CN103881720A - Method for preparing high-doping rare-earth upconversion fluorescence material by utilizing nuclear shell coating - Google Patents
Method for preparing high-doping rare-earth upconversion fluorescence material by utilizing nuclear shell coating Download PDFInfo
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- CN103881720A CN103881720A CN201410035655.2A CN201410035655A CN103881720A CN 103881720 A CN103881720 A CN 103881720A CN 201410035655 A CN201410035655 A CN 201410035655A CN 103881720 A CN103881720 A CN 103881720A
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Abstract
The invention provides a method for preparing a high-doping rare-earth upconversion fluorescence material by utilizing nuclear shell coating, and belongs to the technical field of luminescent materials. The method comprises the following steps of firstly preparing bare nucleus upconversion nanometer particles with different rare-earth ion doping concentrations; then respectively carrying out the nuclear shell coating on the obtained bare nucleus upconversion nanometer particles with different rare-earth ion doping concentrations to obtain upconversion nanometer particles with nuclear shell structures, wherein the thickness of a shell layer is more than 2 nanometers. The method provided by the invention effectively increases the quenching concentration of doped rare-earth ions by isolating the surface effect of the rare-earth doping nanometer particles by utilizing the shell layer and realizes that the color of an upconversion spectrum is adjustable by regulating rare-earth doping concentration.
Description
Technical field
The invention belongs to luminescent material technical field, be specifically related to a kind of method of utilizing the highly doped rare earth upconverting fluorescent material of the coated preparation of nucleocapsid.
Background technology
Rear-earth-doped upconverting fluorescent material is a kind of fluorescent material that utilizes lanthanide ion doping near infrared light to be converted into visible ray and UV-light.It is in sun power utilization, data storage, and the fields such as 3-D display and imaging in biological tissues and detection and drug delivery all have a wide range of applications.Take biological detection direction as example, compared with traditional organic fluorescent dye or semiconductor-quantum-point, it is low that rear-earth-doped up-conversion has toxicity, and chemical stability is high, unglazed bleaching phenomenon, the advantage such as the life time of the level is long.More because of within its excitation wavelength can be positioned at " optical window " of human body, penetration depth high (cm magnitude) to tissue, and its utilizing emitted light signal is without the interference of background fluorescence, and glow color is adjustable, therefore be for example widely used in, at complex system (human body, whole blood) in the multicolor fluorescence marker detection of carrying out, it detects lower limit can reach 10
-9mol/L magnitude (Efficient fluorescence resonance energy transfer between upconversion nanophosphors and graphene oxide:a highly sensitive biosensing platform, Chem.Communication, 2011,47,4661-4663.), be a kind of fluorescent mark material of excellent performance.
But rear-earth-doped upconverting fluorescent material, in the further application in above-mentioned field, is all being restricted by the problem of an essence---be that its luminous efficiency is too low, luminous intensity is inadequate.With most effective hexagonal phase NaYF
4: Yb
3+, Er
3+mixing altogether nanoparticle is example, at 150W/cm
2980nm laser excitation under, conventionally only have upper efficiency of conversion (the Absolute quantum yield measurements of colloidal NaYF of 0.3% left and right
4: Er
3+, Yb
3+upconverting nanoparticles, Nanoscale, 2010,2,1417-1419.).Therefore improving its luminous efficiency and luminous intensity is a problem demanding prompt solution.
Obviously, the doping content that improves nanoparticle Rare Earth Ion is expected to improve its luminous intensity, but we notice, at present in actual applications, the doping content of rare earth ion in matrix still remains at low levels, this is between the rare earth ion due to high-dopant concentration, to be easy to strong cross relaxation and concentration quenching effect occur, and causes high doping content conventionally all to cause on the contrary the reduction of luminous intensity.Although have recently bibliographical information in very high power density (10
6w/cm
2) excite down (Single-nanocrystal sensitivity achieved by enhanced upconversion luminescence, Nature Nanotechnology, 2013, 8, 729-734.), or in special matrix structure (Enhancing multiphoton upconversion through energy clustering at sublattice level, Nature Materials, Published online24November2013), the quenching concentration of rare earth ion can be greatly improved, but these methods still enjoy restriction in practicality and ubiquity.The former desired high excitation light power density is difficult to realize in many practical applications, for example, in living organisms application, require excitation light power density to be controlled at several W/cm
2below, in immunoassay detects, excitation light power density is conventionally only in 10～100W/cm
2scope, from 10
6w/cm
2all differ from several orders of magnitude, thereby do not observe phenomenon described in it.Latter is only applicable to KYb
2f
7this special matrix, for conventional matrix, especially the highest to luminous efficiency hexagonal phase NaYF
4matrix also to no effect.Therefore, finding a kind of pervasive method and improve the quencher upper limit of doping concentration of rare earth ion, is very important actual demand.
Summary of the invention
The object of the invention is in order to solve existing method repeatability and the poor problem of ubiquity, and a kind of method of utilizing the highly doped rare earth upconverting fluorescent material of the coated preparation of nucleocapsid is provided.
The invention provides a kind of method of utilizing the highly doped rare earth upconverting fluorescent material of the coated preparation of nucleocapsid, comprising:
Step 1: the bare nucleus up-conversion nanoparticles of preparing different levels of doping rare earth ion;
Step 2: it is coated that the bare nucleus up-conversion nanoparticles of the different levels of doping rare earth ion that step 1 is obtained carries out respectively nucleocapsid, obtains the up-conversion nanoparticles of nucleocapsid structure; Described shell thickness is greater than 2nm.
Preferably, described bare nucleus up-conversion nanoparticles is with NaYF
4for matrix, doping Er
3+ion.
Preferably, described doping content is 2～80%.
Preferably, described shell thickness is 2-6 nanometer.
Principle of the present invention
The principle of concentration quenching is that energy transmits back and forth between identical ion, finally be delivered to quencher in addition in defect, nanoparticle is owing to possessing great specific surface area, cause the defect overwhelming majority in particle to be all positioned at its surface, the present invention is coated by carrying out homogeneity nucleocapsid, coated shell thickness must be enough to the disadvantageous effect of isolated surface effects to rare earth ion, like this can the interaction of the rare earth ion in nanoparticle and surface imperfection is isolated.Method of the present invention has universality in nanoparticle system, therefore can (comprise NaYF at arbitrary substrate
4) nanoparticle in improve the quenching concentration of institute's doping with rare-earth ions.
Beneficial effect of the present invention
First the present invention prepares the bare nucleus up-conversion nanoparticles of different levels of doping rare earth ion, is then coated respectively shell thereon, and coated shell thickness must be enough to the disadvantageous effect of isolated surface effects to rare earth ion, and described shell thickness is greater than 2nm.Existing nucleocapsid is coated, all to have used shell isolated after surface effects, nanoparticle is in the situation that doping content is constant, luminous intensity is improved, compared with prior art, the present invention finds that its luminescence center quenching concentration, under nucleocapsid structure, also can be greatly enhanced, thereby can utilize the highly doped mode of luminescence center further to promote the luminous intensity of up-conversion nanoparticles, experimental result shows: by Er
3+the NaYF singly mixing
4nanocrystalline Er
3+quenching concentration 5% during from bare nucleus risen to 40% nucleocapsid structure, thereby effectively improved its fluorescence intensity of approximately 6 times (approximately 2 times of green glows, approximately 10 times of ruddiness).On the other hand, utilize the strong cross relaxation effect of highly doped generation, can also effectively regulate the emissive porwer of the each energy level of rare earth ion, thereby realize controlled multicolor luminous.Method of the present invention has universality in nanoparticle system, therefore can (comprise NaYF at arbitrary substrate
4) nanoparticle in improve the quenching concentration of institute's doping with rare-earth ions.
Accompanying drawing explanation
Fig. 1 is the bare nucleus (a) prepared of the embodiment of the present invention 1 and the transmission electron microscope figure of nucleocapsid structure (b) up-conversion nanoparticles;
Fig. 2 is Er prepared by the embodiment of the present invention 1
3+the bare nucleus (2a-2f) that ionic concn changes and the ultimate analysis collection of illustrative plates of nucleocapsid structure (2g-2l) nanoparticle;
Fig. 3 embodiment of the present invention 1 under 980nm laser excitation, Er
3+the bare nucleus (a-b) that concentration changes and the fluorescence spectrum figure of nucleocapsid structure (c-d) nanoparticle;
Fig. 4 embodiment of the present invention 1 under 980nm laser excitation, Er
3+the red-green glow of the core-shell structure nanometer particle that concentration changes is than figure.
Embodiment
The invention provides a kind of method of utilizing the highly doped rare earth upconverting fluorescent material of the coated preparation of nucleocapsid, comprising:
Step 1: the bare nucleus up-conversion nanoparticles of preparing different levels of doping rare earth ion;
Step 2: it is coated that the bare nucleus up-conversion nanoparticles of the different levels of doping rare earth ion that step 1 is obtained carries out respectively nucleocapsid, obtains the up-conversion nanoparticles of nucleocapsid structure; Described shell thickness is greater than 2nm.
According to the present invention, the preparation method of the bare nucleus up-conversion nanoparticles of the present invention to the different rare earth ions doping content described in step 1 is the conventional method in this area, be not particularly limited, concrete preparation method can reference Monodisperse silica-coated polyvinylpyrrolidone/NaYF
4nanocrystals with multicolor upconversion fluorescence emission, Angew.Chem.Int.Ed, 2006,45,7732-7735.
According to the present invention, the principle of concentration quenching is that energy transmits back and forth between identical ion, finally be delivered to quencher in addition in defect, nanoparticle, owing to possessing great specific surface area, causes the defect overwhelming majority in particle to be all positioned at its surface, therefore, the present invention is not particularly limited bare nucleus up-conversion nanoparticles, have universality, preferably, described bare nucleus up-conversion nanoparticles is with NaYF
4for matrix, doping Er
3+ion.Doping content scope of the present invention is preferably 2～80%.
According to the present invention, the bare nucleus up-conversion nanoparticles of different levels of doping rare earth ion is carried out respectively to nucleocapsid to be coated, the coated method of described nucleocapsid is the conventional method in this area, be not particularly limited, concrete grammar can reference Synthesis of hexagonal-phase core-shell NaYF
4nanocrystals with tunable upconversion fluorescence, Langmuir, 2008,24,12123-12125.
According to the present invention, described shell thickness is greater than 2nm, and so coated shell thickness just can be enough to the disadvantageous effect of isolated surface effects to rare earth ion, and described shell thickness is preferably 2-6nm, more preferably 3nm.
Below in conjunction with specific embodiment, the present invention is further described.
Embodiment 1
Singly to mix Er
3+naYF
4nanoparticle is example, and the concrete preparation method of its bare nucleus is (Monodisperse silica-coated polyvinylpyrrolidone/NaYF
4nanocrystals with multicolor upconversion fluorescence emission, Angew.Chem.Int.Ed, 2006,45,7732-7735.): by doping content Er
3+concentration is respectively 2%, 5%, 10%, 20%, 40%, 80% and gets the ErCl that determines proportioning
36H
2o and YCl
36H
2(the two is totally 1 mmole, wherein ErCl for O
36H
2o amount of substance is that doping content is multiplied by 1 mmole, and all the other are all YCl
36H
2o) powder is placed in 100ml three-necked bottle, adds the 1-octadecylene liquid of 6ml oleic acid and 15ml, is warming up to 155 ℃ and naturally cools to room temperature after it is dissolved completely, then splash into 6ml containing 100mg NaOH and 148mgNH under protection of inert gas
4the methanol solution of F; after fully stirring, be warming up to 70 ℃ and remove methyl alcohol; under protection of inert gas, be progressively warming up to subsequently after 300～330 ℃; react 90 minutes; naturally cool to subsequently room temperature, with acetone, ethanol centrifuge washing gained solution three times; remaining solid (about 150mg) is dispersed in 8ml hexanaphthene, obtains respectively the Er of diameter 20nm
3+doping content be 2%, 5%, 10%, 20%, 40%, 80% NaYF
4bare nucleus nanoparticle;
The preparation method of homogeneity nucleocapsid structure (take inertia shell as example) nanoparticle is (Synthesis of hexagonal-phase core-shell NaYF
4nanocrystals with tunable upconversion fluorescence, Langmuir, 2008,24,12123-12125.): by the YCl of 152mg
36H
2o powder is placed in 100ml three-necked bottle, adds the 1-octadecylene liquid of 6ml oleic acid and 15ml, is warming up to 150 ℃ and naturally cools to room temperature after it is dissolved completely, then splash into respectively 4ml containing 75mgEr under protection of inert gas
3+doping content be 2%, 5%, 10%, 20%, 40%, 80% NaYF
4the cyclohexane solution of bare nucleus nanoparticle, is slowly warming up to 80 ℃ and removes hexanaphthene, then be cooled to room temperature, splashes into 3ml containing 50mgNaOH and 74mgNH
4the methanol solution of F, then be warming up to 70 ℃ and remove methyl alcohol, under protection of inert gas, be progressively warming up to subsequently after 300～330 ℃, react 60 minutes, naturally cool to subsequently room temperature.With acetone, ethanol centrifuge washing gained solution three times, is dispersed in remaining solid (about 150mg) in 8ml hexanaphthene, obtains a series of Er of mixing
3+naYF
4core-shell structure nanometer particle.
Because mix Er
3+concentration does not affect the pattern of nanoparticle, and Fig. 1 is with doping Er
3+5% nanoparticle is example, has provided bare nucleus (a) and nucleocapsid structure (b) NaYF
4the transmission electron microscope figure of up-conversion nanoparticles.As can be seen from Figure 1, the NaYF of bare nucleus and nucleocapsid structure
4nanoparticle monodispersity is good, and size distribution is even, and size changing rate is less than 5 percent, and the diameter of bare nucleus is about 20 nanometers, and the diameter of core-shell structure nanometer particle is about 26 nanometers, so the thick 3 nanometer left and right that should be of shell.
Fig. 2 is Er prepared by the embodiment of the present invention 1
3+the bare nucleus (2a-2f) that ionic concn changes and the ultimate analysis collection of illustrative plates of nucleocapsid structure (Fig. 2 g-2l) nanoparticle; 2a-2f figure in Fig. 2 is NaYF
4in bare nucleus, doping Er
3+concentration is respectively 2%, 5%, 10%, 20%, 40%, 80% X-ray energy spectrum figure.The results of elemental analyses of having listed doped samples in each table, from table, result can be found out, Er
3+actual doping ratio basic consistent with our predicated value.2g-2l in Fig. 2 is the 2a-2f sample coated inertia shell (NaYF of the lanthanon that do not adulterate respectively in Fig. 2
4shell) after, in corresponding core-shell structure nanometer particle, the X-ray energy spectrum figure of each element.In the table of 2g-2l from Fig. 2, result can be found out, after coated inertia shell, and Er
3+doping ratio all decline to some extent compared with before coated, this confirmed our shell coated be successful.
Fig. 3 embodiment of the present invention 1 under 980nm laser excitation, Er
3+the bare nucleus (a-b) that concentration changes and the fluorescence spectrum figure of nucleocapsid structure (c-d) nanoparticle; A-b from Fig. 3 can find out, NaYF
4bare nucleus nanoparticle list is mixed Er
3+quenching concentration be only 5%, further improve its concentration, will cause concentration quenching effect, thereby cause luminescent decay.C-d in Fig. 3 can find out, NaYF
4core-shell structure nanometer particle, due to shell passivation surface, by Er in surface and nanoparticle
3+interaction isolated, therefore its quenching concentration has improved significantly to 40%, thereby further strengthen its luminous intensity, compared with the core-shell structure nanometer particle of 5% doping, highly doped 40% sample Up-conversion Intensity in same nucleocapsid structure has strengthened about 6 times (approximately 2 times of green glows, approximately 10 times of ruddiness).
Fig. 4 embodiment of the present invention 1 under 980nm laser excitation, Er
3+the red-green glow of the core-shell structure nanometer particle that concentration changes is than figure.As can be seen from Figure 4, by changing Er in core
3+doping content, the red-green glow ratio of up-conversion luminescence can be realized from adjustable continuously between 0.48-6.62, thereby has realized the up-conversion luminescence of controlled polychrome, for the application such as the multi-color marking of upper conversion provide experimental basis.
Above-described embodiment is only explanation technical conceive of the present invention and feature, and its object is to allow person skilled in the art can understand content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalences that spirit is done according to the present invention change or modify, within all should being encompassed in protection scope of the present invention.
Claims (4)
1. a method of utilizing the highly doped rare earth upconverting fluorescent material of the coated preparation of nucleocapsid, is characterized in that, comprising:
Step 1: the bare nucleus up-conversion nanoparticles of preparing different levels of doping rare earth ion;
Step 2: it is coated that the bare nucleus up-conversion nanoparticles of the different levels of doping rare earth ion that step 1 is obtained carries out respectively nucleocapsid, obtains the up-conversion nanoparticles of nucleocapsid structure; Described shell thickness is greater than 2nm.
2. a kind of method of utilizing the highly doped rare earth upconverting fluorescent material of the coated preparation of nucleocapsid according to claim 1, is characterized in that, described bare nucleus up-conversion nanoparticles is with NaYF
4for matrix, doping Er
3+ion.
3. a kind of method of utilizing the highly doped rare earth upconverting fluorescent material of the coated preparation of nucleocapsid according to claim 1, is characterized in that, described doping content scope is 2～80%.
4. a kind of method of utilizing the highly doped rare earth upconverting fluorescent material of the coated preparation of nucleocapsid according to claim 1, is characterized in that, described shell thickness is 2-6 nanometer.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105203506A (en) * | 2015-09-24 | 2015-12-30 | 上海大学 | Nanoprobe for heavy metal ion up-conversion luminescence detection and preparation method thereof |
| CN105419801A (en) * | 2015-12-22 | 2016-03-23 | 中国科学院长春光学精密机械与物理研究所 | Highly-doped multi-band excitation rare earth upconversion fluorescence nano material and preparation method thereof |
| CN106566527A (en) * | 2016-08-12 | 2017-04-19 | 中国计量大学 | Method for increasing doping concentration of Tm<3+> in up-conversion luminescence nanocrystals |
| CN106590659A (en) * | 2016-12-19 | 2017-04-26 | 中国科学院长春光学精密机械与物理研究所 | Highly doped rare earth up-conversion fluorescent nano 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 |
| 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 |
| 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 |
| 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 |
| 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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| CN110964526A (en) * | 2020-01-14 | 2020-04-07 | 华中科技大学 | Up-conversion nanoparticles with core-shell structure, preparation method and application thereof |
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| CN105203506A (en) * | 2015-09-24 | 2015-12-30 | 上海大学 | Nanoprobe for heavy metal ion up-conversion luminescence detection and preparation method thereof |
| CN105419801A (en) * | 2015-12-22 | 2016-03-23 | 中国科学院长春光学精密机械与物理研究所 | Highly-doped multi-band excitation rare earth upconversion fluorescence nano material and preparation method thereof |
| CN106566527B (en) * | 2016-08-12 | 2019-02-26 | 中国计量大学 | Tm in a kind of raising up-conversion luminescence nanometer crystal3+The method of doping concentration |
| CN106566527A (en) * | 2016-08-12 | 2017-04-19 | 中国计量大学 | Method for increasing doping concentration of Tm<3+> in up-conversion luminescence nanocrystals |
| CN106590659A (en) * | 2016-12-19 | 2017-04-26 | 中国科学院长春光学精密机械与物理研究所 | Highly doped rare earth up-conversion fluorescent nano 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 |
| 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 |
| 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 |
| 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 |
| CN108384547B (en) * | 2018-04-25 | 2020-05-19 | 华中科技大学 | Up-conversion luminescent material with single-doped-enriched core-shell structure and preparation method thereof |
| CN110255619A (en) * | 2019-06-21 | 2019-09-20 | 南京工业大学 | A method of based on upper conversion nano particle preparation three-dimensional hollow structure molybdenum sulfide |
| CN110255619B (en) * | 2019-06-21 | 2022-04-22 | 南京工业大学 | Method for preparing molybdenum sulfide with three-dimensional hollow structure based on up-conversion nanoparticles |
| CN110964526A (en) * | 2020-01-14 | 2020-04-07 | 华中科技大学 | Up-conversion nanoparticles with core-shell structure, preparation method and application thereof |
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Application publication date: 20140625 |