CN106590659A - Highly doped rare earth up-conversion fluorescent nano material and preparation method thereof - Google Patents
Highly doped rare earth up-conversion fluorescent nano material and preparation method thereof Download PDFInfo
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- CN106590659A CN106590659A CN201611177064.4A CN201611177064A CN106590659A CN 106590659 A CN106590659 A CN 106590659A CN 201611177064 A CN201611177064 A CN 201611177064A CN 106590659 A CN106590659 A CN 106590659A
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- 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
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Abstract
The invention provides a highly doped rare earth up-conversion fluorescent nano material. The highly doped rare earth up-conversion fluorescent nano material consists of rare earth ions-doped up-conversion nano-particles serving as a nuclear structure and a shell structure which coats the nuclear structure; the doping concentration of rare earth ions is greater than 5 percent. According to the highly doped rare earth up-conversion fluorescent nano material, the quenching concentration of the doped rare earth ions is improved by utilizing the shell layer, and the cross relaxation of the doped rare earth ions is reduced, so that the light intensity of the up-conversion nano-particles is further improved through a mode of effectively increasing the doping concentration of the rare earth ions in a light emitting centre. On the other hand, the emission intensity of each energy level of the rare earth ions can be effectively regulated by utilizing the strong cross relaxation produced by high doping; therefore, controllable multi-colour light emitting of the highly doped rare earth up-conversion fluorescent nano material is realized.
Description
Technical field
The present invention relates to luminescent material technical field, more particularly to a kind of highly doped rare earth up-conversion fluorescent nano material and
Its preparation method.
Background technology
Rear-earth-doped upconverting fluorescent material be it is a kind of using lanthanide ion doping, by near infrared light be converted into visible ray with
The fluorescent material of ultraviolet light.It is in Solar use, data storage, three dimensional display and imaging in biological tissues and detection and medicine
The field such as transport all to have a wide range of applications.By taking biological detection direction as an example, with traditional organic fluorescent dye or quasiconductor amount
Son point is compared, and rear-earth-doped up-conversion has toxicity low, and chemical stability is high, unglazed bleaching phenomenon, life time of the level length etc.
Advantage.More because its excitation wavelength is can be located within " optical window " of human body, penetration depth height (cm magnitudes) to tissue,
And its transmitting interference of optical signal without background fluorescence, and glow color is adjustable, therefore be widely used in complex system
The multicolor fluorescence marker detection carried out in (such as human body, whole blood), its Monitoring lower-cut is up to 10-9Mol/ml magnitudes, are a kind of property
The excellent fluorescence labeling material of energy.
But rear-earth-doped upconverting fluorescent material is in the further application in above-mentioned field, all by the problem of an essence
Govern --- i.e. its luminous efficiency is too low, and luminous intensity is inadequate.With efficiency highest hexagonal phase NaYF4:Yb3+,Er3+It is co-doped with receiving
As a example by rice corpuscles, in 150W/cm2980nm laser excitations under, generally only 0.3% or so upper conversion efficiency.Therefore improve
Its luminous efficiency, luminous intensity are a problem demanding prompt solutions.
Obviously, the doping content for improving nanoparticle Rare Earth Ion is expected to improve its luminous intensity, but we note that
Arrive, at present in actual applications, doping content of the rare earth ion in substrate is still in relatively low level, is typically only 2%
～5%, this is to be easy to strong cross relaxation and concentration quenching effect between rare earth ion due to high-dopant concentration, is led
High doping content is caused generally all to cause the reduction of luminous intensity on the contrary.Although having document report recently in very high power density
(106W/cm2) excite down, or (the KYb in special matrix structure2F7), the quenching concentration of rare earth ion can be obtained greatly
Improve, but these methods still enjoy restriction in practicality and universality, so, find a kind of pervasive method to improve
The quenching upper limit of doping concentration of rare earth ion, is very important actual demand.
The content of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of highly doped rare earth up-conversion fluorescent nanometer material
Material and preparation method thereof, the rare earth up-conversion fluorescent nano material of preparation have higher doping concentration of rare earth ion, while tool
There is higher luminous efficiency.
The invention provides a kind of highly doped rare earth up-conversion fluorescent nano material, is received by the upper conversion of doping with rare-earth ions
Rice corpuscles are used as nuclear structure, and the shell structure composition of cladding nuclear structure；
The doping content of the rare earth ion is more than 5%.
In some embodiments of the invention, the doping content of the rare earth ion is 10%～100%.
In some embodiments of the invention, the doping content of the rare earth ion is 10%～80%.
In some embodiments of the invention, the up-conversion nanoparticles are with NaYF4For substrate.
In some embodiments of the invention, the rare earth ion is Er3+、Tm3+Or Ho3+。
In some embodiments of the invention, the shell structure is with NaYF4For substrate.
In some embodiments of the invention, the shell structure thickness is 2～5nm.
Present invention also offers the preparation method of above-mentioned highly doped rare earth up-conversion fluorescent nano material, including following step
Suddenly：
A the up-conversion nanoparticles of doping with rare-earth ions) are prepared；
B) to step A) nanoparticle that obtains carries out shell cladding.
In some embodiments of the invention, step A) preparation method be chloride-Oleic acid predecessor method
Or trifluoroacetate decomposition method.
In some embodiments of the invention, step B) it is specially：
By step A) nanoparticle for preparing is added in inertia husk as raw material, and 300 DEG C～330 DEG C temperature reactions of Jing are formed
Nanoparticle with nucleocapsid structure.
Compared with prior art, the invention provides a kind of highly doped rare earth up-conversion fluorescent nano material, dilute by adulterating
The up-conversion nanoparticles of native ion are used as nuclear structure, and the shell structure composition of cladding nuclear structure；The doping of the rare earth ion
Concentration is more than 5%.The present invention improves the quenching concentration of doping with rare-earth ions using shell, reduces its cross relaxation and acts on, and then
Up-conversion nanoparticles luminous strong is improved by way of being effectively increased centre of luminescence doping concentration of rare earth ion further
Degree.On the other hand, using highly doped produced strong cross relaxation effect, each energy level of rare earth ion can effectively be adjusted
Emissive porwer, so as to realize which is controllable multicolor luminous.
Description of the drawings
Fig. 1 is the transmission electron microscope figure of bare nucleus up-conversion nanoparticles prepared by embodiment 1；
Fig. 2 is different Er under 980nm laser excitations3+The fluorescence spectra of the bare nucleus up-conversion nanoparticles of doping content；
Fig. 3 is the transmission electron microscope figure of nucleocapsid structure up-conversion nanoparticles prepared by embodiment 2；
Fig. 4 is different Er under 980nm laser excitations3+The fluorescence light of the nucleocapsid structure up-conversion nanoparticles of doping content
Spectrogram；
Fig. 5 is different Er under 980nm laser excitations3+The red-green glow of the nucleocapsid structure up-conversion nanoparticles of doping content
Than figure.
Specific embodiment
The highly doped rare earth up-conversion fluorescent nano material that the present invention is provided, by the upper conversion nano grain of doping with rare-earth ions
Son is used as nuclear structure, and the shell structure composition of cladding nuclear structure；
The doping content of the rare earth ion is more than 5%.
The highly doped rare earth up-conversion fluorescent nano material is nucleocapsid structure.
Up-conversion nanoparticles of the nuclear structure of the nucleocapsid structure for doping with rare-earth ions.The present invention is to the nanoparticle
The substrate of son, dopant ion are not particularly limited, the substrate with upper conversion function that can be known to the skilled person,
Dopant ion.In some embodiments of the invention, the up-conversion nanoparticles are with NaYF4For substrate.The rare earth
Ion is Er3+、Tm3+Or Ho3+。
In above-mentioned nuclear structure, the doping content of rare earth ion is more than 5%；In some embodiments of the invention, institute
Doping content is stated for 10%～100%；The present invention other specific embodiment in, the doping content be 80%～
100%；In the other specific embodiment of the present invention, the doping content is 10%～80%；In the present invention in addition
In some specific embodiments, the doping content is 10%, 20%, 40% or 80%.
The present invention is to the shell structure of the nucleocapsid structure and is not particularly limited, can for it is well known to those skilled in the art can
For the material of nucleocapsid structure.
In some embodiments of the invention, the highly doped rare earth up-conversion fluorescent nano material is homogeneity nucleocapsid
Structure, homogeneity inertia shell of the shell structure for nuclear structure.In some embodiments of the invention, the shell structure with
NaYF4For substrate.
The present invention is to the thickness of the shell structure and is not particularly limited, and the quenching that thickness can improve doping with rare-earth ions is dense
Degree, while reduce its cross relaxation acting on.In some embodiments of the invention, the thickness of the shell structure is 2
～5nm.
Present invention also offers the preparation method of above-mentioned highly doped rare earth up-conversion fluorescent nano material, including following step
Suddenly：
A the up-conversion nanoparticles of doping with rare-earth ions) are prepared；
B) to step A) nanoparticle that obtains carries out shell cladding.
The those skilled in the art that are prepared as of the up-conversion nanoparticles of above-mentioned doping with rare-earth ions know technology, specifically, can
Using chloride-Oleic acid predecessor method or trifluoroacetate decomposition method.
Then the nanoparticle of preparation is added in inertia husk as raw material, 300 DEG C～330 DEG C temperature reactions of Jing, forms tool
There is the nanoparticle of nucleocapsid structure.
With NaYF4As a example by inertia shell,
Above-mentioned steps B) it is specially：By YCl3.6H2O powder is dissolved in Oleic acid and 1- octadecylene mixed solutions, Ran Houyu
Step A) obtain nanoparticle cyclohexane solution mixing, after mixing high temperature remove hexamethylene, NaOH is added in reaction system
And NH4F, lower 300 DEG C～330 DEG C temperature reactions of inert gas shielding form the nanoparticle with nucleocapsid structure.
The above-mentioned preparation method that the present invention is provided is simple, reproducible, with universality.
The present invention is directed to highly doped rare earth up-conversion fluorescent nano material, solves rare earth ion by nucleocapsid structure high
Concentration quenching effect and cross-relaxation effect that doping causes, by the quenching concentration for effectively improving doping with rare-earth ions, make
There is highly doped and high luminous intensity to be possibly realized simultaneously to obtain rare earth up-conversion fluorescent nano material.On the other hand, using highly doped
Strong cross relaxation effect produced by miscellaneous, can effectively adjust the emissive porwer of each energy level of rare earth ion, so as to realize
Which is controllable multicolor luminous.
The present invention is strong by the fluorescent emission of bare nucleus nanoparticle and core-shell structure nanometer particle to different levels of doping
Degree is contrasted, it was demonstrated that after nucleocapsid cladding, nucleocapsid structure improves the quenching concentration of dopant ion really.The application will
Er3+The NaYF for singly mixing4Nanocrystalline Er3+Quenching concentration from bare nucleus when 5% lifting to 40% in nucleocapsid structure, so as to have
Its 6 times of fluorescence intensity is improve effect.
In order to further illustrate the present invention, with reference to the highly doped rare earth up-conversion fluorescent that embodiment is provided to the present invention
Nano material and preparation method thereof is described in detail.
Embodiment 1
Er is mixed singly3+NaYF4The preparation of nanoparticle bare nucleus：The ErCl of certain proportioning is taken by doping content3·6H2O and
YCl3·6H2(the two totally 1 mM, adulterate O Er3+Concentration be respectively 5%, 10%, 20%, 40%, 80%) powder be placed in
In 100ml three-necked bottles, the 1- octadecylene liquid of 6ml Oleic acid and 15ml is added, and 155 DEG C are warming up under inert gas shielding makes which
Room temperature is naturally cooled to after being completely dissolved, then instills 6ml NaOH containing 100mg and 148mg NH4The methanol solution of F, is sufficiently stirred for
After be warming up to 70 DEG C removing methanol, after being subsequently progressively warming up to 300～330 DEG C under inert gas shielding, react 90 minutes, with
After naturally cool to room temperature.With acetone, ethanol centrifuge washing resulting solution three times, remaining solid (about 150mg) is dispersed in into 8ml
In hexamethylene, obtain final product diameter about 20nm mixes Er3+NaYF4Bare nucleus nanoparticle.
Doping Er3+Concentration is that the pattern of 40% bare nucleus nanoparticle is shown in that Fig. 1, Fig. 1 are the transmission electricity of bare nucleus nanoparticle
Sub- microscope figure.From figure 1 it appears that bare nucleus NaYF4Nanoparticle monodispersity is good, even particle size distribution, change in size
Rate is less than 5 percent.
Nanoparticle to preparing carries out elementary analysiss, the results are shown in Table 1.
1 embodiment of table, 1 elementary analysiss result collects
| Doping content | 5% | 10% | 20% | 40% | 80% |
| Er:Y rate of charges | 1:19 | 1:9 | 1:4 | 2:3 | 4:1 |
| Er:Y tests ratio | 1:19.1 | 1:9.9 | 1:4.5 | 2:3.18 | 3.93:1 |
As it can be seen from table 1 the actual doping ratio of Er is consistent with desired value.
Measurement bare nucleus nanoparticle cyclohexane solution emission spectrum (the 980nm laser excitations of equal-wattage and hot spot, and
Ensure that nanoparticle concentration is consistent), to obtain the quenching concentration of Er ions in bare nucleus nanoparticle, experimental result is shown in Fig. 2, its
In, left figure is the up-conversion fluorescence spectrogram of bare nucleus nanoparticle；Right figure is the total intensity of upper conversion HONGGUANG, green glow and red-green glow
With the variation relation figure of Er ion doping concentration.As seen from Figure 2, NaYF4Bare nucleus nanoparticle list mixes Er3+Quenching concentration
Only 5%, its concentration is further improved, concentration quenching effect will be caused, so as to cause luminescent decay.
Embodiment 2
The preparation method of homogeneity core-shell structure nanometer particle：By the YCl of 152mg3·6H2O powder is placed in 100ml three-necked bottles
In, add the 1- octadecylene liquid of 6ml Oleic acid and 15ml, be warming up under inert gas shielding 150 DEG C be completely dissolved which after
Naturally cool to room temperature, then be respectively dropped into the preparation of 4ml embodiments containing 75mg 1 mix Er3+NaYF4(the doping of bare nucleus nanoparticle
Er3+Concentration respectively 5%, 10%, 20%, 40%, cyclohexane solution 80%), is to slowly warm up to 80 DEG C of removing hexamethylene, then
Room temperature is cooled to, 3ml NaOH containing 50mg and 74mg NH are instilled4The methanol solution of F, then 70 DEG C of removing methanol are warming up to, subsequently
After 300～330 DEG C are progressively warming up under inert gas shielding, react 60 minutes, subsequently naturally cool to room temperature.With acetone,
Ethanol centrifuge washing resulting solution three times, remaining solid (about 150mg) is dispersed in 8ml hexamethylene, obtains final product doping Er3+'s
NaYF4Core-shell structure nanometer particle, doping content are that 40% core-shell structure nanometer particle pattern is shown in Fig. 3.
From figure 3, it can be seen that the NaYF of nucleocapsid structure4Nanoparticle monodispersity is good, even particle size distribution, and size becomes
Rate is less than 5 percent.
Nanoparticle to preparing carries out elementary analysiss, the results are shown in Table 2.
2 embodiment of table, 2 elementary analysiss result collects
| Doping content | 5% | 10% | 20% | 40% | 80% |
| Er:Y bare nucleus | 1:19.1 | 1:9.9 | 1:4.5 | 2:3.18 | 3.93:1 |
| E:Y nucleocapsids | 1:15.6 | 1:7.8 | 1:3.2 | 2:2.86 | 3.19:1 |
As can be seen from Table 2, after coating inertia shell, Er3+Doping ratio declined compared with before cladding, thus
Prove the success of shell cladding.
(the 980nm laser of equal-wattage and hot spot swashs the emission spectrum of measurement core-shell structure nanometer particle cyclohexane solution
Send out, and ensure that nanoparticle concentration is consistent), to obtain the quenching concentration of Er ions in core-shell structure nanometer particle, experimental result
See Fig. 4, left figure is the up-conversion fluorescence spectrogram of core-shell structure nanometer particle；Right figure be change on core-shell structure nanometer particle it is red
Variation relation figure of the total intensity of light, green glow and red-green glow with Er ion doping concentration.As seen from Figure 4, NaYF4Nucleocapsid is tied
Structure nanoparticle, reduces its cross-relaxation and acts on, and its quenching concentration has improved significantly to 40%, so as to further enhancing which
Luminous intensity, compared with the core-shell structure nanometer particle of 5% doping, highly doped 40% sample in same nucleocapsid structure on
Conversion luminous intensity enhances about 6 times.
Intensity integration is done respectively to the red-green glow in the core-shell structure nanometer particle luminescent spectrum of preparation, different Er are tried to achieve3+
The red-green glow ratio of the core-shell structure nanometer particle of concentration.
Fig. 5 is the experimental result of embodiment 2.From fig. 5, it can be seen that by changing Er in core3+Doping content, upper conversion
Luminous red-green glow ratio can realize the continuously adjustabe between 0.48～6.62.It is achieved thereby that the upper conversion of controllable multi-color is sent out
Light.The application such as multi-color marking for upper conversion provides experimental basis.
From above-described embodiment, the present invention improves the quenching concentration of highly doped nanoparticle by nucleocapsid structure, and
Reduce its cross-relaxation to act on, and then while realize highly doped and high luminous intensity.
The explanation of above example is only intended to help and understands the method for the present invention and its core concept.It should be pointed out that right
For those skilled in the art, under the premise without departing from the principles of the invention, the present invention can also be carried out
Some improvement and modification, these improve and modification is also fallen in the protection domain of the claims in the present invention.
Claims (10)
1. a kind of highly doped rare earth up-conversion fluorescent nano material, it is characterised in that by the upper conversion nano of doping with rare-earth ions
Particle is used as nuclear structure, and the shell structure composition of cladding nuclear structure；
The doping content of the rare earth ion is more than 5%.
2. nano material according to claim 1, it is characterised in that the doping content of the rare earth ion is 10%～
100%.
3. nano material according to claim 1, it is characterised in that the doping content of the rare earth ion is 10%～
80%.
4. nano material according to claim 1, it is characterised in that the up-conversion nanoparticles are with NaYF4For substrate.
5. nano material according to claim 1, it is characterised in that the rare earth ion is Er3+、Tm3+Or Ho3+。
6. nano material according to claim 1, it is characterised in that the shell structure is with NaYF4For substrate.
7. nano material according to claim 1, it is characterised in that the shell structure thickness is 2～5nm.
8. the preparation method of the highly doped rare earth up-conversion fluorescent nano material described in any one of claim 1～7, its feature exist
In comprising the following steps：
A the up-conversion nanoparticles of doping with rare-earth ions) are prepared；
B) to step A) nanoparticle that obtains carries out shell cladding.
9. preparation method according to claim 8, it is characterised in that step A) preparation method be chloride-oil
Sour predecessor method or trifluoroacetate decomposition method.
10. preparation method according to claim 8, it is characterised in that step B) it is specially：
By step A) nanoparticle for preparing is added in inertia husk as raw material, and 300 DEG C～330 DEG C temperature reactions of Jing, formation have
The nanoparticle of nucleocapsid structure.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107418553A (en) * | 2017-04-17 | 2017-12-01 | 华南农业大学 | A kind of up-conversion luminescent material of core shell structure and preparation method thereof |
| CN108384547A (en) * | 2018-04-25 | 2018-08-10 | 华中科技大学 | A kind of list doping-enrichment nucleocapsid up-conversion luminescent material and preparation method thereof |
| WO2019114832A1 (en) * | 2017-12-15 | 2019-06-20 | Tcl集团股份有限公司 | Quantum dot composite material and preparation method therefor |
| CN109929542A (en) * | 2017-12-15 | 2019-06-25 | Tcl集团股份有限公司 | A kind of quantum dot composite material and preparation method thereof |
| CN109929538A (en) * | 2017-12-15 | 2019-06-25 | Tcl集团股份有限公司 | A kind of quantum dot composite material and preparation method thereof |
| CN109929543A (en) * | 2017-12-15 | 2019-06-25 | Tcl集团股份有限公司 | A kind of quantum dot composite material and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107418553A (en) * | 2017-04-17 | 2017-12-01 | 华南农业大学 | A kind of up-conversion luminescent material of core shell structure and preparation method thereof |
| CN107418553B (en) * | 2017-04-17 | 2019-11-08 | 华南农业大学 | A kind of up-conversion luminescent material of nucleocapsid structure and preparation method thereof |
| WO2019114832A1 (en) * | 2017-12-15 | 2019-06-20 | Tcl集团股份有限公司 | Quantum dot composite material and preparation method therefor |
| CN109929542A (en) * | 2017-12-15 | 2019-06-25 | Tcl集团股份有限公司 | A kind of quantum dot composite material and preparation method thereof |
| CN109929538A (en) * | 2017-12-15 | 2019-06-25 | Tcl集团股份有限公司 | A kind of quantum dot composite material and preparation method thereof |
| CN109929543A (en) * | 2017-12-15 | 2019-06-25 | Tcl集团股份有限公司 | A kind of quantum dot composite material and preparation method thereof |
| CN108384547A (en) * | 2018-04-25 | 2018-08-10 | 华中科技大学 | A kind of list doping-enrichment nucleocapsid up-conversion luminescent material and preparation method thereof |
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Application publication date: 20170426 |