CN103694994A - Pure-organic long-afterglow composite material and preparation method thereof - Google Patents
Pure-organic long-afterglow composite material and preparation method thereof Download PDFInfo
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- CN103694994A CN103694994A CN201410012241.8A CN201410012241A CN103694994A CN 103694994 A CN103694994 A CN 103694994A CN 201410012241 A CN201410012241 A CN 201410012241A CN 103694994 A CN103694994 A CN 103694994A
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Abstract
The invention discloses a pure-organic long-afterglow composite material and a preparation method thereof, belongs to the technical field of luminescent materials and is used for solving the problems that the preparation process of a long-afterglow luminescent material is complex, potential toxicity exists in the preparation process, and preparation raw materials are scarce in the prior art. The preparation method comprises the following steps of pyrolyzing ethylene diamine tetraacetic acid disodium for 2-4 hours at 200-400 DEG C in inert atmosphere so as to obtain black fluffy solids, carrying out ultrasonic dissolving on the black fluffy solids, carrying out centrifuging to remove black precipitates, taking an upper-layer tan clear solution as a water solution of carbon nanodots, finally adequately mixing the water solution of the carbon nanodots with a polyvinyl alcohol water solution, and drying to obtain the pure-organic long-afterglow composite material. The pure-organic long-afterglow composite material has the advantages that the afterglow decay time can reach multiple seconds, and the material is non-toxic, is good in biocompatibility and can be applied to the field of biological medicines.
Description
Technical field
The invention belongs to luminescent material technical field, be specifically related to a kind of pure organic steady persistence matrix material and preparation method thereof.
Background technology
Long after glow luminous material refers to still can be luminous after excitation light irradiation stops, and have compared with the material of steady persistence time.Existing long after glow luminous material comprises radioactive rays excitated type and sulfide type.Radioactive rays excitated type is that to mix the quantity of radiant energy that the radiating material in material sends be excitaton source, and stimulated luminescence center is and luminous, and this class material is harmful to environment and human health owing to containing radioactive substance, by most countries, has been prohibited use; Sulfide type comprises ZnS, CaS etc., but this class material is due to easily hydrolysis or photodissociation under moisture and ultraviolet effect, so chemical property less stable comparatively speaking, work-ing life is shorter.
Most widely used long after glow luminous material is to take aluminate stupalith as matrix at present, in order to form prepared by the doped element of luminescence center and Trapping Centers to take rare earth material, this material has overcome the short technical problem of sulfide type material lifetime, there is good night display function, add after adhesives, can make and show or trim component various forms of nights.But this long-afterglow material is water insoluble, during fabricate devices, need to pass through special processing, and be distributed in organic solvent, technique is comparatively complicated, and there is certain toxicity in the organic solvent volatile matter producing in treating processes.In addition, it adopts rare earth material as doped element, has caused the consumption of nonrenewable resources.
Carbon material is that a kind of green, environmental protection, reserves are abundant, reproducible material.Carbon nano dot owing to thering is chemical stability, without optical flare, fast lightly float, the advantage of nontoxic, excellent many uniquenesses such as biocompatibility is subject to increasing concern (LuminescentCarbonNanodots:EmergentNanolights, SheilaN.Baker, GaryA.Baker, Angew.Chem.Int.Ed., 2010,49,6726).
Summary of the invention
The object of the invention is to solve that the remaining luminous brightness material preparation process of existing length is complicated, preparation process exists genotoxic potential and the rare problem of raw materials, the invention provides a kind of pure organic steady persistence matrix material and preparation method thereof.
The preparation method of pure organic steady persistence matrix material of the present invention, comprises the following steps:
(1), under inert atmosphere, at 200-400 ℃ of pyrolysis disodium ethylene diamine tetraacetate 2-4h, obtain the fluffy solid of black;
(2), by the fluffy solid ultrasonic dissolution of black, centrifugal removal black precipitate, gets upper strata brown color clear liquid, is the aqueous solution of carbon nano dot;
(3) aqueous solution of carbon nano dot is fully mixed with polyvinyl alcohol water solution, obtain mixing solutions, after mixing solutions is dry, obtain pure organic steady persistence matrix material;
In described mixing solutions, the mass ratio of carbon nano dot and polyvinyl alcohol is 1:50-1:500.
Preferably, described centrifugal rotational speed is 3000-10000rpm, and centrifugation time is 10-20min.
Preferably, described drying temperature is 60-90 ℃.
Pure organic steady persistence matrix material that the present invention also provides the preparation method of above-mentioned pure organic steady persistence matrix material to prepare.
Beneficial effect of the present invention:
(1) the present invention is purified and is obtained oxidized carbon nano-particle by high temperature pyrolysis disodium ethylene diamine tetraacetate, the carbon nano-particle surface of preparation has abundant carbon-oxygen bond, make it have between high photoluminescence quantum efficiencies and singlet-triplet state system and pass through probability, after compound with polyvinyl alcohol, the material decay of afterglow time can reach the several seconds, nontoxic, good biocompatibility, can be applied to the aspects such as biological and medical science;
(2) simple, the asepsis environment-protecting of preparation technology of the present invention, has overcome the consumption that prior art is used the Nonrenewable resources that rare earth causes.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope figure of the carbon nano dot of the embodiment of the present invention 1;
Fig. 2 is the carbon nano dot aqueous solution, the fluorescence spectrum figure of matrix material and the phosphorescence spectrum figure of matrix material of the embodiment of the present invention 1.
Fig. 3 is the phosphorescence temporal resolution spectrogram of the matrix material of the embodiment of the present invention 1 preparation.
Embodiment
The preparation method of pure organic steady persistence matrix material, comprises the following steps:
(1), under inert atmosphere, at 200-400 ℃ of pyrolysis disodium ethylene diamine tetraacetate 2-4h, obtain the fluffy solid of black;
(2) by the fluffy solid ultrasonic dissolution of black, centrifugal 3000-10000rpm, centrifugation time 10-20min, remove black precipitate, get upper strata brown color clear liquid, be the aqueous solution of carbon nano dot, wherein, the surface of carbon nano dot is partially oxidized, has abundant carbon-oxygen bond;
(3) aqueous solution of carbon nano dot is fully mixed with polyvinyl alcohol water solution, obtain mixing solutions, in mixing solutions, the mass ratio of carbon nano dot and polyvinyl alcohol is 1:50-1:500, after dry by mixing solutions 60-90 ℃, obtain pure organic steady persistence matrix material.
In present embodiment, the concentration of aqueous solution of carbon nano dot is 2mg/ml, polyvinyl alcohol water solution concentration 10wt%.
Pure organic steady persistence matrix material that the present invention also provides above-mentioned preparation method to prepare.
Below in conjunction with embodiment and accompanying drawing, further illustrate the present invention.
Embodiment 1
The crucible that 1.6 grams of ethylenediamine tetraacetic acid (EDTA)s are housed is put into tube furnace, at nitrogen atmosphere, 400 ℃, keep 4h, the complete pyrolysis of disodium ethylene diamine tetraacetate, obtains the fluffy solid of black; The fluffy solid of this black is dissolved in 80ml water by ultrasonic assisting, more centrifugal (9500rpm, 10min) removal macrobead, obtain the brown color aqueous solution, purify and obtain the aqueous solution of carbon nano dot; Configuration quality mark is the polyvinyl alcohol water solution of 10wt%, and solution and the 5ml polyvinyl alcohol water solution of the carbon nano dot water that is 2mg/ml by 1ml concentration fully mix, and obtain mixing solutions, mixing solutions in 60 ℃ dry, obtain pure organic steady persistence matrix material.
Ultraviolet lamp matrix material for (wavelength is 365nm) of embodiment 1 preparation is irradiated, and observation can be sent cold white light, still has the green glow that continues the several seconds after turning off ultraviolet lamp, illustrates that matrix material prepared by embodiment 1 has steady persistence character.
Fig. 1 is the transmission electron microscope figure of the carbon nano dot that obtains after dry of the aqueous solution of carbon nano dot of embodiment 1 preparation, and as can be seen from Figure 1, the median size of carbon nano dot is at 5nm; Fig. 2 is the carbon nano dot aqueous solution, the fluorescence spectrum figure of matrix material and the phosphorescence spectrum figure of matrix material of embodiment 1, wherein, curve 1 is the fluorescence spectrum figure of the carbon nano dot aqueous solution, the fluorescence spectrum figure that curve 2 is matrix material, the phosphorescence spectrum figure that curve 3 is matrix material, as can be seen from Figure 2, the luminous covering of the phosphorescence 400-600nm scope of matrix material, peak position is at 500nm, Fig. 3 is the phosphorescence temporal resolution spectrogram of the matrix material of embodiment 1, as can be seen from Figure 3, the matrix material lighting time interval of embodiment 1 preparation reaches 4s.
The crucible that 1.6 grams of ethylenediamine tetraacetic acid (EDTA)s are housed is put into tube furnace, at nitrogen atmosphere, 200 ℃, keep 2h, the complete pyrolysis of disodium ethylene diamine tetraacetate, obtains the fluffy solid of black; The fluffy solid of this black is dissolved in 80ml water by ultrasonic assisting, more centrifugal (3000rpm, 20min) removal macrobead, obtain the brown color aqueous solution, purify and obtain the aqueous solution of carbon nano dot; Configuration quality mark is the polyvinyl alcohol water solution of 10wt%, and the carbon nano dot aqueous solution that is 2mg/ml by 1ml concentration and 1ml polyvinyl alcohol water solution fully mix, and obtain mixing solutions, mixing solutions in 90 ℃ dry, obtain pure organic steady persistence matrix material.
Ultraviolet lamp matrix material for (wavelength is 365nm) of embodiment 2 preparation is irradiated, and observation can be sent cold white light, still has the green glow that continues the several seconds after turning off ultraviolet lamp, illustrates that matrix material prepared by embodiment 2 has steady persistence character.
The crucible that 1.6 grams of ethylenediamine tetraacetic acid (EDTA)s are housed is put into tube furnace, at nitrogen atmosphere, 300 ℃, keep 3h, the complete pyrolysis of disodium ethylene diamine tetraacetate, obtains the fluffy solid of black; The fluffy solid of this black is dissolved in 80ml water by ultrasonic assisting, more centrifugal (5000rpm, 10min) removal macrobead, obtain the brown color aqueous solution, purify and obtain the aqueous solution of carbon nano dot; Configuration quality mark is the polyvinyl alcohol water solution of 10wt%, and the carbon nano dot aqueous solution that is 2mg/ml by 1ml concentration and 10ml polyvinyl alcohol water solution fully mix, and obtain mixing solutions, mixing solutions in 80 ℃ dry, obtain pure organic steady persistence matrix material.
Ultraviolet lamp matrix material for (wavelength is 365nm) of embodiment 3 preparation is irradiated, and observation can be sent cold white light, still has the green glow that continues the several seconds after turning off ultraviolet lamp, illustrates that matrix material prepared by embodiment 3 has steady persistence character.
Obviously, the explanation of above embodiment is just for helping to understand method of the present invention and core concept thereof.It should be pointed out that the those of ordinary skill for described technical field, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of the claims in the present invention.
Claims (4)
1. the preparation method of pure organic steady persistence matrix material, is characterized in that, comprises the following steps:
(1), under inert atmosphere, at 200-400 ℃ of pyrolysis disodium ethylene diamine tetraacetate 2-4h, obtain the fluffy solid of black;
(2), by the fluffy solid ultrasonic dissolution of black, centrifugal removal black precipitate, gets upper strata brown color clear liquid, is the aqueous solution of carbon nano dot;
(3) aqueous solution of carbon nano dot is fully mixed with polyvinyl alcohol water solution, obtain mixing solutions, after mixing solutions is dry, obtain pure organic steady persistence matrix material;
In described mixing solutions, the mass ratio of carbon nano dot and polyvinyl alcohol is 1:50-1:500.
2. the preparation method of pure organic steady persistence matrix material according to claim 1, is characterized in that, described centrifugal rotational speed is 3000-10000rpm, and centrifugation time is 10-20min.
3. the preparation method of pure organic steady persistence matrix material according to claim 1, is characterized in that, described drying temperature is 60-90 ℃.
4. pure organic steady persistence matrix material that prepared by the preparation method of the pure organic steady persistence matrix material of claim 1-3 described in any one.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105838364A (en) * | 2016-04-29 | 2016-08-10 | 济南大学 | Method for preparing fluorescent carbon dots by pyrolyzing ammonium carboxylate |
| CN106497560A (en) * | 2016-08-29 | 2017-03-15 | 北京化工大学 | Controllable carbon point based compound nano material of luminescent properties and preparation method and application |
| CN108587600A (en) * | 2018-03-28 | 2018-09-28 | 中国科学院长春光学精密机械与物理研究所 | Room temperature phosphorimetry composite material, preparation method and application based on carbon nano dot |
| CN109111919A (en) * | 2018-09-30 | 2019-01-01 | 湖北大学 | A kind of preparation method of the manganese ion doping carbon quantum dot of complete water-soluble products |
| CN110951486A (en) * | 2019-04-30 | 2020-04-03 | 江南大学 | Light-adjustable room-temperature phosphorescent carbon dot material and preparation method and application thereof |
| CN114410299A (en) * | 2022-01-27 | 2022-04-29 | 郑州大学 | Carbon dot and preparation method of carbon dot-based composite material |
-
2014
- 2014-01-10 CN CN201410012241.8A patent/CN103694994A/en active Pending
Non-Patent Citations (2)
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| DENGYU PAN ET AL.: "Observation of pH-, solvent-, spin-, and excitation-dependent blue photoluminescence from carbon nanoparticles", 《CHEM. COMMUN.》 * |
| YEHAO DENG ET AL.: "Long lifetime pure organic phosphorescence based on water soluble carbon dots", 《CHEM. COMMUN.》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105838364A (en) * | 2016-04-29 | 2016-08-10 | 济南大学 | Method for preparing fluorescent carbon dots by pyrolyzing ammonium carboxylate |
| CN106497560A (en) * | 2016-08-29 | 2017-03-15 | 北京化工大学 | Controllable carbon point based compound nano material of luminescent properties and preparation method and application |
| CN108587600A (en) * | 2018-03-28 | 2018-09-28 | 中国科学院长春光学精密机械与物理研究所 | Room temperature phosphorimetry composite material, preparation method and application based on carbon nano dot |
| CN108587600B (en) * | 2018-03-28 | 2019-12-27 | 中国科学院长春光学精密机械与物理研究所 | Room-temperature phosphorescent composite material based on carbon nanodots, and preparation method and application thereof |
| CN109111919A (en) * | 2018-09-30 | 2019-01-01 | 湖北大学 | A kind of preparation method of the manganese ion doping carbon quantum dot of complete water-soluble products |
| CN110951486A (en) * | 2019-04-30 | 2020-04-03 | 江南大学 | Light-adjustable room-temperature phosphorescent carbon dot material and preparation method and application thereof |
| CN110951486B (en) * | 2019-04-30 | 2020-12-29 | 江南大学 | Light-adjustable room-temperature phosphorescent carbon dot material and preparation method and application thereof |
| CN114410299A (en) * | 2022-01-27 | 2022-04-29 | 郑州大学 | Carbon dot and preparation method of carbon dot-based composite material |
| CN114410299B (en) * | 2022-01-27 | 2023-09-26 | 郑州大学 | Carbon dot and preparation method of carbon dot-based composite material |
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Application publication date: 20140402 |