CN105505373A - Luminous Janus colloid and manufacturing method thereof - Google Patents
Luminous Janus colloid and manufacturing method thereof Download PDFInfo
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- CN105505373A CN105505373A CN201510994625.9A CN201510994625A CN105505373A CN 105505373 A CN105505373 A CN 105505373A CN 201510994625 A CN201510994625 A CN 201510994625A CN 105505373 A CN105505373 A CN 105505373A
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
- C09K11/881—Chalcogenides
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Abstract
The invention discloses a luminous Janus colloid and a manufacturing method thereof. The method includes the steps that A, a precious metal colloid precursor solution and an alkyl-amino-based methylbenzene solution are mixed, and the mixed solution is ultrasonically treated for 10-20 min at room temperature; B, the mixed solution is irradiated by ultraviolet, and then a quantum dot precursor is added to the mixed solution in the inert gas environment and stirred; C, finally, methyl alcohol is added to the mixed solution, and the luminous Janus colloid is manufactured through centrifugal purification. Precious metal particles are introduced into the manufactured luminous Janus colloid, a large number of free electrons exist around the precious metal particles, the free electrons can generate surface plasma waves under induction of exciting light or excited state fluorescence, after the precious metal particles are introduced into the quantum dot precursor to form the luminous Janus colloid, the spontaneous radiation speed of excitons is increased, and meanwhile the quantum yield of quantum dots can be effectively increased through the precious metal surface plasma effect.
Description
Technical field
The present invention relates to quantum dot field, particularly relate to a kind of luminous Janus colloid and preparation method thereof.
Background technology
Janus in " Janus " Yuan Zhi ancient Roman mythology, 1991, French famous scientist Gennies held with this morphology the colloidal solid that those have chemical asymmetry first in its Nobel wins a prize speech.Quantum dot refer to exciton on three-dimensional space direction all in bond live semiconductor nano material, particle diameter is generally at 1-100nm.Due to the existence of " quantum confinement " effect, along with quantum dot size reduces further, continuous print energy band structure becomes discontinuous discrete energy levels structure, can send remarkable fluorescence after being excited.The quantum dot with different bandwidth can be obtained by the size of quantum point.There is the quantum dot of different bandwidth, the photon of different-energy can be sent under the shooting conditions of certain wavelength, namely the light of different colours.
The synthesis of quantum dot is generally carried out in the middle of solution, and the quantum dot essence adopting chemical solution growth method to synthesize is " semi-conductor colloid nanocrystalline ", and as colloid, it has polymolecularity thus is easy to physical operations on the one hand; The highly homogeneous quantum dot of particle diameter has the excellent performance such as emmission spectrum spectral purity is high, luminous quantum efficiency is high, glow color is adjustable, long service life on the other hand.These characteristics make the quantum dot enhanced film LCD TV (QDEF-LCD) using quanta point material as luminescent layer and light emitting diode with quantum dots (QLED) receive the extensive concern of academia and industrial community, and light emitting diode with quantum dots has very high application prospect as a kind of novel display material.And the making method of the quantum yield of quantum dot in prior art, is not strengthened by plasma.
Therefore, prior art has yet to be improved and developed.
Summary of the invention
In view of above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of luminous Janus colloid and preparation method thereof, be intended to solve the problem that the quantum yield of existing quantum dot is low.
Technical scheme of the present invention is as follows:
A making method for luminous Janus colloid, wherein, comprises step:
A, by precious metal colloid precursor solution and alkylamino radical toluene solution mixing, supersound process mixing solutions 10-20 minute under room temperature;
B, by mixing solutions described in UV-irradiation, then in an inert atmosphere quantum dot presoma to be joined in described mixing solutions and to stir;
C, finally in described mixing solutions, add methyl alcohol, then obtain luminous Janus colloid by centrifugal purification.
The making method of described luminous Janus colloid, wherein, in described steps A, the preparation process of precious metal colloid precursor solution is as follows:
A0, the noble metal halide be dissolved in toluene solution and four octyl group brometo de amonios are carried out being mixed to get mixing solutions a;
A1, described mixing solutions a is at room temperature carried out supersound process, obtain precious metal colloid precursor solution.
The making method of described luminous Janus colloid, wherein, in described mixing solutions a, the concentration range of noble metal halide is: 1 ~ 10mg/mL.
The making method of described luminous Janus colloid, wherein, in described mixing solutions a, the mass ratio of four octyl group brometo de amonios and noble metal halide is: 1:2 ~ 10.
The making method of described luminous Janus colloid, wherein, described precious metal is the one in Au, Ag, Pt, Pd.
The making method of described luminous Janus colloid, wherein, described alkylamino radical toluene is the one in octane carbaryl, decane carbaryl, n-Laurylamine toluene, tetradecylamine toluene, cetylamine toluene and octadecylamine toluene.
The making method of described luminous Janus colloid, wherein, in described step B, quantum dot precursor preparation process is as follows:
CdSe/CdS quantum dot toluene solution and Octadecane base phosphoric acid are mixed to form quantum dot presoma.
The making method of described luminous Janus colloid, wherein, in described step B, described UV-light is wavelength is 254 ~ 400nm.
A kind of luminous Janus colloid, wherein, adopts the making method as described in any one of claim 1 ~ 8 to make.
Beneficial effect: the present invention passes through the precious metal colloid presoma be dissolved in toluene solution and the quantum dot presoma hybrid reaction under rare gas element and ultraviolet lighting environment be dissolved in alkylphosphonic acid carboxylic acid, thus forms luminous Janus colloid.Form luminous Janus colloid by introducing noble metal granule in quantum dot presoma, the spontaneous emission rate of exciton is accelerated, utilize precious metal surface plasma effect effectively can improve the quantum yield of quantum dot simultaneously.
Accompanying drawing explanation
Fig. 1 is the schema of the making method preferred embodiment of a kind of luminous Janus colloid of the present invention.
Fig. 2 is the structural representation of a kind of luminous Janus colloid of the present invention preferred embodiment.
Embodiment
The invention provides a kind of luminous Janus colloid and preparation method thereof, for making object of the present invention, technical scheme and effect clearly, clearly, the present invention is described in more detail below.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Refer to Fig. 1, Fig. 1 is the schema of the making method preferred embodiment of a kind of luminous Janus of the present invention, and as shown in the figure, it comprises step:
S100, by precious metal colloid precursor solution and alkylamino radical toluene solution mixing, supersound process mixing solutions 10-20 minute under room temperature;
S110, by mixing solutions described in UV-irradiation, then in an inert atmosphere quantum dot presoma to be joined in described mixing solutions and to stir;
S120, finally in described mixing solutions, add methyl alcohol, then obtain luminous Janus colloid by centrifugal purification.
In the present invention, because plasmons coupling can strengthen spontaneous fluorescent radiation transition, exciton can pass through radiative transition, and nonradiative transition two kinds of modes decay.The present invention passes through the precious metal colloid presoma be dissolved in toluene solution and the quantum dot presoma hybrid reaction under rare gas element and ultraviolet lighting environment be dissolved in alkylphosphonic acid carboxylic acid, thus form luminous Janus colloid, due to Janus colloid introducing noble metal nano particles, and around noble metal granule, there is a large amount of unbound electrons, these unbound electrons can produce surface plasma-wave under the induction of exciting light or excited state fluorescence.When emission wavelength and the surface plasma resonance peak match(ing) of fluorescent material, surface plasma resonance can be there is.Now, part energy can be coupled in surface plasma by exciton, and this process is more faster than the speed of exciton spontaneous radiation; Meanwhile, because resonance result in the enhancing of local electric field near fluorescent material, thus increase density of states(DOS), in conjunction with the theory of Purcell, the spontaneous emission rate of exciton is relevant with the density of states(DOS) of photon.Therefore, the present invention, by after introducing noble metal granule form luminous Janus colloid in quantum dot presoma, makes the spontaneous emission rate of exciton accelerate, utilizes precious metal surface plasma effect effectively can improve the quantum yield of quantum dot simultaneously.
Before step S100, first prepare precious metal colloid precursor solution, it comprises: S10, the noble metal halide be dissolved in toluene solution and four octyl group brometo de amonios are carried out being mixed to get mixing solutions a; S11, described mixing solutions a is at room temperature carried out supersound process, obtain precious metal colloid precursor solution.
Particularly, described precious metal is the one in Au, Ag, Pt, Pd, and the present invention is with AuCl
3for example prepares precious metal colloid precursor solution, first the AuCl in non-polar solution will be dissolved in
3four octyl group brometo de amonios carry out mixed dissolution and form mixing solutions a, then mixing solutions a are at room temperature carried out supersound process until solution presents garnet, namely obtain golden precursor solution.
Further, described non-polar solution is preferably toluene solution, noble metal halide is more easily dissolved in toluene solution, in described mixing solutions a, the concentration range of noble metal halide is: 1 ~ 10mg/mL, preferably, the concentration of the preferred noble metal halide of the present invention is 5mg/mL, and precious metal colloid precursor solution obtained under this concentration has polymolecularity.
Further, in described mixing solutions a, the mass ratio of described four octyl group brometo de amonios and noble metal halide is 1:2 ~ 10, preferably, the mass ratio of the present invention preferably four octyl group brometo de amonios and noble metal halide is 1:4, the activity of precious metal colloid precursor solution obtained under this mass ratio is high, easily deposition Janus colloid.
Further, with PtCl
2for the method for example preparation Pt presoma is: will the PtCl in toluene solution be dissolved in
2form mixing solutions with four octyl group brometo de amonio mixed dissolutions, above-mentioned mixing solutions is at room temperature carried out supersound process until present limpid garnet, and gained solution is Pt precursor solution.
In the step s 100, by precious metal colloid precursor solution and the mixing of alkylamino radical toluene solution, supersound process mixing solutions 10-20 minute under room temperature, particularly, described alkylamino radical toluene solution is octane carbaryl, decane carbaryl, n-Laurylamine toluene, tetradecylamine toluene, one in cetylamine toluene and octadecylamine toluene, the present invention is preferably by precious metal colloid precursor solution and the mixing of n-Laurylamine toluene solution, further, preferably at room temperature to mixing solutions supersound process 15 minutes, noble metal precursor liquid solution is fully mixed with n-Laurylamine toluene solution.
Before step S110, also comprise the preparation of quantum dot precursor solution, here for CdSe/CdS quantum dot, by CdSe/CdS quantum dot toluene solution and Octadecane base phosphoric acid are mixed to form quantum dot presoma.Further, the CdSe/CdS quantum dot toluene solution (about 50 μMs) of 0.5mL and the Octadecane base phosphoric acid of 12mg are mixed to form quantum dot presoma by the present invention.
In step s 110, by mixing solutions described in UV-irradiation, then in an inert atmosphere quantum dot presoma to be joined in described mixing solutions and to stir, particularly, the present invention is by being mixing solutions described in a kind of UV-irradiation between 254 ~ 400nm with wavelength, preferably, optimal wavelength is mixing solutions described in the UV-irradiation of 300nm, preferably in a nitrogen environment quantum dot precursor solution is joined in mixing solutions fast further, and at room temperature stir 20 minutes, the abundant deposition growing of precious metal can be realized to CdSe/CdS surface by above-mentioned steps.
In the step s 120, the present invention by adding methyl alcohol in described mixing solutions, then obtains luminous Janus colloid by centrifugal purification.Particularly, the present invention by adding methyl alcohol generation quencher reaction in mixing solutions, described quencher reaction refers to that the excited state molecule of fluorescent substance is by the impact effect with quencher molecule, loses its excitation energy and return ground state with the mechanism of the mechanism of energy trasfer or charge transfer.Further, product by centrifugal purification, is dispersed in toluene solvant after adding methyl alcohol generation quencher reaction in the mixture by the present invention, final obtained luminous Janus colloid.
Further, the present invention by controlling the activity of precious metal colloid presoma and quantum dot presoma, feed rate, reactant concn go to realize to control the structure of luminous Janus colloid and size.
Based on aforesaid method, the present invention also provides a kind of luminous Janus colloid, and as shown in Figure 2, the making method of the luminous Janus colloid described in described luminous Janus colloid adopts is made.The luminous Janus colloid that the present invention obtains introduces noble metal granule 110, and around noble metal granule, there is a large amount of unbound electrons, these unbound electrons can produce surface plasma-wave under the induction of exciting light or excited state fluorescence, the present invention by after introducing noble metal granule 110 and forming luminous Janus colloid in quantum dot presoma 100, the spontaneous emission rate of exciton is accelerated, utilizes precious metal 110 surface plasma effect effectively can improve the quantum yield of quantum dot simultaneously.
With specific embodiment, the present invention is elaborated below:
Embodiment 1
1), the 0.15M n-Laurylamine toluene solution of the noble metal precursor liquid solution of 10mL and 10mL is blended in 100mL flask, ultrasonic 15 minutes of room temperature;
2) be, with wavelength the UV-irradiation mixing solutions of 300nm, in a nitrogen environment quantum dot precursor solution joined in described mixing solutions fast, stirred at ambient temperature 20 minutes;
3) in described mixing solutions, finally add the methyl alcohol of 25mL, then obtain luminous Janus colloid by centrifugal purification.
Embodiment 2
1), the 0.15M n-Laurylamine toluene solution of the noble metal precursor liquid solution of 10mL and 10mL is blended in 100mL flask, ultrasonic 25 minutes of room temperature;
2) be, with wavelength the UV-irradiation mixing solutions of 400nm, in a nitrogen environment quantum dot precursor solution joined in described mixing solutions fast, stirred at ambient temperature 30 minutes;
3) in described mixing solutions, finally add the methyl alcohol of 25mL, then obtain luminous Janus colloid by centrifugal purification.
Embodiment 3
1), the 0.15M n-Laurylamine toluene solution of the noble metal precursor liquid solution of 10mL and 10mL is blended in 100mL flask, ultrasonic 40 minutes of room temperature;
2) be, with wavelength the UV-irradiation mixing solutions of 250nm, in a nitrogen environment quantum dot precursor solution joined in described mixing solutions fast, stirred at ambient temperature 45 minutes;
3) in described mixing solutions, finally add the methyl alcohol of 25mL, then obtain luminous Janus colloid by centrifugal purification.
In sum, luminous Janus colloid of one provided by the invention and preparation method thereof, by by the precious metal colloid presoma be dissolved in toluene solution be dissolved in quantum dot presoma hybrid reaction under rare gas element and ultraviolet lighting environment in alkylphosphonic acid carboxylic acid, thus form luminous Janus colloid.The luminous Janus colloid that the present invention obtains introduces noble metal granule, and around noble metal granule, there is a large amount of unbound electrons, these unbound electrons can produce surface plasma-wave under the induction of exciting light or excited state fluorescence, the present invention by after introducing noble metal granule and forming luminous Janus colloid in quantum dot presoma, the spontaneous emission rate of exciton is accelerated, utilizes precious metal surface plasma effect effectively can improve the quantum yield of quantum dot simultaneously.
Should be understood that, application of the present invention is not limited to above-mentioned citing, for those of ordinary skills, can be improved according to the above description or convert, and all these improve and convert the protection domain that all should belong to claims of the present invention.
Claims (9)
1. a making method for luminous Janus colloid, is characterized in that, comprise step:
A, by precious metal colloid precursor solution and alkylamino radical toluene solution mixing, supersound process mixing solutions 10-20 minute under room temperature;
B, by mixing solutions described in UV-irradiation, then in an inert atmosphere quantum dot presoma to be joined in described mixing solutions and to stir;
C, finally in described mixing solutions, add methyl alcohol, then obtain luminous Janus colloid by centrifugal purification.
2. the making method of luminous Janus colloid according to claim 1, is characterized in that, in described steps A, the preparation process of precious metal colloid precursor solution is as follows:
A0, the noble metal halide be dissolved in toluene solution and four octyl group brometo de amonios are carried out being mixed to get mixing solutions a;
A1, described mixing solutions a is at room temperature carried out supersound process, obtain precious metal colloid precursor solution.
3. the making method of luminous Janus colloid according to claim 2, is characterized in that, in described mixing solutions a, the concentration range of noble metal halide is: 1 ~ 10mg/mL.
4. the making method of luminous Janus colloid according to claim 2, is characterized in that, in described mixing solutions a, the mass ratio of four octyl group brometo de amonios and noble metal halide is: 1:2 ~ 10.
5. the making method of luminous Janus colloid according to claim 1, is characterized in that, described precious metal is the one in Au, Ag, Pt, Pd.
6. the making method of luminous Janus colloid according to claim 1, it is characterized in that, described alkylamino radical toluene is the one in octane carbaryl, decane carbaryl, n-Laurylamine toluene, tetradecylamine toluene, cetylamine toluene and octadecylamine toluene.
7. the making method of luminous Janus colloid according to claim 1, is characterized in that, in described step B, quantum dot precursor preparation process is as follows:
CdSe/CdS quantum dot toluene solution and Octadecane base phosphoric acid are mixed to form quantum dot presoma.
8. the making method of luminous Janus colloid according to claim 1, is characterized in that, in described step B, described UV-light is wavelength is 254 ~ 400nm.
9. a luminous Janus colloid, is characterized in that, adopts the making method as described in any one of claim 1 ~ 8 to make.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108913143A (en) * | 2018-07-03 | 2018-11-30 | 山东交通学院 | A kind of preparation method and application of organometallic polymer load Au doped quantum dot composite material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108913143A (en) * | 2018-07-03 | 2018-11-30 | 山东交通学院 | A kind of preparation method and application of organometallic polymer load Au doped quantum dot composite material |
| CN108913143B (en) * | 2018-07-03 | 2021-03-09 | 山东交通学院 | Preparation method and application of metal organic polymer loaded Au-doped quantum dot composite material |
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Application publication date: 20160420 |