CN106829920A - A kind of green fluorescence carbon quantum dot material and preparation method thereof - Google Patents
A kind of green fluorescence carbon quantum dot material and preparation method thereof Download PDFInfo
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000463 material Substances 0.000 title claims abstract description 11
- 239000006228 supernatant Substances 0.000 claims abstract description 17
- 238000000703 high-speed centrifugation Methods 0.000 claims abstract description 8
- 239000012153 distilled water Substances 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims abstract description 5
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229940068041 phytic acid Drugs 0.000 claims abstract description 5
- 235000002949 phytic acid Nutrition 0.000 claims abstract description 5
- 239000000467 phytic acid Substances 0.000 claims abstract description 5
- 238000001556 precipitation Methods 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000003763 carbonization Methods 0.000 claims abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 229910052799 carbon Inorganic materials 0.000 claims description 12
- 239000002096 quantum dot Substances 0.000 claims description 3
- 239000003480 eluent Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000008014 freezing Effects 0.000 claims 1
- 238000007710 freezing Methods 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 238000001514 detection method Methods 0.000 abstract description 6
- 238000004108 freeze drying Methods 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 238000006555 catalytic reaction Methods 0.000 abstract 1
- 238000011017 operating method Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 11
- 238000006862 quantum yield reaction Methods 0.000 description 5
- 239000012530 fluid Substances 0.000 description 4
- 238000010791 quenching Methods 0.000 description 4
- 230000000171 quenching effect Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002171 ethylene diamines Chemical class 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002795 fluorescence method Methods 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000004054 semiconductor nanocrystal Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N2021/6432—Quenching
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Abstract
The invention discloses a kind of green fluorescence carbon quantum dot material and preparation method thereof.Preparation method of the invention is comprised the following steps that：1) it is (1.8~2) according to volume ratio：(18~20)：1, phytic acid, distilled water and ethylenediamine are stirred 10~15 minutes under conditions of room temperature, solution is changed into turbid solution from clarifying, then high speed centrifugation removal insoluble substance, takes supernatant；2) it is carbonized in the supernatant of taking-up being added into autoclave；3) carbonization solution is taken out, high speed centrifugation, removal insoluble matter precipitation takes supernatant, carries out gel column purifying, freeze-drying and obtain green fluorescence carbon quantum dot.The inventive method operating procedure is simple, and with low cost, the fluorescent yield of the carbon quantum dot of preparation is high, can be directly used for metal Hg2+The detection of ion, can also be widely used in the fields such as biological detection, biological mirror image, photoelectric conversion and catalysis.
Description
Technical field
The present invention relates to a kind of green fluorescence carbon quantum dot material and preparation method thereof, belong to nano material preparation technology neck
Domain.
Background technology
Carbon quantum dot, is a kind of novel fluorescence carbon nanomaterial for occurring in recent years, and it is a kind of approximate ball-type and diameter
Zero-dimensional semiconductor nanocrystal less than 10nm and with good dispersiveness.This nano material overcomes traditional II-IV
Some shortcomings of race's quantum dot, with nontoxic, high-fluorescence quantum yield, good biocompatibility and light high, chemically stable
Property etc., can be used for the numerous areas such as bio-sensing, bio-imaging, environment measuring, photocatalysis and pharmaceutical carrier.The carbon point of low toxicity
Have begun to the larger II-IV races quantum dot of replacement bio-toxicity and be applied to life science.
The preparation method of carbon quantum dot has many kinds, is originated according to carbon source, can be divided into inorganic carbon source and organic carbon source.Generally
The fluorescence quantum yield of the carbon quantum dot prepared through inorganic carbon source is low, and complex operation.But prepare carbon quantum with organic carbon source
Point luminous efficiency is more preferably.The means such as chemical oxidation, microwave treatment, hydro-thermal method are typically with it is hereby achieved that thin small and scattered
Carbon quantum dot, but because the carbon quantum dot obtained by such method is generally blue emitting phosphor, so being unfavorable in biology
Internal application.
The content of the invention
It is to provide a kind of nontoxic, uniform particle sizes, the green of longer emission wavelength (near 520nm) that the purpose of the present invention is
Carbon quantum dot material of fluorescence and preparation method thereof.Preparation method of the present invention is simple, and the carbon quantum dot of the green fluorescence for obtaining can
Directly apply to metal Hg2+The detection of ion.
Technical scheme is specifically described as follows.
The present invention provides a kind of green fluorescence carbon quantum dot material, in the case where the wavelength of 360~440nm is excited, green fluorescence
The launch wavelength of carbon quantum dot is between 510~525nm.
The present invention also provides a kind of preparation method of above-mentioned green fluorescence carbon quantum dot material, comprises the following steps that：
1) it is (1.8~2) according to volume ratio：(18~20)：1, by phytic acid, distilled water and ethylenediamine under conditions of room temperature
Stirring 10~15 minutes, solution is changed into turbid solution from clarifying, then high speed centrifugation removal insoluble substance, takes supernatant；
2) it is carbonized in the supernatant of taking-up being added into autoclave, temperature setting is 175~185 DEG C, stirring speed
It is 360~400 revs/min to spend, and the reaction time is 7~9 hours；
3) carbonization solution is taken out, high speed centrifugation, removal insoluble matter precipitation takes supernatant, carries out gel column purifying, eluent
Freeze-drying obtains green fluorescence carbon quantum dot material.
Preferably, step 2) in, temperature setting is 180~185 DEG C.
Compared to the prior art, it is an advantage of the invention that：
(1) preparation method of the present invention is simple, easy to operate, and reappearance is high.The prices of raw materials are cheap and can obtain pure carbon
Quantum dot powder.
(2) the carbon quantum dot transmitting green fluorescence (center emission wavelength is near 520nm) prepared by, fluorescent emission bands
Higher than the launch wavelength of traditional major part blue light carbon quantum dot, can be directly used for Hg2+Detection, also is adapted for biologic applications field.
(3) fluorescent yield of the carbon quantum dot that the present invention is provided is up to 72%, can be used for biological detection, mirror image, Yi Jiyou
The application of the high-photoelectric transformation efficiency in machine semiconductor.
Brief description of the drawings
Under the conditions of Fig. 1 is embodiment 1, transmission electron microscope picture (a) of the invention and size distribution plot (b).
Fig. 2 is under the conditions of embodiment 1, the present invention excites lower acquisition fluorescent emission collection of illustrative plates in 300~480nm wavelength.
Fig. 3 be embodiment 1 under the conditions of, the UV absorption and fluorescent emission spectrogram of the water-soluble fluid samples of carbon quantum dot.Illustration
(left side) is the water-soluble fluid samples photo of carbon quantum dot, in colourless；Illustration (right side) is the carbon quantum dot under 365nm length ultraviolet light irradiations
Fluorescence photo, in green.
Fig. 4 be embodiment 1 under the conditions of, Hg2+To carbon quantum dot aqueous solution fluorescent quenching collection of illustrative plates.Wherein figure (a) is carbon quantum
Point is to Hg2+Quenching fluorescence pattern, figure (b) be carbon quantum dot to metalloform-selective collection of illustrative plates, figure (c) be carbon quantum dot pair
Hg2+Sensitivity collection of illustrative plates.
Specific embodiment
Technical scheme is further described with reference to example.
Embodiment 1
1) distilled water of 20mL is added in the beaker of 100mL at ambient temperature, the phytic acid of 2mL is subsequently adding, in magnetic
Under power stirring, 1mL ethylenediamines are slowly added to, reacted 10 minutes.Solution turned cloudy, generates insoluble salt during this period.Reaction
It is centrifuged after end, removal precipitation takes supernatant.
2) supernatant of taking-up is added in autoclave, and adds medium size rotor.Reaction temperature is set to 180
DEG C, 8 hours time, 400 revs/min of rotating speed after reaction terminates, takes out 8000 revs/min of solution high speed centrifugation, and removal is precipitated,
Take supernatant.
3) above-mentioned supernatant is poured into gel column (G-50), the gel for being added is 1/2nd of column length.Gel makes
With preceding, need to steep 24 hours in distilled water, the purpose is to remove the impurity in gel, abundant foam washing.
4) solution after filtering is collected, is rotated, improve the concentration of carbon quantum dot solution.Last freeze-drying 48 is small
When obtain solid powder.Under the conditions of Fig. 1 is embodiment 1, transmission electron microscope picture (a) of the invention and size distribution plot (b), carbon quantum
The particle diameter distribution of point is 2.5-7.5nm, and uniform-dimension is 4.2nm.
The fluorescent yield of the carbon quantum dot that embodiment 1 is provided that is, under identical shooting condition, is divided using method measure is haggled over
Not Ce Ding carbon quantum dot and fluorescence reference standard thing fluorescence area, substitute into formula below：
In formula, Φsample、ΦrefThe respectively fluorescence quantum yield of testing sample and fluorescence reference standard thing, Fsample、
FrefRespectively the fluorescent emission peak area or fluorescence intensity of testing sample and fluorescence reference standard thing, Asample、ArefRespectively treat
The absorbance that test sample product and fluorescence reference standard thing have at excitation wavelength, nsample、nrefRespectively testing sample and
The refractive index of solvent where fluorescence reference standard thing.
Using rhodamine B as fluorescence reference standard thing, the fluorescence quantum yield of the carbon quantum dot that embodiment 1 is provided after measured
It is 0.72.
Fig. 2 is under the conditions of embodiment 1, the present invention excites lower acquisition fluorescent emission collection of illustrative plates in 300~480nm wavelength.As a result
Represent, in the case where the wavelength of 360~440nm is excited, the launch wavelength of green fluorescence carbon quantum dot is between 510~525nm.
Fig. 3 be embodiment 1 under the conditions of, the UV absorption and fluorescent emission spectrogram of the water-soluble fluid samples of carbon quantum dot.Illustration
(left side) is the water-soluble fluid samples photo of carbon quantum dot, in colourless；Illustration (right side) is the carbon quantum dot under 365nm length ultraviolet light irradiations
Fluorescence photo, in green.
Fig. 4 be embodiment 1 under the conditions of, Hg2+To carbon quantum dot aqueous solution fluorescent quenching collection of illustrative plates.Wherein figure (a) is carbon quantum
Point is to Hg2+Quenching fluorescence pattern, figure (b) be carbon quantum dot to metalloform-selective collection of illustrative plates, figure (c) be carbon quantum dot pair
Hg2+Sensitivity collection of illustrative plates.Result shows that carbon quantum dot of the invention can be realized to Hg2+Selectivity and high-sensitivity detection.
Embodiment 2
1) distilled water of 18mL is added in the beaker of 100mL at ambient temperature, the phytic acid of 1.8mL is subsequently adding,
Under magnetic agitation, 1mL ethylenediamines are slowly added to, reacted 15 minutes.Solution turned cloudy, generates insoluble salt during this period.Instead
It is centrifuged after should terminating, removal precipitation takes supernatant.
2) supernatant of taking-up is added in autoclave, and adds medium size rotor.Reaction temperature is set to 185
DEG C, 8 hours time, 3600 revs/min of rotating speed after reaction terminates, takes out 8000 revs/min of solution high speed centrifugation, and removal is precipitated,
Take supernatant.
3) above-mentioned supernatant is poured into gel column (G-50), the gel for being added is 1/2nd of column length.Gel makes
With preceding, need to steep 24 hours in distilled water, the purpose is to remove the impurity in gel, abundant foam washing.
4) solution after filtering is collected, is rotated, improve the concentration of carbon quantum dot solution.Last freeze-drying 48 is small
When obtain solid powder.
The particle diameter 2.5-7.5nm of the carbon quantum dot that embodiment 2 is obtained.In the case where the wavelength of 360~440nm is excited, green is glimmering
The launch wavelength of light carbon quantum dot is between 510~525nm.The fluorescence of the carbon quantum dot under 365nm length ultraviolet light irradiations shines
Piece, in green.The fluorescence quantum yield of carbon quantum dot is 72%.
Claims (3)
1. a kind of green fluorescence carbon quantum dot material, it is characterised in that in the case where the wavelength of 360~440nm is excited, green fluorescence carbon
The launch wavelength of quantum dot is between 510~525nm.
2. the preparation method of green fluorescence carbon quantum dot material as claimed in claim 1, it is characterised in that specific steps are such as
Under：
1) it is (1.8~2) according to volume ratio：(18~20)：1, phytic acid, distilled water and ethylenediamine are stirred under conditions of room temperature
10~15 minutes, solution was changed into turbid solution from clarifying, then high speed centrifugation removal insoluble substance, took supernatant；
2) it is carbonized in the supernatant of taking-up being added into autoclave, temperature setting is 175~185 DEG C, mixing speed is
360~400 revs/min, the reaction time is 7~9 hours；
3) carbonization solution is taken out, high speed centrifugation, removal insoluble matter precipitation takes supernatant, carries out gel column purifying, eluent freezing
It is dried to obtain green fluorescence carbon quantum dot material.
3. preparation method as claimed in claim 2, it is characterised in that step 2) in, temperature setting is 180-185 DEG C.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108559496A (en) * | 2018-03-16 | 2018-09-21 | 南京工业大学 | A method of preparing green fluorescence carbon quantum dot |
| CN109880614A (en) * | 2019-03-16 | 2019-06-14 | 复旦大学 | Carbon dots-starch composite phosphor and preparation method thereof for fingerprint detection of diving |
| CN109880620A (en) * | 2019-03-02 | 2019-06-14 | 福建医科大学 | It is a kind of using biomass as the preparation and application of the green fluorescence carbon quantum dot of presoma |
| CN110018146A (en) * | 2019-04-28 | 2019-07-16 | 上海应用技术大学 | A method of palladium ion is detected based on fluorescent carbon quantum dot |
| CN110437839A (en) * | 2019-08-27 | 2019-11-12 | 杨国俊 | A kind of graphene quantum dot soil-solidified-agent preparation method |
| CN115231551A (en) * | 2022-09-05 | 2022-10-25 | 云南师范大学 | Method for preparing carbon quantum dots by using dimethyl phthalate |
| CN116855246A (en) * | 2023-07-03 | 2023-10-10 | 广西科学院 | Phosphorus self-doping type biomass carbon quantum dot corrosion inhibitor and preparation method and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108559496A (en) * | 2018-03-16 | 2018-09-21 | 南京工业大学 | A method of preparing green fluorescence carbon quantum dot |
| CN109880620A (en) * | 2019-03-02 | 2019-06-14 | 福建医科大学 | It is a kind of using biomass as the preparation and application of the green fluorescence carbon quantum dot of presoma |
| CN109880614A (en) * | 2019-03-16 | 2019-06-14 | 复旦大学 | Carbon dots-starch composite phosphor and preparation method thereof for fingerprint detection of diving |
| CN110018146A (en) * | 2019-04-28 | 2019-07-16 | 上海应用技术大学 | A method of palladium ion is detected based on fluorescent carbon quantum dot |
| CN110018146B (en) * | 2019-04-28 | 2021-08-13 | 上海应用技术大学 | Method for detecting palladium ions based on fluorescent carbon quantum dots |
| CN110437839A (en) * | 2019-08-27 | 2019-11-12 | 杨国俊 | A kind of graphene quantum dot soil-solidified-agent preparation method |
| CN115231551A (en) * | 2022-09-05 | 2022-10-25 | 云南师范大学 | Method for preparing carbon quantum dots by using dimethyl phthalate |
| CN115231551B (en) * | 2022-09-05 | 2023-09-01 | 云南师范大学 | Method for preparing carbon quantum dots by using dimethyl phthalate |
| CN116855246A (en) * | 2023-07-03 | 2023-10-10 | 广西科学院 | Phosphorus self-doping type biomass carbon quantum dot corrosion inhibitor and preparation method and application thereof |
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