CN106497560B - The controllable carbon dots based compound nano material and the preparation method and application thereof of luminescent properties - Google Patents
The controllable carbon dots based compound nano material and the preparation method and application thereof of luminescent properties Download PDFInfo
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Abstract
The present invention provides a kind of carbon dots based compound nano material and the preparation method and application thereof that luminescent properties are controllable.Cyanuric acid is added by having to surface modification in the carbon quantum dot aqueous solution of carboxylic group, or alkali metal hydroxide and cyanuric acid is added, gained mixed liquor is agitated, centrifuges, and collects precipitation, is freeze-dried up to the controllable carbon dots based compound nano material of luminescent properties.The present invention preparation process is simple, at low cost, asepsis environment-protecting.By adjusting pH value, the fluorescence radiation efficiency of material can not only be greatly improved, and color and the service life of material sunset glow can be changed, there is important application value in anti-fake, bio-sensing and the fields such as display and illumination.
Description
Technical field
The present invention relates to material engineering fields, specifically, being related to a kind of carbon dots base composite nano that luminescent properties are controllable
Material and the preparation method and application thereof.
Background technology
Carbon quantum dot is that the grain size of discovered in recent years being made of the near-spherical particle disperseed is below with hair in 10nm
The carbon particle of light property.Since self-discovery, due to itself unique performance, the great interest of numerous researchers has been caused.Carbon amounts
Son point has the excellent properties different from traditional quantum dot, such as luminescence generated by light, low toxicity, chemical inertness and good biocompatibility,
It has broad application prospects in opto-electronic device, biological detection, medicine and other fields.Wherein of greatest concern is its photic hair
Light characteristic.But the carbon dots based compound nano material that they prepare, due to being influenced by carbon dots intrinsic property, luminescent properties are
It is uncontrollable.Therefore, the controllable carbon dots based compound nano material of luminescent properties is realized by simple method, can substantially reduce life
Produce cost.
Invention content
The present invention is complicated for optical material preparation process in the prior art, prepares that raw material is rare and optical property can not
The problems such as control, provides a kind of carbon dots based compound nano material and preparation method thereof that luminescent properties are controllable.
It is a further object of the present invention to provide the applications of the controllable carbon dots based compound nano material of the luminescent properties.
In order to realize that the object of the invention, the present invention provide the preparation side of the controllable carbon dots based compound nano material of luminescent properties
Method, the method are cyanuric acid to be added into the carbon quantum dot aqueous solution that surface modification has carboxylic group, or alkali gold is added
Belong to hydroxide and cyanuric acid, gained mixed liquor is agitated, centrifuges, and collects precipitation, is freeze-dried controllable up to luminescent properties
Carbon dots based compound nano material.
The surface modification, which can be prepared as follows, the carbon quantum dot aqueous solution of carboxylic group：
(1) by folic acid and citric acid in mass ratio 1:0.1-10 dissolves in deionized water, and the mass ratio of folic acid and water is
1:50-1000 obtains mixed liquor I；
(2) mixed liquor obtained by (1) is placed in polytetrafluoroethylene (PTFE) high pressure sealing tank, heating or microwave at 150~300 DEG C
1~5h is reacted, solution II is obtained；
(3) solution II for obtaining (2) centrifuges 5~30min at 3000~10000rpm, takes supernatant, with retention point
Bag filter 12~72h of dialysis treatment that son amount is 500-3500Da, obtains fluorescent carbon quantum dot aqueous solution III；
(4) by the freeze-dried 12~96h of (3) acquired solution III, obtaining surface modification has the carbon quantum dot of carboxylic group
Powder；The temperature of freeze-drying is -44 DEG C；
(5) powder obtained by (4) is dissolved in deionized water, is configured to the solution of 0.01-10mg/L, as surface modification has
The carbon quantum dot aqueous solution of carboxylic group.
Alkali metal hydroxide used in the present invention is sodium hydroxide and/or potassium hydroxide.
Method above-mentioned has addition 0.2-2g melamines in the carbon quantum dot aqueous solution of carboxylic group to 8mL surface modifications
Acid and 0-8g alkali metal hydroxides, stirring 2~obtain emulsion for 24 hours.Wherein, cyanuric acid and alkali metal hydroxide rub
You are than being 1：0.01-6.
Method above-mentioned, centrifugal condition are：5000~10000rpm centrifuges 5~20min.
The condition of method above-mentioned, freeze-drying is：- 44 DEG C of 12~96h of freeze-drying.
The present invention also provides the controllable carbon dots based compound nano materials of the luminescent properties prepared according to the above method.Wherein,
The weight percent that carbon quantum dot accounts for the composite nano materials is 0.01%~0.5%.
The present invention also provides the carbon dots based compound nano materials to prepare anti-fake material, biological sensing material, display
Application in material and illuminating material.
The present invention further provides the anti-fake material prepared by the carbon dots based compound nano material, biological sensing material,
Display material and illuminating material.
The present invention has the following advantages：
(1) present invention is adjusted using carbon quantum dot and cyanuric acid as raw material by alkali metal hydroxide (such as sodium hydroxide)
The pH value for saving mixed solution, prepares the controllable carbon dots based compound nano material of luminescent properties.When cyanuric acid and sodium hydroxide
Molar ratio ＜ 3：When 1, composite material sends out blue-fluorescence and blue sunset glow under the ultra violet lamp of 365nm wavelength；Work as hydrogen-oxygen
Change molar ratio >=3 of sodium and cyanuric acid：When 1, composite material sent out under the ultra violet lamp of 365nm wavelength blue-fluorescence and
Yellow sunset glow, and gradually increased with the increase fluorescence quantum yield of sodium hydroxide concentration.
(2) preparation method of the invention is simple, and entire technological process is environmentally protective, need to only adjust the addition of sodium hydroxide
Amount, the pH value by adjusting solution can prepare the luminescent material in fluorescence, Phosphor efficiency different, colorful, different service life.
(3) the controllable carbon dots based compound nano material stability of the luminescent properties that prepare of the present invention is good, long lifespan, sunset glow
Die-away time has important application value up to the several seconds, in fields such as information anti-fake, biomarkers.
Description of the drawings
Fig. 1 is the fluorescence of the composite optical material for preparing under the ultra violet lamp of 365nm wavelength in the embodiment of the present invention 1
Photo (left side) and long afterglow photo (right side)；
Fig. 2 is the composite optical material steady-state fluorescence spectrogram prepared in the embodiment of the present invention 1；
Fig. 3 is the stable state spectrogram that the composite optical material prepared in the embodiment of the present invention 1 measures under phosphorescence pattern；
Fig. 4 is that the composite optical material for preparing is under the excitation of 380nm wavelength in the embodiment of the present invention 1, the sunset glow at 520nm
Attenuation curve figure；
Fig. 5 is the steady-state fluorescence spectrum of the composite optical material for preparing under different excitation wavelengths in the embodiment of the present invention 2
Figure；
Fig. 6 is the stable state spectrogram that the composite optical material prepared in the embodiment of the present invention 2 measures under phosphorescence pattern；
Fig. 7 is that the composite optical material for preparing is under the excitation of 380nm wavelength in the embodiment of the present invention 2, the sunset glow at 520nm
Attenuation curve；
Fig. 8 is the fluorescence of the composite optical material for preparing under the ultra violet lamp of 365nm wavelength in the embodiment of the present invention 3
Photo (left side) and long afterglow photo (right side)；
Fig. 9 is the composite optical material steady-state fluorescence spectrogram prepared in the embodiment of the present invention 3；
Figure 10 is the stable state spectrogram that the composite optical material prepared in the embodiment of the present invention 3 measures under phosphorescence pattern；
Figure 11 is that the composite optical material for preparing is remaining at 520nm under the excitation of 380nm wavelength in the embodiment of the present invention 3
Sunshine attenuation curve figure；
Figure 12 is the steady-state fluorescence spectrum of the composite optical material for preparing under different excitation wavelengths in the embodiment of the present invention 4
Figure；
Figure 13 is the stable state spectrogram that the composite optical material prepared in the embodiment of the present invention 4 measures under phosphorescence pattern；
Figure 14 is that the composite optical material for preparing is remaining at 520nm under the excitation of 380nm wavelength in the embodiment of the present invention 4
Sunshine attenuation curve；
Figure 15 is the fluorescence quantum yield comparison diagram of the composite optical material prepared in 1-4 of the embodiment of the present invention.
Specific implementation mode
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..Unless otherwise specified, embodiment
Used in the conventional means that are well known to those skilled in the art of technological means, raw materials used is commercial goods.
The condition being freeze-dried in following embodiment is：- 44 DEG C of 12~96h of freeze-drying.
The controllable carbon dots based compound nano material and preparation method thereof of 1 luminescent properties of embodiment
(1) surface modification has the preparation of the carbon quantum dot aqueous solution of carboxylic group
1, it weighs 0.5g folic acid and 1.0g citric acids is dissolved in the deionized water of 50ml, be sufficiently stirred 10 minutes, then
It will obtain mixed solution to be placed in polytetrafluoroethylene (PTFE) high pressure sealing reaction kettle, and be heated 4 hours at 250 DEG C, obtain initial soln；
2, initial soln obtained above is centrifuged 20 minutes at rotating speed 10000rpm, removes black precipitate, takes upper layer
Brown color clear liquid, using the bag filter that molecular cut off is 500Da, dialysis treatment 24 hours obtains pure fluorescence carbon quantum
Point aqueous solution；
3, by freeze-dried 96 hours of above-mentioned obtained carbon quantum dot aqueous solution, obtain surface contain a large amount of carboxyls and
The fluorescent carbon quantum dot powder of amino；
4, powder obtained above is dissolved in deionized water, is configured to the solution of 2mg/L, as surface modification has carboxyl
The carbon quantum dot aqueous solution of group.
(2) preparation of the controllable carbon dots based compound nano material of luminescent properties
Include the following steps：
(1) 8ml surface modifications are had to the carbon quantum dot aqueous solution and sodium hydroxide 0.62g and cyanuric acid powder of carboxylic group
Last 1g is uniformly mixed, and then magnetic agitation 10h obtains emulsion；
(2) emulsion obtained by (1) is centrifuged into 10min at rotating speed 10000rpm, abandons supernatant, obtain aqueous carbon dots base
Composite nano materials；
(3) (2) obtained aqueous carbon dots based compound nano material is freeze-dried controllable to get luminescent properties for 24 hours
Carbon dots based compound nano material.The weight percent that wherein carbon quantum dot accounts for dry composite material is 0.02%.
The property representation of the carbon dots based compound nano material prepared in the present embodiment is shown in Fig. 1~Fig. 4.
Fig. 1 is fluorescence photo and long afterglow photo of the composite optical material under the ultra violet lamp of 365nm wavelength；Fig. 1
Show that composite material in the ultra violet lamp exhibits blue fluorescence (left figure) of 365nm wavelength, there are naked eyes can after ultraviolet lamp extinguishing
The blue sunset glow (right figure) seen.
Fig. 2 is steady-state fluorescence spectrogram of the composite optical material under different excitation wavelengths；Figure it is seen that it is most
Good excitation wavelength is 380nm, maximum emission wavelength 435nm.
Fig. 3 is the stable state spectrogram that composite optical material measures under phosphorescence pattern；Fig. 3 shows composite material in 360nm
Wavelength excitation under, maximum emission wavelength in 435nm, and 380nm excitation under, maximum emission wavelength 525nm.
Fig. 4 be composite optical material 380nm wavelength excitation under, the sunset glow attenuation curve at 520nm；Fig. 4 shows compound
There are one longer sunset glow service life, average life span 289ms for material tool.
The controllable carbon dots based compound nano material and preparation method thereof of 2 luminescent properties of embodiment
(1) surface modification has the preparation of the carbon quantum dot aqueous solution of carboxylic group
1, it weighs 0.5g folic acid and 0.2g citric acids is dissolved in the deionized water of 50ml, be sufficiently stirred 10 minutes, then
It will obtain mixed solution to be placed in polytetrafluoroethylene (PTFE) high pressure sealing tank, be heated 4 hours at power 700w, 240 DEG C, be obtained initial
Solution；
2, initial soln obtained above is centrifuged 20 minutes at rotating speed 10000rpm, removes black precipitate, takes upper layer
Brown color clear liquid, using the bag filter that molecular cut off is 500Da, dialysis treatment 24 hours obtains pure fluorescence carbon quantum
Point aqueous solution；
3, by freeze-dried 96 hours of above-mentioned obtained carbon quantum dot aqueous solution, obtain surface contain a large amount of carboxyls and
The fluorescent carbon quantum dot powder of amino；
4, powder obtained above is dissolved in deionized water, is configured to the solution of 1mg/L, as surface modification has carboxyl
The carbon quantum dot aqueous solution of group.
(2) preparation of the controllable carbon dots based compound nano material of luminescent properties
Include the following steps：
(1) 8ml surface modifications there is the carbon quantum dot aqueous solution of carboxylic group to be uniformly mixed with cyanuric acid powder 1g, so
Magnetic agitation 10h obtains emulsion afterwards；
(2) emulsion obtained by (1) is centrifuged into 10min at rotating speed 10000rpm, abandons supernatant, obtain aqueous carbon dots base
Composite nano materials；
(3) (2) obtained aqueous carbon dots based compound nano material is freeze-dried controllable to get luminescent properties for 24 hours
Carbon dots based compound nano material.The weight percent that wherein carbon quantum dot accounts for dry composite material is 0.02%.
The property representation of the carbon dots based compound nano material prepared in the present embodiment is shown in Fig. 5~Fig. 7.
Composite material has naked eyes visible in the ultra violet lamp exhibits blue fluorescence of 365nm wavelength after ultraviolet lamp extinguishing
Blue sunset glow.
Fig. 5 is steady-state fluorescence spectrogram of the composite optical material under different excitation wavelengths；From fig. 5, it can be seen that it is most
Good excitation wavelength is 380nm, maximum emission wavelength 475nm.
Fig. 6 is the stable state spectrogram that composite optical material measures under phosphorescence pattern；Fig. 6 shows composite material in 340nm
Under wavelength excitation, maximum emission wavelength is in 475nm.
Fig. 7 be composite optical material 380nm wavelength excitation under, the sunset glow attenuation curve at 520nm；Fig. 7 shows compound
There are one longer sunset glow service life, average life span 120ms for material tool.
The controllable carbon dots based compound nano material and preparation method thereof of 3 luminescent properties of embodiment
(1) surface modification has the preparation of the carbon quantum dot aqueous solution of carboxylic group
1, it weighs 0.5g folic acid and 1.0g citric acids is dissolved in the deionized water of 50ml, be sufficiently stirred 10 minutes, then
It will obtain mixed solution to be placed in polytetrafluoroethylene (PTFE) high pressure sealing reaction kettle, and be heated 4 hours at 240 DEG C, obtain initial soln；
2, initial soln obtained above is centrifuged 20 minutes at rotating speed 10000rpm, removes black precipitate, takes upper layer
Brown color clear liquid, using the bag filter that molecular cut off is 500Da, dialysis treatment 24 hours obtains pure fluorescence carbon quantum
Point aqueous solution；
3, by freeze-dried 96 hours of above-mentioned obtained carbon quantum dot aqueous solution, obtain surface contain a large amount of carboxyls and
The fluorescent carbon quantum dot powder of amino；
4, powder obtained above is dissolved in deionized water, is configured to the solution of 2mg/L, as surface modification has carboxyl
The carbon quantum dot aqueous solution of group.
(2) preparation of the controllable carbon dots based compound nano material of luminescent properties
Include the following steps：
(1) 8ml surface modifications are had to the carbon quantum dot aqueous solution and sodium hydroxide 0.93g and cyanuric acid powder of carboxylic group
Last 1g is uniformly mixed, and then magnetic agitation 10h obtains emulsion；
(2) emulsion obtained by (1) is centrifuged into 10min at rotating speed 10000rpm, abandons supernatant, obtain aqueous carbon dots base
Composite nano materials；
(3) (2) obtained aqueous carbon dots based compound nano material is freeze-dried controllable to get luminescent properties for 24 hours
Carbon dots based compound nano material.The weight percent that wherein carbon quantum dot accounts for dry composite material is 0.02%.
The property representation of the carbon dots based compound nano material prepared in the present embodiment is shown in Fig. 8~Figure 11.
Fig. 8 is fluorescence photo and long afterglow photo of the composite optical material under the ultra violet lamp of 365nm wavelength；Fig. 8
Show that composite material in the ultra violet lamp exhibits blue fluorescence (left figure) of 365nm wavelength, there are naked eyes can after ultraviolet lamp extinguishing
The yellow green sunset glow (right figure) seen.
Fig. 9 is steady-state fluorescence spectrogram of the composite optical material under different excitation wavelengths；From fig. 9, it can be seen that it is most
Good excitation wavelength is 380nm, maximum emission wavelength 435nm.
Figure 10 is the stable state spectrogram that composite optical material measures under phosphorescence pattern；Figure 10 shows that composite material exists
Under the excitation of 360nm and 380nm wavelength, maximum emission wavelength is at 525nm.
Figure 11 be composite optical material 380nm wavelength excitation under, the sunset glow attenuation curve at 520nm；Figure 11 shows multiple
There are one longer sunset glow service life, average life span 380ms for condensation material tool.
The controllable carbon dots based compound nano material and preparation method thereof of 4 luminescent properties of embodiment
(1) surface modification has the preparation of the carbon quantum dot aqueous solution of carboxylic group
1, it weighs 0.5g folic acid and 0.5g citric acids is dissolved in the deionized water of 50ml, be sufficiently stirred 10 minutes, then
It will obtain mixed solution to be placed in polytetrafluoroethylene (PTFE) high pressure sealing reaction kettle, and be heated 3 hours at 300 DEG C, obtain initial soln；
2, initial soln obtained above is centrifuged 20 minutes at rotating speed 10000rpm, removes black precipitate, takes upper layer
Brown color clear liquid, using the bag filter that molecular cut off is 500Da, dialysis treatment 24 hours obtains pure fluorescence carbon quantum
Point aqueous solution；
3, by freeze-dried 96 hours of above-mentioned obtained carbon quantum dot aqueous solution, obtain surface contain a large amount of carboxyls and
The fluorescent carbon quantum dot powder of amino；
4, powder obtained above is dissolved in deionized water, is configured to the solution of 1mg/L, as surface modification has carboxyl
The carbon quantum dot aqueous solution of group.
(2) preparation of the controllable carbon dots based compound nano material of luminescent properties
Include the following steps：
(1) 8ml surface modifications are had to the carbon quantum dot aqueous solution and sodium hydroxide 2g and cyanuric acid powder of carboxylic group
1g is uniformly mixed, and then magnetic agitation 10h obtains emulsion；
(2) emulsion obtained by (1) is centrifuged into 10min at rotating speed 10000rpm, abandons supernatant, obtain aqueous carbon dots base
Composite nano materials；
(3) (2) obtained aqueous carbon dots based compound nano material is freeze-dried controllable to get luminescent properties for 24 hours
Carbon dots based compound nano material.The weight percent that wherein carbon quantum dot accounts for dry composite material is 0.02%.
The property representation of the carbon dots based compound nano material prepared in the present embodiment is shown in Fig. 5~Fig. 7.
Composite material has naked eyes visible in the ultra violet lamp exhibits blue fluorescence of 365nm wavelength after ultraviolet lamp extinguishing
Yellow green sunset glow.
Figure 12 is steady-state fluorescence spectrogram of the composite optical material under different excitation wavelengths；It can be recognized from fig. 12 that its
Optimum excitation wave a length of 380nm, maximum emission wavelength 435nm.
Figure 13 is the stable state spectrogram that composite optical material measures under phosphorescence pattern；Figure 13 shows that composite material exists
Under the excitation of 360nm and 380nm wavelength, maximum emission wavelength is at 525nm.
Figure 14 be composite optical material 380nm wavelength excitation under, the sunset glow attenuation curve at 520nm；Figure 14 shows multiple
There are one longer sunset glow service life, average life span 331ms for condensation material tool.
The fluorescence quantum yield comparison result of the composite optical material prepared in embodiment 1-4 is shown in Figure 15.
Although above the present invention is described in detail with a general description of the specific embodiments,
On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements, belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (10)
1. the preparation method of the controllable carbon dots based compound nano material of luminescent properties, which is characterized in that have carboxyl to surface modification
Cyanuric acid is added in the carbon quantum dot aqueous solution of group, or alkali metal hydroxide and cyanuric acid is added, gained mixing
Liquid is agitated, centrifuges, and collects precipitation, is freeze-dried up to the controllable carbon dots based compound nano material of luminescent properties.
2. according to the method described in claim 1, it is characterized in that, the surface modification has the carbon quantum dot of carboxylic group water-soluble
The preparation method of liquid is as follows：
(1) by folic acid and citric acid in mass ratio 1:0.1-10 dissolves in deionized water, and the mass ratio of folic acid and water is 1:50-
1000, obtain mixed liquor I；
(2) mixed liquor I obtained by (1) is placed in polytetrafluoroethylene (PTFE) high pressure sealing tank, heating or microwave are anti-at 150~300 DEG C
1~5h is answered, solution II is obtained；
(3) solution II for obtaining (2) centrifuges 5~30min at 3000~10000rpm, takes supernatant, uses molecular cut off
For bag filter 12~72h of dialysis treatment of 500-3500Da, fluorescent carbon quantum dot aqueous solution III is obtained；
(4) by the freeze-dried 12~96h of (3) acquired solution III, obtaining surface modification has the carbon quantum dot powder of carboxylic group
End；
(5) powder obtained by (4) is dissolved in deionized water, is configured to the solution of 0.01-10mg/L, as surface modification has carboxyl
The carbon quantum dot aqueous solution of group.
3. according to the method described in claim 2, it is characterized in that, having the carbon quantum dot water of carboxylic group to 8mL surface modifications
0.2-2g cyanuric acids and 0-8g alkali metal hydroxides, stirring 2~obtain emulsion for 24 hours are added in solution.
4. according to claim 1-3 any one of them methods, which is characterized in that the condition of centrifugation is：5000~10000rpm
Centrifuge 5~20min.
5. according to claim 1-3 any one of them methods, which is characterized in that the condition of freeze-drying is：In -44 DEG C of freezings
Dry 12~96h.
6. according to claim 1-3 any one of them methods, which is characterized in that the alkali metal hydroxide is sodium hydroxide
And/or potassium hydroxide.
7. according to the controllable carbon dots based compound nano material of luminescent properties prepared by any one of claim 1-6 the methods.
8. carbon dots based compound nano material according to claim 7, which is characterized in that carbon quantum dot accounts for the composite Nano
The weight percent of material is 0.01%~0.5%.
9. the carbon dots based compound nano material of claim 7 or 8 is preparing anti-fake material, biological sensing material, display equipment
Application in material and illuminating material.
10. the anti-fake material, biological sensing material, the display that are prepared by the carbon dots based compound nano material of claim 7 or 8
Material and illuminating material.
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| CN111334285B (en) * | 2020-04-08 | 2022-08-09 | 中国科学院长春光学精密机械与物理研究所 | Carbon nanodot composite material with cyanuric acid doped in carbon nanodots, preparation method and application |
| CN112745838A (en) * | 2021-02-01 | 2021-05-04 | 郑州大学 | Large-scale solid green fluorescent carbon nanodots and preparation method thereof |
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