CN106497560A - Controllable carbon point based compound nano material of luminescent properties and preparation method and application - Google Patents
Controllable carbon point based compound nano material of luminescent properties and preparation method and application Download PDFInfo
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Abstract
The present invention provides controllable carbon point based compound nano material of a kind of luminescent properties and preparation method and application.By adding cyanuric acid in carbon quantum dot aqueous solution from carboxylic group to surface modification that have, or add alkali metal hydroxide and cyanuric acid, gained mixed liquor is agitated, centrifugation, collects precipitation, and lyophilization obtains final product the controllable carbon point based compound nano material of luminescent properties.The preparation process is simple of the present invention, low cost, asepsis environment-protecting.By adjusting pH value, the fluorescence radiation efficiency of material can not only be greatly improved, and can change color and the life-span of material sunset glow, in false proof, bio-sensing and show, with fields such as illuminations, there is important using value.
Description
Technical field
The present invention relates to material engineering field, specifically, is related to a kind of controllable carbon point base composite nano of luminescent properties
Material and preparation method and application.
Background technology
Carbon quantum dot be discovered in recent years the particle diameter being made up of scattered near-spherical granule below 10nm with send out
The carbon granule of light property.Since self-discovery, due to the performance of itself uniqueness, the great interest of vast researcher 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,
Have broad application prospects in opto-electronic device, biological detection, medicine and other fields.That wherein of greatest concern is its photic
Light characteristic.But due to being affected by carbon point intrinsic property, its luminescent properties is the carbon point based compound nano material that they prepare
Uncontrollable.Therefore, the controllable carbon point based compound nano material of luminescent properties is realized by simple method, life can be substantially reduced
Produce cost.
Content of the invention
The present invention is directed to optical material complicated process of preparation in prior art, preparing raw material is rare and optical property can not
A kind of the problems such as control, there is provided controllable carbon point based compound nano material of luminescent properties and preparation method thereof.
It is a further object of the present invention to provide the application of the controllable carbon point 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 point based compound nano material of luminescent properties
Method, methods described are addition cyanuric acids in the carbon quantum dot aqueous solution for having carboxylic group to surface modification, or add alkali gold
Category hydroxide and cyanuric acid, gained mixed liquor is agitated, centrifugation, collects precipitation, and it is controllable that lyophilization obtains final product luminescent properties
Carbon point based compound nano material.
The surface modification 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) (1) gained mixed liquor is placed in politef high pressure sealing tank, heating or microwave at 150~300 DEG C
1~5h of reaction, obtains solution II;
(3) solution II for obtaining (2) is centrifuged 5~30min under 3000~10000rpm, takes supernatant, with retention point
Son amount is the bag filter 12~72h of dialysis treatment of 500-3500Da, obtains fluorescent carbon quantum dot aqueous solution III;
(4) by freeze-dried for (3) resulting solution III 12~96h, obtaining surface modification has the carbon quantum dot of carboxylic group
Powder;Cryodesiccated temperature is -44 DEG C;
(5) (4) gained powder 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.
In the present invention, alkali metal hydroxide used is sodium hydroxide and/or potassium hydroxide.
Aforesaid method, 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, 2~24h of stirring obtain emulsion.Wherein, cyanuric acid and alkali metal hydroxide rub
You are than being 1:0.01-6.
Aforesaid method, centrifugal condition is:5000~10000rpm is centrifuged 5~20min.
Aforesaid method, cryodesiccated condition is:- 44 DEG C of 12~96h of lyophilization.
The present invention also provides the carbon point based compound nano material controllable according to the luminescent properties of said method preparation.Wherein,
It is 0.01%~0.5% that carbon quantum dot accounts for the percentage by weight of the composite nano materials.
The present invention also provides the carbon point based compound nano material and is preparing anti-fake material, biological sensing material, display
Application in material and illuminating material.
The present invention further provides by the carbon point based compound nano material prepare anti-fake material, biological sensing material,
Display material and illuminating material.
The present invention has advantages below:
(1) present invention is adjusted by alkali metal hydroxide (such as sodium hydroxide) with carbon quantum dot and cyanuric acid as raw material
The pH value of section mixed solution, prepares the controllable carbon point based compound nano material of luminescent properties.When cyanuric acid and sodium hydroxide
Mol ratio < 3:When 1, composite sends blue-fluorescence and blue sunset glow under the ultra violet lamp of 365nm wavelength;Work as hydrogen-oxygen
Change mol ratio >=3 of sodium and cyanuric acid:When 1, composite send under the ultra violet lamp of 365nm wavelength blue-fluorescence and
Yellow sunset glow, and gradually increase with the increase fluorescence quantum yield of sodium hydroxide concentration.
(2) preparation method of the invention is simple, whole technological process environmental protection, need to only adjust the addition of sodium hydroxide
By adjusting the pH value of solution, amount, can prepare that fluorescence, Phosphor efficiency be different, colorful, different life-spans luminescent materials.
(3) the controllable carbon point based compound nano material good stability of the luminescent properties of present invention preparation, life-span length, sunset glow
Die-away time, up to the several seconds, has important using value in fields such as information anti-fake, biomarkers.
Description of the drawings
Fig. 1 is fluorescence of the composite optical material prepared in the embodiment of the present invention 1 under the ultra violet lamp of 365nm wavelength
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 is determined under phosphorescence pattern;
Fig. 4 is sunset glow of the composite optical material prepared in the embodiment of the present invention 1 in the case where 380nm wavelength is excited, at 520nm
Attenuation curve figure;
Fig. 5 is steady-state fluorescence spectrum of the composite optical material prepared in the embodiment of the present invention 2 under different excitation wavelengths
Figure;
Fig. 6 is the stable state spectrogram that the composite optical material prepared in the embodiment of the present invention 2 is determined under phosphorescence pattern;
Fig. 7 is sunset glow of the composite optical material prepared in the embodiment of the present invention 2 in the case where 380nm wavelength is excited, at 520nm
Attenuation curve;
Fig. 8 is fluorescence of the composite optical material prepared in the embodiment of the present invention 3 under the ultra violet lamp of 365nm wavelength
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 is determined under phosphorescence pattern;
Figure 11 be the embodiment of the present invention 3 in prepare composite optical material in the case where 380nm wavelength is excited, remaining at 520nm
Sunshine attenuation curve figure;
Figure 12 is steady-state fluorescence spectrum of the composite optical material prepared in the embodiment of the present invention 4 under different excitation wavelengths
Figure;
Figure 13 is the stable state spectrogram that the composite optical material prepared in the embodiment of the present invention 4 is determined under phosphorescence pattern;
Figure 14 be the embodiment of the present invention 4 in prepare composite optical material in the case where 380nm wavelength is excited, remaining at 520nm
Sunshine attenuation curve;
Figure 15 is the fluorescence quantum yield comparison diagram of the composite optical material prepared in embodiment of the present invention 1-4.
Specific embodiment
Following examples are used for the present invention to be described, but are not limited to the scope of the present invention.If not specializing, embodiment
In the conventional meanses that are well known to those skilled in the art of technological means used, raw materials used be commercial goods.
In following examples, cryodesiccated condition is:- 44 DEG C of 12~96h of lyophilization.
Controllable carbon point based compound nano material of 1 luminescent properties of embodiment and preparation method thereof
(1) surface modification has the preparation of the carbon quantum dot aqueous solution of carboxylic group
1st, weigh 0.5g Folic Acid and 1.0g citric acids are dissolved in the deionized water of 50ml, be sufficiently stirred for 10 minutes, then
Mixed solution will be obtained to be placed in politef high pressure sealing reactor, heated 4 hours at 250 DEG C, obtained initial soln;
2nd, initial soln obtained above is centrifuged 20 minutes under rotating speed 10000rpm, removes black precipitate, take upper strata
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;
3rd, will be freeze-dried 96 hours for 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;
4th, 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 point based compound nano material of luminescent properties
Comprise the following steps:
(1) 8ml surface modifications are had the carbon quantum dot aqueous solution and sodium hydroxide 0.62g and cyanuric acid powder of carboxylic group
Last 1g mix homogeneously, then magnetic agitation 10h obtain emulsion;
(2) emulsion of (1) gained is centrifuged 10min under rotating speed 10000rpm, abandons supernatant, obtain aqueous carbon point base
Composite nano materials;
(3) by freeze-dried for hydrocarbon point based compound nano material obtained by (2) 24h, luminescent properties are obtained final product controllable
Carbon point based compound nano material.The percentage by weight that wherein carbon quantum dot accounts for dry composite material is 0.02%.
The property representation of the carbon point based compound nano material prepared in the present embodiment is shown in Fig. 1~Fig. 4.
Fig. 1 is fluorescence photo of the composite optical material under the ultra violet lamp of 365nm wavelength and long afterglow photo;Fig. 1
Show ultra violet lamp exhibits blue fluorescence (left figure) of the composite in 365nm wavelength, having after uviol lamp extinguishes visually can
The blue sunset glow (right figure) that sees.
Fig. 2 is steady-state fluorescence spectrogram of the composite optical material under different excitation wavelengths;Figure it is seen which is most
Good excitation wavelength is 380nm, and maximum emission wavelength is 435nm.
Fig. 3 is the stable state spectrogram that composite optical material is determined under phosphorescence pattern;Fig. 3 shows composite in 360nm
Wavelength is excited down, and maximum emission wavelength is in 435nm, and in the case where 380nm is excited, maximum emission wavelength is 525nm.
Fig. 4 is sunset glow attenuation curve of the composite optical material in the case where 380nm wavelength is excited, at 520nm;Fig. 4 shows to be combined
Material has a longer sunset glow life-span, and its average life is 289ms.
Controllable carbon point based compound nano material of 2 luminescent properties of embodiment and preparation method thereof
(1) surface modification has the preparation of the carbon quantum dot aqueous solution of carboxylic group
1st, weigh 0.5g Folic Acid and 0.2g citric acids are dissolved in the deionized water of 50ml, be sufficiently stirred for 10 minutes, then
Mixed solution will be obtained to be placed in politef high pressure sealing tank, in power 700w, heated 4 hours at 240 DEG C, be obtained initial
Solution;
2nd, initial soln obtained above is centrifuged 20 minutes under rotating speed 10000rpm, removes black precipitate, take upper strata
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;
3rd, will be freeze-dried 96 hours for 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;
4th, 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 point based compound nano material of luminescent properties
Comprise the following steps:
(1) the carbon quantum dot aqueous solution that 8ml surface modifications are had carboxylic group is mixed homogeneously with cyanuric acid powder 1g, so
Magnetic agitation 10h obtains emulsion afterwards;
(2) emulsion of (1) gained is centrifuged 10min under rotating speed 10000rpm, abandons supernatant, obtain aqueous carbon point base
Composite nano materials;
(3) by freeze-dried for hydrocarbon point based compound nano material obtained by (2) 24h, luminescent properties are obtained final product controllable
Carbon point based compound nano material.The percentage by weight that wherein carbon quantum dot accounts for dry composite material is 0.02%.
The property representation of the carbon point based compound nano material prepared in the present embodiment is shown in Fig. 5~Fig. 7.
Ultra violet lamp exhibits blue fluorescence of the composite in 365nm wavelength, has naked eyes visible after uviol lamp extinguishes
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 which is most
Good excitation wavelength is 380nm, and maximum emission wavelength is 475nm.
Fig. 6 is the stable state spectrogram that composite optical material is determined under phosphorescence pattern;Fig. 6 shows composite in 340nm
Wavelength is excited down, and maximum emission wavelength is in 475nm.
Fig. 7 is sunset glow attenuation curve of the composite optical material in the case where 380nm wavelength is excited, at 520nm;Fig. 7 shows to be combined
Material has a longer sunset glow life-span, and its average life is 120ms.
Controllable carbon point based compound nano material of 3 luminescent properties of embodiment and preparation method thereof
(1) surface modification has the preparation of the carbon quantum dot aqueous solution of carboxylic group
1st, weigh 0.5g Folic Acid and 1.0g citric acids are dissolved in the deionized water of 50ml, be sufficiently stirred for 10 minutes, then
Mixed solution will be obtained to be placed in politef high pressure sealing reactor, heated 4 hours at 240 DEG C, obtained initial soln;
2nd, initial soln obtained above is centrifuged 20 minutes under rotating speed 10000rpm, removes black precipitate, take upper strata
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;
3rd, will be freeze-dried 96 hours for 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;
4th, 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 point based compound nano material of luminescent properties
Comprise the following steps:
(1) 8ml surface modifications are had the carbon quantum dot aqueous solution and sodium hydroxide 0.93g and cyanuric acid powder of carboxylic group
Last 1g mix homogeneously, then magnetic agitation 10h obtain emulsion;
(2) emulsion of (1) gained is centrifuged 10min under rotating speed 10000rpm, abandons supernatant, obtain aqueous carbon point base
Composite nano materials;
(3) by freeze-dried for hydrocarbon point based compound nano material obtained by (2) 24h, luminescent properties are obtained final product controllable
Carbon point based compound nano material.The percentage by weight that wherein carbon quantum dot accounts for dry composite material is 0.02%.
The property representation of the carbon point based compound nano material prepared in the present embodiment is shown in Fig. 8~Figure 11.
Fig. 8 is fluorescence photo of the composite optical material under the ultra violet lamp of 365nm wavelength and long afterglow photo;Fig. 8
Show ultra violet lamp exhibits blue fluorescence (left figure) of the composite in 365nm wavelength, having after uviol lamp extinguishes visually can
The yellow green sunset glow (right figure) that sees.
Fig. 9 is steady-state fluorescence spectrogram of the composite optical material under different excitation wavelengths;From fig. 9, it can be seen which is most
Good excitation wavelength is 380nm, and maximum emission wavelength is 435nm.
Figure 10 is the stable state spectrogram that composite optical material is determined under phosphorescence pattern;Figure 10 shows that composite exists
360nm and 380nm wavelength is excited down, and maximum emission wavelength is at 525nm.
Figure 11 is sunset glow attenuation curve of the composite optical material in the case where 380nm wavelength is excited, at 520nm;Figure 11 shows multiple
Condensation material has a longer sunset glow life-span, and its average life is 380ms.
Controllable carbon point based compound nano material of 4 luminescent properties of embodiment and preparation method thereof
(1) surface modification has the preparation of the carbon quantum dot aqueous solution of carboxylic group
1st, weigh 0.5g Folic Acid and 0.5g citric acids are dissolved in the deionized water of 50ml, be sufficiently stirred for 10 minutes, then
Mixed solution will be obtained to be placed in politef high pressure sealing reactor, heated 3 hours at 300 DEG C, obtained initial soln;
2nd, initial soln obtained above is centrifuged 20 minutes under rotating speed 10000rpm, removes black precipitate, take upper strata
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;
3rd, will be freeze-dried 96 hours for 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;
4th, 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 point based compound nano material of luminescent properties
Comprise the following steps:
(1) 8ml surface modifications are had the carbon quantum dot aqueous solution and sodium hydroxide 2g and cyanuric acid powder of carboxylic group
1g mix homogeneously, then magnetic agitation 10h obtain emulsion;
(2) emulsion of (1) gained is centrifuged 10min under rotating speed 10000rpm, abandons supernatant, obtain aqueous carbon point base
Composite nano materials;
(3) by freeze-dried for hydrocarbon point based compound nano material obtained by (2) 24h, luminescent properties are obtained final product controllable
Carbon point based compound nano material.The percentage by weight that wherein carbon quantum dot accounts for dry composite material is 0.02%.
The property representation of the carbon point based compound nano material prepared in the present embodiment is shown in Fig. 5~Fig. 7.
Ultra violet lamp exhibits blue fluorescence of the composite in 365nm wavelength, has naked eyes visible after uviol lamp extinguishes
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
The a length of 380nm of optimum excitation wave, maximum emission wavelength is 435nm.
Figure 13 is the stable state spectrogram that composite optical material is determined under phosphorescence pattern;Figure 13 shows that composite exists
360nm and 380nm wavelength is excited down, and maximum emission wavelength is at 525nm.
Figure 14 is sunset glow attenuation curve of the composite optical material in the case where 380nm wavelength is excited, at 520nm;Figure 14 shows multiple
Condensation material has a longer sunset glow life-span, and its average life is 331ms.
The fluorescence quantum yield comparative 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 point based compound nano material of luminescent properties, it is characterised in that have carboxyl to surface modification
Cyanuric acid being added in the carbon quantum dot aqueous solution of group, or adding alkali metal hydroxide and cyanuric acid, gained mixes
Liquid is agitated, centrifugation, collects precipitation, and lyophilization obtains final product the controllable carbon point based compound nano material of luminescent properties.
2. method according to claim 1, it is characterised 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) (1) gained mixed liquor is placed in politef high pressure sealing tank, heating or microwave reaction at 150~300 DEG C
1~5h, obtains solution II;
(3) solution II for obtaining (2) is centrifuged 5~30min under 3000~10000rpm, takes supernatant, uses molecular cut off
For the bag filter 12~72h of dialysis treatment of 500-3500Da, fluorescent carbon quantum dot aqueous solution III is obtained;
(4) by freeze-dried for (3) resulting solution III 12~96h, obtaining surface modification has the carbon quantum dot powder of carboxylic group
End;
(5) (4) gained powder 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. method according to claim 2, it is characterised in that to the carbon quantum dot water that 8mL surface modifications have carboxylic group
0.2-2g cyanuric acids and 0-8g alkali metal hydroxides, 2~24h of stirring is added to obtain emulsion in solution.
4. the method according to any one of claim 1-3, it is characterised in that the condition of centrifugation is:5000~10000rpm
5~20min of centrifugation.
5. the method according to any one of claim 1-4, it is characterised in that cryodesiccated condition is:Freeze in -44 DEG C
Dry 12~96h.
6. the method according to any one of claim 1-5, it is characterised in that the alkali metal hydroxide is sodium hydroxide
And/or potassium hydroxide.
7. according to the carbon point based compound nano material that the luminescent properties of any one of claim 1-6 methods described preparation are controllable.
8. carbon point based compound nano material according to claim 7, it is characterised in that carbon quantum dot accounts for the composite Nano
The percentage by weight of material is 0.01%~0.5%.
9. carbon point based compound nano material described in claim 7 or 8 is preparing anti-fake material, biological sensing material, is showing equipment
Application in material and illuminating material.
10. described in claim 7 or 8 carbon point based compound nano material prepare anti-fake material, biological sensing material, display
Material and illuminating material.
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CN111154486A (en) * | 2020-01-19 | 2020-05-15 | 江苏大学 | Orange fluorescent and red room-temperature afterglow carbon dot material and preparation method and application thereof |
CN111334285A (en) * | 2020-04-08 | 2020-06-26 | 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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CN108130078B (en) * | 2018-01-15 | 2020-07-10 | 清华大学 | Long-life underwater organic room-temperature phosphorescent material and preparation method and application thereof |
CN111154486A (en) * | 2020-01-19 | 2020-05-15 | 江苏大学 | Orange fluorescent and red room-temperature afterglow carbon dot material and preparation method and application thereof |
CN111154486B (en) * | 2020-01-19 | 2022-09-16 | 江苏大学 | Orange fluorescent and red room-temperature afterglow carbon dot material and preparation method and application thereof |
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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 |
CN113025325A (en) * | 2021-03-25 | 2021-06-25 | 盐城工学院 | Preparation method and application of room-temperature phosphorescent carbon-based composite material capable of changing color under single excitation source |
CN113025325B (en) * | 2021-03-25 | 2022-11-01 | 盐城工学院 | Preparation method and application of room temperature phosphorescent carbon-based composite material capable of changing color under single excitation source |
CN113376129A (en) * | 2021-03-26 | 2021-09-10 | 中科院苏州医工所郑州工程技术研究院 | Preparation method and application of carbon dot-based nano composite for detecting iron ions |
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