONGGUANG directional transmissions performance the most according to claim 14:Yb3+/Er3+Micron is brilliant
Body, it is characterised in that: sodium citrate is dissolved in deionized water, is then sequentially added into 0.2mol/L Y (NO3)3Water
Solution, 0.2mol/L Yb (NO3)3Aqueous solution and 0.2mol/L Er (NO3)3Aqueous solution, is stirred at room temperature 30 minutes,
Then drip the sodium fluoride aqueous solution of 1mol/L, continue stirring 20 minutes, with ammonia regulation pH value to 10, institute
Obtain mixed liquor and proceed in teflon-lined autoclave, hydro-thermal reaction 24 hours at 200 DEG C, cooling
To room temperature, it is centrifuged, washs, is dried, obtain the β-NaYF with HONGGUANG directional transmissions performance4:Yb3+/Er3+Micron
Crystal.
β-the NaYF with HONGGUANG directional transmissions performance the most according to claim 24:Yb3+/Er3+Micron is brilliant
Body, it is characterised in that: described Er (NO3)3、Yb(NO3)3、Y(NO3)3, sodium citrate, the rubbing of sodium fluoride
That ratio is 1:10:39:83:1000.
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| CN109913218A (en) * | 2019-03-15 | 2019-06-21 | 湖北文理学院 | A kind of micron order hexagonal phase NaYF4Up-conversion and its quick preparation process |
| CN109913218B (en) * | 2019-03-15 | 2020-10-20 | 湖北文理学院 | Micron-sized hexagonal phase NaYF4Up-conversion material and rapid preparation process thereof |
| CN113897198A (en) * | 2021-10-21 | 2022-01-07 | 西安邮电大学 | Flower-shaped beta-NaYF with adjustable red light intensity and green light intensity4:Yb3+/Er3+Hexagonal prism micron crystal luminescent material |
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