CN102533257B - Surface-modified ZnO quantum dot and preparation method thereof - Google Patents
Surface-modified ZnO quantum dot and preparation method thereof Download PDFInfo
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- CN102533257B CN102533257B CN201010608802.2A CN201010608802A CN102533257B CN 102533257 B CN102533257 B CN 102533257B CN 201010608802 A CN201010608802 A CN 201010608802A CN 102533257 B CN102533257 B CN 102533257B
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- quantum dot
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- silane coupling
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 51
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 36
- 235000013904 zinc acetate Nutrition 0.000 claims description 36
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 25
- 239000004246 zinc acetate Substances 0.000 claims description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 238000013019 agitation Methods 0.000 claims description 17
- 238000006703 hydration reaction Methods 0.000 claims description 11
- DJWUNCQRNNEAKC-UHFFFAOYSA-L zinc acetate Chemical class [Zn+2].CC([O-])=O.CC([O-])=O DJWUNCQRNNEAKC-UHFFFAOYSA-L 0.000 claims description 11
- 230000036571 hydration Effects 0.000 claims description 7
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 6
- 229960004756 ethanol Drugs 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 6
- 229910052744 lithium Inorganic materials 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-O oxonium Chemical compound [OH3+] XLYOFNOQVPJJNP-UHFFFAOYSA-O 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 3
- 230000003000 nontoxic effect Effects 0.000 abstract description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical class [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 abstract 4
- XKKVXDJVQGBBFQ-UHFFFAOYSA-L zinc ethanol diacetate Chemical compound C(C)O.C(C)(=O)[O-].[Zn+2].C(C)(=O)[O-] XKKVXDJVQGBBFQ-UHFFFAOYSA-L 0.000 abstract 3
- NHNKWEHVEHQUDE-UHFFFAOYSA-M lithium ethanol hydroxide Chemical compound [Li+].[OH-].CCO NHNKWEHVEHQUDE-UHFFFAOYSA-M 0.000 abstract 2
- 238000003760 magnetic stirring Methods 0.000 abstract 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 230000004048 modification Effects 0.000 abstract 1
- 238000012986 modification Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 13
- 230000005855 radiation Effects 0.000 description 11
- 238000003860 storage Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 239000003086 colorant Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 229910004613 CdTe Inorganic materials 0.000 description 1
- 238000000018 DNA microarray Methods 0.000 description 1
- 230000005640 de Broglie wave Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 238000001215 fluorescent labelling Methods 0.000 description 1
- 230000001795 light effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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Abstract
The invention relates to a surface-modified ZnO quantum dot, which is a surface-modified ZnO quantum dot subjected to surface modification by a silane coupling agent; the preparation method comprises the following steps: firstly, preparing a zinc acetate ethanol solution stabilized by a silane coupling agent, then adding the silane coupling agent, and preparing the zinc acetate ethanol solution stabilized by the silane coupling agent under magnetic stirring; then preparing a lithium hydroxide ethanol solution, finally adding the lithium hydroxide ethanol solution into a zinc acetate ethanol solution stabilized by a silane coupling agent, and preparing colorless and transparent ZnO quantum dots modified by the surface of the silane coupling agent under magnetic stirring; the quantum dot has the characteristics of high fluorescence intensity and good stability, and the luminescent wavelength of the ZnO quantum dot with the modified surface can be adjusted and is nontoxic; and the preparation method has simple process and low cost, and is beneficial to realizing industrial production.
Description
Technical field
The present invention relates to a kind of ZnO quantum dot and preparation method thereof, be particularly related to ZnO quantum dot of a kind of finishing and preparation method thereof, more particularly, the present invention relates to the ZnO quantum dot and preparation method thereof of the adjustable finishing of a kind of fluorescence radiation intensity, high stability and emission wavelength with enhancing.
Background technology
After semiconductor material is gradually reduced to certain critical size mutually from body, the characteristic dimension of material in three dimensions all with the de Broglie wave of electronics or electron mean free path is comparable or more hour, the motion of electronics in material is subject to three-dimensional restriction, the energy that is to say electronics is all quantized in three dimensions, we this electronics in three dimensions all restricted material call quantum dot.
The research of semiconductor-quantum-point is an emerging field in solid luminescent material, relates to multi-disciplinary intersection.Quantum technology comes from 20 century 70s the earliest, it is found that, when semiconductor material is reduced to nano-scale, it is compared with massive material has unique optical characteristics.
Quantum dot is as a kind of state-of-the art fluorescent material, and it is compared and have multiple advantage with traditional fluorescent material, mainly contains 3 points:
(1) quantum dot of single kind can produce the monochromatic ray of different colours according to dimensional change, white light even, and this is that conventional fluorescent powder cannot be realized at all;
(2) advantages such as quantum dot has exciting light spectrum width and continuous distribution, and emmission spectrum monochromaticity is good;
(3) particle diameter of quantum dot is very little, only has several nanometers, can avoid the caused scattering of light effect of conventional fluorescent powder completely.
Therefore, utilize quantum dot to substitute conventional fluorescent powder significant as fluorescent material.
Semiconductor-quantum-point, as a kind of novel fluorescent material, is widely used in fields such as biological fluorescent labeling, photodiode fluorescent material, biochip, laser apparatus, opto-electronic device, solar cell, nonlinear optical material, photochromicss.
Although study at present the good luminous performance such as the most ripe CdSe quantum dot, CdTe quantum dot in quantum dot, toxicity is too large, cost is higher, has seriously limited its practical application.ZnO quantum dot is because the significant advantage that it is nontoxic, cost is low causes investigator's extensive concern.But the ZnO quantum dot luminous intensity of having reported is at present low, poor stability, visible region emission wavelength regulation range is very narrow.
Summary of the invention
The object of the invention is to provide that a kind of fluorescence radiation intensity is high, good stability and can realize the ZnO quantum dot of multicolor luminous finishing;
Another object of the present invention is to provide the preparation method of the ZnO quantum dot of above-mentioned finishing.
Technical scheme of the present invention is as follows:
The ZnO quantum dot of finishing provided by the invention, its finishing ZnO quantum dot for carrying out finishing through silane coupling agent, its particle diameter is less than 10nm.
The preparation method of the ZnO quantum dot of finishing provided by the invention, its finishing ZnO quantum dot for carrying out finishing through silane coupling agent, its preparation process is as follows:
(1) preparation is through the stable zinc acetate ethanolic soln of silane coupling agent
Two hydration zinc acetates are joined in dehydrated alcohol under magnetic agitation, be heated to 80 ℃ of condensing reflux 1-5h, obtaining concentration is the zinc acetate ethanolic soln of 0.1mol/L;
Zinc acetate ethanolic soln is chilled to 0 ℃ in advance, then adds silane coupling agent, magnetic agitation 15-60min, obtains through the stable zinc acetate ethanolic soln of silane coupling agent;
The weight part proportioning of described silane coupling agent and two hydration zinc acetates is 40-80: 60-20.
(2) prepare the ZnO quantum dot of silane coupling agent finishing
One hydronium(ion) oxidation lithium is joined in ethanol, ultrasonic dissolution, obtaining concentration is the lithium hydroxide ethanolic soln of 0.1-0.35mol/L;
Lithium hydroxide ethanolic soln is joined in the stable zinc acetate ethanolic soln of silane coupling agent, and magnetic agitation 30min, makes the ZnO quantum dot that water white particle diameter is less than the silane coupling agent finishing of 10nm.
Compared with prior art, the ZnO quantum dot of finishing of the present invention and method for making tool have the following advantages:
1, the ZnO quantum dot of finishing of the present invention is nontoxic, has overcome the large outstanding problems of traditional quantum dot toxicity such as CdSe;
2, the ZnO quantum dot fluorescence radiation intensity of finishing of the present invention is high, has solved the low problem of common ZnO quantum dot fluorescence intensity;
3, the ZnO quantum dot stability of finishing of the present invention is high, has solved the problem of common ZnO quantum dot poor stability;
4, the ZnO quantum dot of finishing of the present invention can be prepared the ZnO quantum dot of different glow colors easily, has improved the controllability of ZnO quantum dot emission wavelength;
5, preparation method's technique of the ZnO quantum dot of finishing of the present invention is simple, with low cost, is beneficial to and realizes suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the fluorescence radiation spectrum schematic diagram of the ZnO quantum dot (a) of not finishing and the ZnO quantum dot (b) of finishing;
Fig. 2 is 3 weeks front and back fluorescence intensity contrast schematic diagram of ZnO quantum dot room temperature storage of not finishing;
Fig. 3 is 3 weeks front and back fluorescence intensity contrast schematic diagram of ZnO quantum dot room temperature storage of finishing;
Fig. 4 is the infrared spectrogram of ZnO quantum dot of ZnO quantum dot, silane coupling agent and the silane coupling agent finishing of not finishing;
Fig. 5 is the high-resolution-ration transmission electric-lens figure of the ZnO quantum dot of finishing of the present invention.
Embodiment
Below by specific embodiment and comparative example, further illustrate the present invention:
Embodiment 1
0.439g bis-hydration zinc acetates are added in 20mL dehydrated alcohol under magnetic agitation, be heated to 80 ℃ of condensing reflux 2h, obtain the zinc acetate ethanolic soln of 0.1mol/L;
Zinc acetate ethanolic soln is chilled to 0 ℃ in advance, then adds 0.293g silane coupling agent, magnetic agitation 60min, obtains the stable zinc acetate ethanolic soln of silane coupling agent.
0.0839g mono-hydronium(ion) oxidation lithium is joined in 20mL ethanol, ultrasonic dissolution, obtaining concentration is the lithium hydroxide ethanolic soln of 0.1mol/L;
Lithium hydroxide ethanolic soln is joined in the stable zinc acetate ethanolic soln of silane coupling agent, and magnetic agitation 30min, makes the ZnO quantum dot of the water white silane coupling agent finishing of the present embodiment.The median size of this ZnO quantum dot is 3nm, and fluorescence radiation peak position is 497nm, is green fluorescence, and its fluorescence radiation intensity is high, good stability.In this embodiment, the weight part proportioning of silane coupling agent and two hydration zinc acetates is 40: 60.
Fig. 5 is the high-resolution-ration transmission electric-lens figure of the ZnO quantum dot of the prepared finishing of embodiment 1, as seen from the figure: the ZnO quantum dot particle diameter of prepared finishing is less than 10nm.
Embodiment 2
0.439g bis-hydration zinc acetates are added in 20mL dehydrated alcohol under magnetic agitation, be heated to 80 ℃ of condensing reflux 5h, obtain the zinc acetate ethanolic soln of 0.1mol/L;
Zinc acetate ethanolic soln is chilled to 0 ℃ in advance, then adds 0.6g silane coupling agent, magnetic agitation 15min, obtains the stable zinc acetate ethanolic soln of silane coupling agent.
0.1175g mono-hydronium(ion) oxidation lithium is joined in 20mL ethanol, ultrasonic dissolution, obtaining concentration is the lithium hydroxide ethanolic soln of 0.14mol/L;
Lithium hydroxide ethanolic soln is joined in the stable zinc acetate ethanolic soln of silane coupling agent, and magnetic agitation 30min, makes the ZnO quantum dot of the water white silane coupling agent finishing of the present embodiment.The median size of this ZnO quantum dot is 2nm, and fluorescence radiation peak position is 458nm, is blue-fluorescence, and its fluorescence radiation intensity is high, good stability.In this embodiment, the weight part proportioning of silane coupling agent and two hydration zinc acetates is 58: 42.
Embodiment 3
0.439g bis-hydration zinc acetates are added in 20mL dehydrated alcohol under magnetic agitation, be heated to 80 ℃ of condensing reflux 1h, obtain the zinc acetate ethanolic soln of 0.1mol/L;
Zinc acetate ethanolic soln is chilled to 0 ℃ in advance, then adds 1.75g silane coupling agent, magnetic agitation 30min, obtains the stable zinc acetate ethanolic soln of silane coupling agent.
0.2937g mono-hydronium(ion) oxidation lithium is joined in 20mL ethanol, ultrasonic dissolution, obtaining concentration is the lithium hydroxide ethanolic soln of 0.35mol/L;
Lithium hydroxide ethanolic soln is joined in the stable zinc acetate ethanolic soln of silane coupling agent, and magnetic agitation 30min, makes the ZnO quantum dot of the water white silane coupling agent finishing of the present embodiment.The median size of this ZnO quantum dot is 1nm, and fluorescence radiation peak position is 386nm, is purple fluorescence, and its fluorescence radiation intensity is high, good stability.In this embodiment, the weight part proportioning of silane coupling agent and two hydration zinc acetates is 80: 20.
As shown in table 1, from embodiment 1-3, the method for the invention can make the ZnO quantum dot of the finishing with different glow colors.From each embodiment, the method technique of the ZnO quantum dot of described preparation finishing is simple, easy to operate, with low cost, is beneficial to and realizes suitability for industrialized production.
Table 1
One comparative example is provided below:
0.439g bis-hydration zinc acetates are added in 20mL dehydrated alcohol under magnetic agitation, be heated to 80 ℃ of condensing reflux 2h, obtain the zinc acetate ethanolic soln of 0.1mol/L, then zinc acetate ethanolic soln is chilled to 0 ℃ in advance;
0.0839g mono-hydronium(ion) oxidation lithium is joined in 20mL ethanol, ultrasonic dissolution, obtaining concentration is the lithium hydroxide ethanolic soln of 0.1mol/L; Lithium hydroxide ethanolic soln is joined in zinc acetate ethanolic soln, and magnetic agitation 30min, makes the water white common ZnO quantum dot of this comparative example.
Above-mentioned comparative example is all identical with embodiment 1 at each preparation parameter and processing condition, but do not add the common ZnO quantum dot of preparing under the condition of silane coupling agent, the ZnO quantum dot of finishing prepared by the common ZnO quantum dot that this comparative example makes and method of the present invention contrasts, and its result is as follows:
In Fig. 1, a curve is the fluorescence spectrum of the common ZnO quantum dot of not finishing, and b curve is the fluorescence spectrum of the ZnO quantum dot of finishing of the present invention.As can be seen from Figure 1: the fluorescence intensity of the ZnO quantum dot of finishing of the present invention is approximately 5 times of common ZnO quantum dot of not finishing.
Fig. 2 is the comparison diagram of 3 weeks front and back fluorescence intensities of ZnO quantum dot room temperature storage of not finishing.As seen from the figure, after room temperature storage 3 weeks, the fluorescence of the ZnO quantum dot of finishing does not disappear substantially.
Fig. 3 is the comparison diagram through 3 weeks front and back fluorescence intensities of ZnO quantum dot room temperature storage of silane coupling agent finishing.As seen from the figure, after room temperature storage 3 weeks, the ZnO quantum dot fluorescence intensity of finishing is substantially constant.
As from the foregoing, by silane coupling agent finishing, can significantly strengthen the fluorescence radiation intensity of ZnO quantum dot, can significantly improve its stability simultaneously;
In addition, Fig. 4 is the infrared spectrogram of ZnO quantum dot of ZnO quantum dot, silane coupling agent and the silane coupling agent finishing of not finishing; Wherein, a is the infrared spectrogram of the ZnO quantum dot of not finishing, the infrared spectrogram that b is silane coupling agent, and c is the infrared spectrogram of the ZnO quantum dot of silane coupling agent finishing; As seen from the figure, the characteristic peak that occurs silane coupling agent in the infrared spectrogram of the ZnO quantum dot of silane coupling agent finishing, therefore visible silane coupling agent has successfully been modified ZnO quantum dot surface, and prepared ZnO quantum dot is the ZnO quantum dot through silane coupling agent finishing.
Claims (1)
1. a preparation method for the ZnO quantum dot of finishing, the finishing ZnO quantum dot of the ZnO quantum dot of described finishing for carrying out finishing through silane coupling agent, its preparation process is as follows:
(1) preparation is through the stable zinc acetate ethanolic soln of silane coupling agent
Two hydration zinc acetates are joined in dehydrated alcohol under magnetic agitation, be heated to 80 ℃ of condensing reflux 1-5h, obtaining concentration is the zinc acetate ethanolic soln of 0.1mol/L;
Zinc acetate ethanolic soln is chilled to 0 ℃ in advance, then adds silane coupling agent, magnetic agitation 15-60min, obtains through the stable zinc acetate ethanolic soln of silane coupling agent;
The weight part proportioning of described silane coupling agent and two hydration zinc acetates is 40-80:60-20;
(2) prepare the ZnO quantum dot of silane coupling agent finishing
One hydronium(ion) oxidation lithium is joined in ethanol, ultrasonic dissolution, obtaining concentration is the lithium hydroxide ethanolic soln of 0.1-0.35mol/L;
Lithium hydroxide ethanolic soln is joined in the stable zinc acetate ethanolic soln of silane coupling agent, and magnetic agitation 30min, makes the ZnO quantum dot that water white particle diameter is less than the silane coupling agent finishing of 10nm.
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| CN105268423A (en) * | 2015-09-08 | 2016-01-27 | 陕西科技大学 | ZnO quantum dot-MMT composite photocatalytic material and preparation method |
| FR3053353B1 (en) * | 2016-06-30 | 2018-07-27 | Aledia | PROCESS FOR PRODUCING PHOTOLUMINESCENT PARTICLES |
| CN107384367B (en) * | 2017-06-19 | 2020-06-09 | 江苏大学 | Method for preparing melamine molecular imprinting fluorescence sensor MEL-MIP by using ZnO quantum dot/porous silicon fluorescent material |
| CN108611088A (en) * | 2018-05-22 | 2018-10-02 | 温州大学苍南研究院 | A kind of method that sonochemical method prepares ZnO quantum dot |
| CN111994943A (en) * | 2020-08-10 | 2020-11-27 | 武汉大学 | Synthesis method of silanized zinc oxide quantum dots with uniform size |
| CN116285948A (en) * | 2023-02-22 | 2023-06-23 | 徐州工程学院 | Preparation method of melamine resin coated zinc oxide quantum dot composite fluorescent powder |
| CN116285960A (en) * | 2023-03-08 | 2023-06-23 | 郑州大学 | Preparation method of large-size transparent scintillator |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1657415A (en) * | 2005-02-02 | 2005-08-24 | 苏州大学 | Preparation method of nanometer zinc oxide |
| WO2009041596A1 (en) * | 2007-09-28 | 2009-04-02 | Dai Nippon Printing Co., Ltd. | Electroluminescent device |
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| CN1657415A (en) * | 2005-02-02 | 2005-08-24 | 苏州大学 | Preparation method of nanometer zinc oxide |
| WO2009041596A1 (en) * | 2007-09-28 | 2009-04-02 | Dai Nippon Printing Co., Ltd. | Electroluminescent device |
Non-Patent Citations (2)
| Title |
|---|
| Glass transition temperature changes of melt-blended polymer nanocomposites containing finely dispersed ZnO quantum dots;Minhao Wong, et al.;《Soft Matter》;20100806;第6卷;第4482–4490页 * |
| Minhao Wong, et al..Glass transition temperature changes of melt-blended polymer nanocomposites containing finely dispersed ZnO quantum dots.《Soft Matter》.2010,第6卷 |
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