CN108822850A - A kind of GdF3:Yb3+,Er3+The preparation method of up-conversion fluorescence nanometer rods - Google Patents
A kind of GdF3:Yb3+,Er3+The preparation method of up-conversion fluorescence nanometer rods Download PDFInfo
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Abstract
The invention discloses a kind of GdF3:Yb3+,Er3+The preparation method of up-conversion fluorescence nanometer rods, steps are as follows：A. by sodium hydroxide, oleic acid and dehydrated alcohol mixing, the viscous solution of white is generated；B. by NH4F solution is added while stirring to above-mentioned solution, until forming translucent solution；C. respectively by Gd (NO3)3·6H2O、Yb(NO3)3·5H2O、Er(NO3)3·5H2Above-mentioned translucent solution is added while stirring and continues to stir for O solution；D. step c is prepared liquid to be transferred in polytetrafluoroethylene (PTFE) hydro-thermal autoclave, continuous heating under high temperature；E. cooling to reaction kettle, centrifugation washs precipitating with hexamethylene and dehydrated alcohol, and precipitating is dissolved in hexamethylene；F. step e acquired solution is centrifuged, drying.The present invention enriches the structure and drug loading space of nanoparticle, provides theoretical and experimental basis for the building of further probe and anticancer drug targeted delivery.
Description
Technical field
The present invention relates to field of light emitting materials, specifically a kind of GdF3:Yb3+,Er3+The preparation side of up-conversion fluorescence nanometer rods
Method.
Background technique
Rear-earth-doped up-conversion luminescence nanoparticle (UCNPs) is that one kind can absorb long wavelength's near-infrared photon and emit
The advanced luminescent material of short wavelength UV optical photon.With the down-conversion fluorescents material such as traditional organic dyestuff, semiconductor-quantum-point
Material is compared, and UCNPs is high with chemical stability, bio-toxicity is low, photostability is strong, transmitting band is narrow, fluorescence lifetime is long, unglazed
The advantages that flashing and photobleaching.Moreover, since the excitation wavelength of UCNPs is located at low energy near infrared region, to biological tissue
It damages small and there is deeper tissue penetration, therefore, in field of biomedicine, especially in the Clinics and Practices field table of cancer
Reveal great application prospect.Currently, people are in the control synthesis of up-conversion luminescence nanoparticle, cell marking, living body
Many fields such as the treatment of cancer under imaging, optical dynamic therapy and imaging guidance expand a series of in-depth studies and spy
Rope.
UCNPs is usually made of host material, activator and sensitizer.Host material is mainly that active ions offer is suitble to
Crystalline field, itself will not shine.Currently used host material mainly has oxide, fluoride and sulfide etc..Wherein fluorine
The features such as compound is due to its lower phonon energy, biggish forbidden bandwidth becomes most common host material.It is commonly used for activating
The rare earth element of agent has：Er3+、Tm3+、Ho3+、Eu3+Deng, activator determines the light that conversion nano particle is emitted, such as adulterate
Er3+Green light, doping Tm3+Blue light-emitting, doping Ho3+It glows, wherein Er3+It, can because having the intermediate state energy level lasted a long time
Become the activator of most study with the realization up-conversion luminescence of two or more photons of continuous absorption.Rare earth element y b3+Then
Since excitation wavelength is 980nm and absorption cross-section is big, it is presently the most common and most effective upwards converitng sensitization agent.
There are many preparation method of UCNPs, mainly include coprecipitation, sol-gel method, high temperature thermal decomposition method, hydro-thermal/
Solvent-thermal method, microemulsion method and is waited.Wherein hydro-thermal method can preferably control the size and shape of conversion nano particle, be to answer
With one of widest method.Hydro-thermal method is dissolved and is recrystallized using water as solvent, powder in the pressure vessel of sealing
The method for preparing material.The prominent advantage of this method is that required temperature is lower, to the rare-earth salts used in the process of synthesis
Purity requirement it is relatively low, the generating process of material is easy to control, and the material crystal phase of synthesis is good, uniform particle sizes and products collection efficiency
It is high.Up to the present, scientists have successfully synthesized a variety of up-conversions using this method.In hydrothermal synthesis process
In, the stabilizer of selection, the factors such as ratio, concentration, pH value, synthesis temperature of various raw material can all influence the crystalline substance of nano particle
Type, shape and size.
Up to the present, the research of spherical nanoparticle is more mature, but aspherical nano particle is rarely reported.Aspheric
Shape structure shows apparent superiority in terms of biomedical applications：
First, shape all influences the mechanism of drug release in many aspects, and the degradation and drug for influencing polymer such as it are released
Put dynamics.Adjust the mechanism for carrying the adjustable drug release of shape of medicine particle, it might even be possible to avoid burst release.With planar shaped
Zero order release may be implemented in the aspheric particle of shape, and particle with different thickness can be continuous due to its shape in degradation process
Change, so having unique degradation mode.
Second, shape has an effect on the internal transmission and circulation of polymer particle.Such as:It is compared with spheroidal particle, it is elongated
Particle is easier with fluid motion, therefore they can more be moved smoothly through in curved organ and tissue.The blood platelet of people
Also there is its unique shape with red blood cell, spheroidal particle diameter is less than 200nm could be by spleen, but diameter is at 10 μm or so
Discoid flexible red blood cell can be but filtered in spleen to avoid it.
Third, the shape of particle and local curvature also will affect its targeting ability, when the medicament transport wrapped up to spy
The receptor that targeting group is connected to cell membrane is influenced when fixed cell.Having had been reported that in nearest document proves aspherical grain
Son is more suitable for internal drug targeting than spheroidal particle:By the spherical grain of the different-diameter accumulated in target tissue (100nm-10 μm)
The oval plate-like particle of son and microsize (1 3 μm of μ m) compares, and finds the targeting efficiency ratio of the discoid particle of micron-scale
All high [Muro S, Garnacho C, Champion J A, the et al.Control of the targeting efficiency of any size spheroidal particle
of endothelial targeting and intracellular delivery of therapeutic enzymes by
modulating the size and shape of ICAM-1-targeted carriers.[J].Molecular
Therapy,2008,16(8):1450]。
4th, the shape of particle and the local shape of binding site will affect its rate being phagocytized by cells.By non-phagocytosis
Cell endocytic also has relationship with shape, and the nonspherical particle of high aspect ratio is the 4 of same volume spheroidal particle by the rate of endocytosis
Times.
5th, shape also has important influence to adhesion of the particle on cell membrane.Due to rod-shaped particle complexity
Hydrodynamic and their torque make it be easier to flow towards barrier than spheroidal particle.This illustrates spherical carriers than spherical
Carrier is easier to be attached on cell membrane.
6th, the shape that polymeric therapeutic drug also relies on particle is discharged by degrading.Therefore, it can prepare
The nonspherical particle of specific shape can greatly improve interior curative effect as pharmaceutical carrier.
7th, pass through diffusion of the technique study of the experiment nano particle of different shapes in your at dark night, the results showed that, stick
Shape particle presents diffusion velocity more faster than spheric granules.
It can be seen that aspherical nano particle not only increase can carrying medicament surface area, also drug release, in vivo
Transmission, circulation target ability, by the adhesion on the rate of macrophage endocytosis, cell membrane and in stomach and intestine mucus
Diffusion etc. is many-sided all to show more superior performance than corresponding spheroidal particle.
Moreover, nanometer stick array structure can provide direct channel as electron transfer layer for the transmission of electronics,
To improve migration distance of the electronics in electron transfer layer, recombination rate of the electronics in electron transfer layer is reduced.This array
Structure in terms of solar battery using relatively conventional.In recent years, there are also document report club shaped structure nano particles to close red
The absorption of outer light is also greatly improved compared with spheric granules.
This seminar submits on May 25th, 2017 to State Intellectual Property Office entitled：A kind of GdF3:Yb3+,
Er3+The preparation method of upconversion fluorescence nano material, application No. is 2017103774262 Chinese invention patent applications, this is specially
A kind of GdF of mercaptopropionic acid modification is successfully prepared in benefit application using one step hydro thermal method3:Yb3+,Er3+Up-conversion fluorescence nanometer material
Material.This one step hydro thermal method solves up-conversion nanoparticles preparation and the complicated for operation, higher cost of surface modification two-step method etc.
Problem, the upper conversion nano particle prepared also show stronger Green upconversion luminescent.Based on foregoing invention patent application
Documented synthetic method, this seminar now propose a kind of rodlike GdF3:Yb3+,Er3+The preparation method of up-conversion nanoparticles.
Summary of the invention
The present invention proposes a kind of GdF by improving hydro-thermal method3:Yb3+,Er3+The preparation side of up-conversion fluorescence nanometer rods
Method.
Present invention employs the following technical solutions.
A kind of GdF3:Yb3+,Er3+The preparation method of up-conversion fluorescence nanometer rods, includes the following steps：
A. sodium hydroxide, oleic acid and ethanol solution are mixed, magnetic agitation 10-20 minutes, until it is viscous to generate white
Solution；
B. NH is weighed4F solid prepares solution, is added in the mixed solution that step a is obtained under magnetic agitation, continues magnetic force
Obtain the translucent solution of milky within stir about 10-20 minutes；
C. Gd (NO is weighed respectively3)3·6H2O、Yb(NO3)3·5H2O、Er(NO3)3·5H2O powder prepares solution, magnetic force
It is added with stirring in the mixed solution that step b is obtained, continues magnetic agitation about 10-30 minutes to being completely dissolved；
D. the white suspension prepared by step c is transferred in polytetrafluoroethylene (PTFE) hydro-thermal autoclave, at 160-230 DEG C
Lower continuous heating 8-20 hours；
E. it is cooled to room temperature to polytetrafluoroethylene (PTFE) high-pressure hydrothermal reaction kettle, 2000-3000rpm is centrifuged 2-3 minutes, is used respectively
Alternately washing precipitates for hexamethylene and dehydrated alcohol, will finally be precipitated and dissolved in hexamethylene；
F. step e acquired solution 2000-3000rpm is centrifuged 2-3 minutes, obtains white precipitate and is dried, after dry
White solid powder is GdF3:Yb3+,Er3+Up-conversion fluorescence nanometer rods.
Further, the ratio between the sodium hydroxide in step a and the amount of substance of gadolinium ion in step c are 15:1-30:1.
Further, the ratio between the ammonium fluoride in step b and the amount of substance of total rare earth (TRE) ion in step c are 4:1.
Further, the ratio between amount of substance of gadolinium ion, ytterbium ion and erbium ion is 65 in the step c:30:5-79:
20:1。
Further, the ratio between amount of substance of gadolinium ion, ytterbium ion and erbium ion is 78 in the step c:20:2.
Further, GdF in the step f3:Yb3+,Er3+The aspect ratio of up-conversion fluorescence nanometer rods is 1:3-1:5.
Present invention obtains following beneficial effects.
The present invention improves one step hydro thermal method, using oleic acid as surface stabilizer, passes through control sodium hydroxide and fluorine
Change ammonia amount and with the substance of rare earth ion than etc. conditions achieve the purpose that change nano particle size and pattern, to close
At GdF3:Yb3+,Er3+Up-conversion fluorescence nanometer rods, and obtaining aspect ratio is 1:3~1:5 relatively regular nanometer rods knot
Structure.The luminescent material uniform particle diameter, dispersibility is preferable, and fluorescence intensity is strong.Biggish surface area is also further connection drug
Or targeting substance provides bigger load area.In addition, present invention application hydro-thermal method synthesizes, there is easy to operate, technique stream
The advantages that journey is short, cost is more cheap has in terms of the Clinics and Practices of cell multi-modality imaging, cancer and other major diseases
There is extensive clinical value.
Detailed description of the invention
Fig. 1 is GdF prepared by the embodiment of the present invention 13:20%Yb3+, 2%Er3+Up-conversion fluorescence nanometer rods transmission electron microscope shines
Piece；
Fig. 2 is GdF prepared by the embodiment of the present invention 13:20%Yb3+, 2%Er3+Up-conversion fluorescence nanometer rods scanning electron microscope is shone
Piece；
Fig. 3 is GdF prepared by the embodiment of the present invention 1 under 980nm laser irradiation3:20%Yb3+, 2%Er3+Upper conversion is glimmering
Light spectrogram；
Fig. 4 is GdF prepared by the embodiment of the present invention 23:30%Yb3+, 5%Er3+Up-conversion fluorescence nanometer rods transmission electron microscope shines
Piece；
Fig. 5 is GdF prepared by the embodiment of the present invention 2 under 980nm laser irradiation3:30%Yb3+, 5%Er3+Upper conversion is glimmering
Light spectrogram；
Fig. 6 is GdF prepared by the embodiment of the present invention 33:20%Yb3+, 1%Er3+Up-conversion fluorescence nanometer rods transmission electron microscope shines
Piece；
Fig. 7 is GdF prepared by the embodiment of the present invention 3 under 980nm laser irradiation3:20%Yb3+, 1%Er3+Upper conversion is glimmering
Light spectrogram.
Specific embodiment
Referring to the drawings and the present invention is further detailed in embodiment.
Embodiment 1
A kind of GdF3:20%Yb3+, 2%Er3+One step hydrothermal synthesis method of up-conversion fluorescence nanometer rods, includes the following steps：
A. by 0.7g sodium hydroxide, 7.95mL oleic acid and 12.66mL dehydrated alcohol as in 50mL plastic beaker, magnetic force is stirred
It mixes 20 minutes, mixes well it, until generating the viscous solution of white；
B. 0.2146g NH is weighed4F solid prepares 10mL aqueous solution, 8.3mL is added under magnetic agitation and obtains in step a
Mixed solution in, continue to obtain the translucent solution of milky in magnetic agitation about 20 minutes；
C. Gd (NO is weighed3)3·6H2O、Yb(NO3)3·5H2O、Er(NO3)3·5H2O powder, prepare respectively 0.80M,
The aqueous solution of 0.63M, 0.40M take under magnetic agitation 1.1mL, 0.35mL, 0.05mL that the mixing that step b is obtained is added molten respectively
In liquid, continue magnetic agitation about 20 minutes to being completely dissolved；
D. the white suspension prepared by step c is transferred in polytetrafluoroethylene (PTFE) hydro-thermal autoclave, is held at 180 DEG C
Continuous heating 12 hours；
E. it is cooled to room temperature to polytetrafluoroethylene (PTFE) high-pressure hydrothermal reaction kettle, 2000-3000rpm is centrifuged 3 minutes, uses ring respectively
Alternately washing precipitates for hexane and dehydrated alcohol, will finally be precipitated and dissolved in hexamethylene；
F. step e acquired solution 2000-3000rpm is centrifuged 3 minutes, obtains white precipitate and is dried, it is white after drying
Color solid powder is GdF3:20%Yb3+, 2%Er3+Up-conversion fluorescence nanometer rods.
The GdF that the present embodiment is prepared3:20%Yb3+, 2%Er3+TEM photo as shown in Figure 1, nanoparticle be in stick
Shape structure, diameter about 40nm, length about 150nm, dispersibility is preferably.Fig. 2 is GdF3:20%Yb3+, 2%Er3+The SEM of nanometer rods
Photo, as shown, the cross section of nanometer rods is regular hexagon, nano particle is in six prismatics.It is excited in 980nm near-infrared
Under, GdF3:20%Yb3+, 2%Er3+Up-conversion fluorescence spectrogram as shown in figure 3, in 405-433nm, 515-599nm and
There are three up-conversion fluorescence peaks, respectively blue, green and red emission band at 654-677nm, correspond to Er ion2H9/2—4I15/2、2H11/2,4S3/2—4I15/2、4F9/2—4I15/2Energy level transition, wherein green emitted peak intensity is most strong, and red
Emission peak is most weak, and green emitted peak is about 8 times of blue emission peak, is 13 times or so of red emission peak.
Embodiment 2
A kind of GdF3:30%Yb3+, 5%Er3+One step hydrothermal synthesis method of up-conversion fluorescence nanometer rods, includes the following steps：
A. by 0.7g sodium hydroxide, 7.95mL oleic acid and 12.66mL dehydrated alcohol as in 50mL plastic beaker, magnetic force is stirred
It mixes 20 minutes, mixes well it, until generating thick white solution；
B. 0.2146g NH is weighed4F solid prepares 10mL aqueous solution, 8.3mL is added under magnetic agitation and obtains in step a
Mixed solution in, continue to obtain the translucent solution of milky in magnetic agitation about 20 minutes；
C. Gd (NO is weighed3)3·6H2O、Yb(NO3)3·5H2O、Er(NO3)3·5H2O powder, prepare respectively 0.71M,
The aqueous solution of 1.03M, 1.20M take under magnetic agitation 1.1mL, 0.35mL, 0.05mL that the mixing that step b is obtained is added molten respectively
In liquid, continue magnetic agitation about 20 minutes to being completely dissolved；
D. the white suspension prepared by step c is transferred in polytetrafluoroethylene (PTFE) hydro-thermal autoclave, is held at 180 DEG C
Continuous heating 12 hours；
E. it is cooled to room temperature to polytetrafluoroethylene (PTFE) high-pressure hydrothermal reaction kettle, 2000-3000rpm is centrifuged 3 minutes, uses ring respectively
Alternately washing precipitates for hexane and dehydrated alcohol, will finally be precipitated and dissolved in hexamethylene；
F. step e acquired solution 2000-3000rpm is centrifuged 3 minutes, obtains white precipitate and is dried, it is white after drying
Color solid powder is GdF3:30%Yb3+, 5%Er3+Up-conversion fluorescence nanometer rods.
The GdF that the present embodiment is prepared3:30%Yb3+, 5%Er3+TEM photo as shown in figure 4, nanoparticle be in six
Angle disk-like structure, diameter about 100-200nm, thickness about 40nm, dispersibility is preferably.Under the excitation of 980nm near-infrared, GdF3:
30%Yb3+, 5%Er3+Up-conversion fluorescence spectrogram as shown in figure 5, there are two at 515-599nm and 654-677nm
Up-conversion fluorescence peak, respectively green and red emission band, correspond to Er ion2H11/2,4S3/2—4I15/2、4F9/2—4I15/2's
Energy level transition, wherein green emitted peak intensity is stronger, about 16 of red emission peak times or so.
Embodiment 3
A kind of GdF3:20%Yb3+, 1%Er3+One step hydrothermal synthesis method of up-conversion fluorescence nanometer rods, includes the following steps：
A. by 0.7g sodium hydroxide, 7.95mL oleic acid and 12.66mL dehydrated alcohol as in 50mL plastic beaker, magnetic force is stirred
It mixes 20 minutes, mixes well it, until generating thick white solution；
B. 0.2146g NH is weighed4F solid prepares 10mL aqueous solution, 8.3mL is added under magnetic agitation and obtains in step a
Mixed solution in, continue to obtain the translucent solution of milky in magnetic agitation about 20 minutes；
C. Gd (NO is weighed3)3·6H2O、Yb(NO3)3·5H2O、Er(NO3)3·5H2O powder, prepare respectively 0.86M,
The aqueous solution of 0.69M, 0.24M take under magnetic agitation 1.1mL, 0.35mL, 0.05mL that the mixing that step b is obtained is added molten respectively
In liquid, continue magnetic agitation about 20 minutes to being completely dissolved；
D. the white suspension prepared by step c is transferred in polytetrafluoroethylene (PTFE) hydro-thermal autoclave, is held at 180 DEG C
Continuous heating 12 hours；
E. it is cooled to room temperature to polytetrafluoroethylene (PTFE) high-pressure hydrothermal reaction kettle, 2000-3000rpm is centrifuged 3 minutes, uses ring respectively
Alternately washing precipitates for hexane and dehydrated alcohol, will finally be precipitated and dissolved in hexamethylene；
F. step e acquired solution 2000-3000rpm is centrifuged 3 minutes, obtains white precipitate and is dried, it is white after drying
Color solid powder is GdF3:20%Yb3+, 1%Er3+Up-conversion fluorescence nanometer rods.
The GdF that the present embodiment is prepared3:20%Yb3+, 1%Er3+TEM photo as shown in fig. 6, nanoparticle be in stick
Shape structure, diameter about 100-200nm, thickness about 40nm, dispersibility is preferably.Under the excitation of 980nm near-infrared, GdF3:20%Yb3 +, 1%Er3+Up-conversion fluorescence spectrogram as shown in fig. 7, there are two upper conversions at 515-599nm and 654-677nm
Fluorescence peak, respectively green and red emission band, correspond to Er ion2H11/2,4S3/2—4I15/2、4F9/2—4I15/2Energy level jump
It moves, wherein green emitted peak intensity is stronger, and red emission peak is compared with GdF3:30%Yb3+, 5%Er3+And GdF3:20%Yb3+, 2%
Er3+Enhanced, green emitted peak intensity is about 7 times of red emission peak or so.
Claims (6)
1. a kind of GdF3:Yb3+,Er3+The preparation method of up-conversion fluorescence nanometer rods, it is characterised in that：Include the following steps：
A. sodium hydroxide, oleic acid and ethanol solution are mixed, magnetic agitation 10-20 minutes, until generating the viscous solution of white；
B. NH is weighed4F solid prepares solution, is added in the mixed solution that step a is obtained under magnetic agitation, continues magnetic agitation about
Obtain within 10-20 minutes the translucent solution of milky；
C. Gd (NO is weighed respectively3)3·6H2O、Yb(NO3)3·5H2O、Er(NO3)3·5H2O powder prepares solution, magnetic agitation
In the mixed solution that lower addition step b is obtained, continue magnetic agitation about 10-30 minutes to being completely dissolved；
D. the white suspension prepared by step c is transferred in polytetrafluoroethylene (PTFE) hydro-thermal autoclave, is held at 160-230 DEG C
Continuous heating 8-20 hours；
E. it is cooled to room temperature to polytetrafluoroethylene (PTFE) high-pressure hydrothermal reaction kettle, 2000-3000rpm is centrifuged 2-3 minutes, uses hexamethylene respectively
Alternately washing precipitates for alkane and dehydrated alcohol, will finally be precipitated and dissolved in hexamethylene；
F. step e acquired solution 2000-3000rpm is centrifuged 2-3 minutes, obtains white precipitate and is dried, the white after drying
Solid powder is GdF3:Yb3+,Er3+Up-conversion fluorescence nanometer rods.
2. a kind of GdF according to claim 13:Yb3+,Er3+The preparation method of up-conversion fluorescence nanometer rods, feature exist
In：The ratio between the amount of substance of gadolinium ion in sodium hydroxide and step c in step a is 15:1-30:1.
3. a kind of GdF according to claim 13:Yb3+,Er3+The preparation method of up-conversion fluorescence nanometer rods, feature exist
In：The ratio between the amount of substance of total rare earth (TRE) ion in ammonium fluoride and step c in step b is 4:1.
4. a kind of GdF according to claim 13:Yb3+,Er3+The preparation method of up-conversion fluorescence nanometer rods, feature exist
In：The ratio between amount of substance of gadolinium ion, ytterbium ion and erbium ion is 65 in the step c:30:5-79:20:1.
5. a kind of GdF according to claim 43:Yb3+,Er3+The preparation method of up-conversion fluorescence nanometer rods, feature exist
In：The ratio between amount of substance of gadolinium ion, ytterbium ion and erbium ion is 78 in the step c:20:2.
6. a kind of GdF according to claim 13:Yb3+,Er3+The preparation method of up-conversion fluorescence nanometer rods, feature exist
In：GdF in the step f3:Yb3+,Er3+The aspect ratio of up-conversion fluorescence nanometer rods is 1:3-1:5.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286287A (en) * | 2011-09-15 | 2011-12-21 | 长春理工大学 | Europium ion doped gadolinium sodium tetrafluoride luminescent nano rod and preparation method thereof |
| WO2013112856A2 (en) * | 2012-01-26 | 2013-08-01 | The Regents Of The University Of Colorado, A Body Corporate | Multifunctional nanomaterials for the treatment of cancer |
| CN107033908A (en) * | 2017-05-25 | 2017-08-11 | 天津医科大学 | A kind of GdF3:Yb3+,Er3+The preparation method of upconversion fluorescence nano material |
-
2018
- 2018-08-01 CN CN201810862885.4A patent/CN108822850A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286287A (en) * | 2011-09-15 | 2011-12-21 | 长春理工大学 | Europium ion doped gadolinium sodium tetrafluoride luminescent nano rod and preparation method thereof |
| WO2013112856A2 (en) * | 2012-01-26 | 2013-08-01 | The Regents Of The University Of Colorado, A Body Corporate | Multifunctional nanomaterials for the treatment of cancer |
| CN107033908A (en) * | 2017-05-25 | 2017-08-11 | 天津医科大学 | A kind of GdF3:Yb3+,Er3+The preparation method of upconversion fluorescence nano material |
Non-Patent Citations (1)
| Title |
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Application publication date: 20181116 |