CN109097036A - A kind of longer emission wavelength fluorescent carbon quantum dot and preparation method thereof - Google Patents
A kind of longer emission wavelength fluorescent carbon quantum dot 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 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 4
- 238000000746 purification Methods 0.000 claims abstract description 3
- 238000000926 separation method Methods 0.000 claims abstract description 3
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 5
- 229920002873 Polyethylenimine Polymers 0.000 claims description 5
- 150000004985 diamines Chemical class 0.000 claims description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- 239000012046 mixed solvent Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 9
- 238000003384 imaging method Methods 0.000 abstract description 4
- 239000000090 biomarker Substances 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 238000013019 agitation Methods 0.000 description 4
- 229960000935 dehydrated alcohol Drugs 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 238000002189 fluorescence spectrum Methods 0.000 description 3
- 238000005374 membrane filtration Methods 0.000 description 3
- 238000000502 dialysis Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000001241 arc-discharge method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 125000003916 ethylene diamine group Chemical group 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 150000002466 imines Chemical class 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
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- Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
- Luminescent Compositions (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a kind of longer emission wavelength fluorescent carbon quantum dots and preparation method thereof.A certain proportion of passivator and solvent is added using L-AA as carbon source in this method, uniformly mixes to obtain clear transparent solutions；By mixed liquor be placed in reaction kettle high temperature reaction a few hours after cooled to room temperature；Reaction solution is passed through into separation and purification treatment, obtains fluorescent carbon quantum dot solution.Preparation method simple process of the invention, mild condition, production cost are low, environmentally protective；Carbon quantum dot obtained has the characteristics that fluorescence emission wavelengths are longer, it is uniform to can be realized controllable launch wavelength, good water solubility, surface nature diversity, particle diameter distribution by addition variety classes passivator, can be widely applied for the fields such as cell imaging, biomarker, biochemical sensitive.
Description
Technical field
The invention belongs to carbon field of nanometer technology, and in particular to a kind of longer emission wavelength fluorescent carbon quantum dot and its preparation
Method.
Background technique
Carbon quantum dot is that a kind of size is less than 10nm, the spherical nanoparticle being dispersed in water or other solvents.Carbon amounts
Son point is as a kind of novel fluorescence carbon nanomaterial, compared with traditional semiconductor-quantum-point, has fluorescence property stable, raw
The features such as object compatible degree height, good water solubility, smaller toxicity, can be widely applied to cell imaging, biomarker, drug and pass
It passs, the fields such as analysis detection, photoelectric conversion.
The preparation method of carbon quantum dot can be concluded as two classes: " from top to bottom " and " from bottom to top "." from top to bottom "
Method is that large-sized carbon material is processed into the carbon quantum dot of nano-scale by all means, mainly includes arc discharge
Method, laser ablation, electrochemical process etc.." from bottom to top " method is mainly anti-by a series of chemistry by reactant of small molecule
Carbon quantum dot should be made, mainly include hydro-thermal method, ultrasonic method, template etc..
The preparation of carbon quantum dot and application aspect still have some problems, such as the synthesis of most of carbon quantum dots at this stage
Method and step is cumbersome, higher cost, raw material type is various, aftertreatment technology is complicated；Most carbon quantum dot transmitting blues are glimmering
Light, blue light are small to the penetrability of tissue, and then limit carbon dots in the application in cell imaging field.Therefore, it prepares a kind of cheap
It is easy to get and the longer carbon quantum dot of fluorescence emission wavelengths has very important significance.
Summary of the invention
For at present most of carbon quantum dot preparation methods are cumbersome, fluorescence emission wavelengths concentrate on blue region phenomena such as,
The present invention provides a kind of longer emission wavelength fluorescent carbon quantum dot and preparation method thereof.
The technical solution of the present invention is as follows:
A kind of preparation method of longer emission wavelength fluorescent carbon quantum dot, specifically includes the following steps:
Step 1, using L-AA as carbon source, a certain proportion of passivator and solvent is added, uniformly mixes to clarify saturating
Bright solution；
Step 2, after mixed liquor being placed in reaction kettle high temperature reaction a few hours, cooled to room temperature；
Step 3, reaction solution is passed through into separation and purification treatment, obtains fluorescent carbon quantum dot solution.
Further, the concentration of L-AA is 0.01-0.05g/mL in clear transparent solutions in the step 1.
Further, solvent is that deionized water and methanol mixed solvent, deionized water and ethyl alcohol mixing are molten in the step 1
One of agent, deionized water and isopropyl alcohol mixed solvent, mixed proportion are volume ratio (0.5-1): (0.5-2).
Further, passivator is ethylenediamine (EDA), polyethyleneimine (PEI), polyethyleneoxide diamine in the step 1
One of (PEG-diamine), additional proportion is L-AA: the molar ratio of passivator is 1: (0-0.5).
Further, hydrothermal temperature is 60-200 DEG C in the step 2, and the reaction time is 4-24 hours.
The utility model has the advantages that
Raw material L-AA of the invention is from a wealth of sources, environmentally protective；Preparation method simple process of the invention, condition
Mildly, production cost is low；Carbon quantum dot fluorescence emission wavelengths obtained are longer, can be realized by adding variety classes passivator
Launch wavelength is controllable, and maximum emission wavelength range is 480-620nm, and good water solubility, surface nature diversity, particle diameter distribution
Uniformly, the fields such as cell imaging, biomarker, biochemical sensitive be can be widely applied for.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture of carbon quantum dot prepared by embodiment 1；
Fig. 2 is the fluorescence spectra of carbon quantum dot prepared by embodiment 1；
Fig. 3 is the infrared spectrogram of carbon quantum dot prepared by embodiment 1；
Fig. 4 is the fluorescence spectra of carbon quantum dot prepared by embodiment 2, embodiment 3 and embodiment 4.
Specific embodiment
Further description of the technical solution of the present invention for following embodiment.
Embodiment 1
Accurate measuring 30ml dehydrated alcohol and 30ml deionized water are uniformly mixed, and 1.5g L-AA is added thereto,
Magnetic agitation 15min is completely dissolved up to L-AA, obtains clear transparent solutions；It is 100ml that mixed liquor, which is transferred to volume,
Ptfe autoclave in, be put into 90 DEG C of reaction 6h of baking oven, take out reaction kettle cooled to room temperature；Then gained is anti-
0.22 μm of membrane filtration of liquid is answered, collecting filtrate and being placed in molecular cut off is dialysis in the bag filter of 1000Da for 24 hours to get glimmering
Light carbon quantum dot solution.
Transmission electron microscope, infrared spectroscopy and spectrofluorimetry are carried out to fluorescent carbon quantum dot obtained.
Fig. 1 is the transmission electron microscope picture of fluorescent carbon quantum dot manufactured in the present embodiment, and as can be seen from the figure carbon quantum dot is
Spheroidal particle, favorable dispersibility, even size distribution, average grain diameter are about 5nm.
Fig. 2 is the fluorescence spectra of fluorescent carbon quantum dot manufactured in the present embodiment, as shown, the maximum of the carbon quantum dot
Excitation wavelength and maximum emission wavelength are respectively 373nm and 535nm.
Fig. 3 is the infrared spectrogram of fluorescent carbon quantum dot manufactured in the present embodiment, as can be seen from the figure carbon quantum dot
Contain the hydrophilic radicals such as hydroxyl, carboxyl in surface.
Embodiment 2
Accurate measuring 30ml dehydrated alcohol and 30ml deionized water are uniformly mixed, and 1.5g L-AA is added thereto,
Magnetic agitation 15min is completely dissolved up to L-AA, then 0.01ml ethylenediamine (EDA) is added thereto, is uniformly mixed
Clear transparent solutions；Mixed liquor is transferred in the ptfe autoclave that volume is 100ml, is put into 90 DEG C of baking oven reactions
6h takes out reaction kettle cooled to room temperature；Then by 0.22 μm of membrane filtration of gained reaction solution, collection filtrate, which is placed in, is cut
It stays and dialyses in the bag filter that molecular weight is 1000Da for 24 hours to get fluorescent carbon quantum dot solution.
Embodiment 3
Accurate measuring 30ml dehydrated alcohol and 30ml deionized water are uniformly mixed, and 1.5g L-AA is added thereto,
Magnetic agitation 15min is until L-AA is completely dissolved, then 0.01ml polyethyleneoxide diamine (PEG- is added thereto
Diamine), it is uniformly mixed to obtain clear transparent solutions；Mixed liquor is transferred to the ptfe autoclave that volume is 100ml
In, 90 DEG C of reaction 6h of baking oven are put into, reaction kettle cooled to room temperature is taken out；Then by 0.22 μm of filter membrane of gained reaction solution
Filtering, collecting filtrate and being placed in molecular cut off is dialysis in the bag filter of 1000Da for 24 hours to get fluorescent carbon quantum dot solution.
Embodiment 4
Accurate measuring 30ml dehydrated alcohol and 30ml deionized water are uniformly mixed, and 1.5g L-AA is added thereto,
For magnetic agitation 15min until L-AA is completely dissolved, then 0.01ml polyethyleneimine (PEI) is added thereto, mixing is equal
It is even to obtain clear transparent solutions；Mixed liquor is transferred in the ptfe autoclave that volume is 100ml, is put into 90 DEG C of baking oven instead
6h is answered, reaction kettle cooled to room temperature is taken out；Then it by 0.22 μm of membrane filtration of gained reaction solution, collects filtrate and is placed in
Molecular cut off is to dialyse in the bag filter of 1000Da for 24 hours to get fluorescent carbon quantum dot solution.
Spectrofluorimetry is carried out to fluorescent carbon quantum dot made from embodiment 2, embodiment 3 and embodiment 4, such as Fig. 4 institute
Show, by adding variety classes passivator, to can be realized launch wavelength controllable, and ethylenediamine, polyethyleneoxide diamine, polyethylene is added
The maximum emission wavelength of carbon quantum dot made from imines is respectively 485nm, 534nm and 609nm.
It should be pointed out that as described above is only to explain the preferred embodiments of the invention, it is right accordingly to be not intended to
The present invention is subject to any form of limitation, therefore all have any modification for making the related present invention under identical spirit
Or change, it should all be included in the scope that the invention is intended to protect.
Claims (7)
1. a kind of preparation method of longer emission wavelength fluorescent carbon quantum dot, which is characterized in that specific step is as follows:
(1) using L-AA as carbon source, a certain proportion of passivator and solvent is added, uniformly mixes to obtain clear transparent solutions；
(2) after mixed liquor being placed in reaction kettle high temperature reaction a few hours, cooled to room temperature；
(3) reaction solution is passed through into separation and purification treatment, obtains fluorescent carbon quantum dot solution.
2. the preparation method of longer emission wavelength fluorescent carbon quantum dot according to claim 1, which is characterized in that the step
Suddenly the concentration of L-AA is 0.01-0.05g/mL in clear transparent solutions in (1).
3. the preparation method of longer emission wavelength fluorescent carbon quantum dot according to claim 1, which is characterized in that the step
Suddenly solvent is that deionized water and methanol mixed solvent, deionized water and alcohol mixed solvent, deionized water and isopropanol are mixed in (1)
One of bonding solvent, mixed proportion are volume ratio (0.5-1): (0.5-2).
4. the preparation method of longer emission wavelength fluorescent carbon quantum dot according to claim 1, which is characterized in that the step
Suddenly passivator is one of ethylenediamine, polyethyleneimine, polyethyleneoxide diamine in (1), and additional proportion is L-AA: blunt
The molar ratio of agent is 1: (0-0.5).
5. the preparation method of longer emission wavelength fluorescent carbon quantum dot according to claim 1, which is characterized in that the step
Suddenly hydrothermal temperature is 60-200 DEG C in (1), and the reaction time is 4-24 hours.
6. a kind of utilize fluorescent carbon quantum dot made from the preparation method as described in claim any one of 1-5, which is characterized in that institute
Stating carbon quantum dot is spheroidal particle, partial size 2-9nm.
7. fluorescent carbon quantum dot according to claim 6, which is characterized in that the carbon quantum dot transmitting longer wavelength is glimmering
Light, by adding variety classes passivator, to can be realized launch wavelength controllable, and maximum emission wavelength range is 480-620nm.
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Cited By (10)
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| CN109455692A (en) * | 2018-12-29 | 2019-03-12 | 太原理工大学 | A kind of chirality carbon quantum dot and preparation method thereof |
| CN109705850A (en) * | 2019-01-28 | 2019-05-03 | 天津师范大学 | The synthetic method and its application of one type graphene quantum dot MB |
| CN109777407A (en) * | 2019-02-18 | 2019-05-21 | 东北林业大学 | A kind of double transmitting carbon quantum dots and its organic compound film, preparation method and application with pH sensibility |
| CN109991200A (en) * | 2019-04-08 | 2019-07-09 | 皖西学院 | The amine-modified ascorbic acid carbon nano dot of polyethyleneimine, preparation method and application |
| CN112461807A (en) * | 2020-11-26 | 2021-03-09 | 山西大学 | Application of carbon quantum dots in targeted nucleolus wash-free imaging |
| CN113201332A (en) * | 2021-04-27 | 2021-08-03 | 晋中学院 | Preparation method of green fluorescent carbon quantum dot hydrogel |
| CN114806554A (en) * | 2022-04-13 | 2022-07-29 | 中国科学院苏州生物医学工程技术研究所 | Phosphorescent carbon dot, application thereof in anti-counterfeiting and information encryption and LED lamp bead based on phosphorescent carbon dot |
| CN115159506A (en) * | 2022-07-12 | 2022-10-11 | 苏州大学 | Branched polyethyleneimine-based nitrogen-doped multicolor fluorescent carbon dot and preparation method thereof |
| CN115322776A (en) * | 2022-07-12 | 2022-11-11 | 公安部物证鉴定中心 | Fingerprint developing agent based on nitrogen-doped multicolor fluorescent carbon dots, preparation method and application |
| CN115820250A (en) * | 2022-12-20 | 2023-03-21 | 珠海科技学院 | Method for simultaneously synthesizing hydrophilic carbon quantum dots and hydrophobic carbon quantum dots |
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Cited By (15)
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| CN109455692A (en) * | 2018-12-29 | 2019-03-12 | 太原理工大学 | A kind of chirality carbon quantum dot and preparation method thereof |
| CN109705850A (en) * | 2019-01-28 | 2019-05-03 | 天津师范大学 | The synthetic method and its application of one type graphene quantum dot MB |
| CN109705850B (en) * | 2019-01-28 | 2022-04-15 | 天津师范大学 | Synthetic method and application of graphene-like quantum dot MB |
| CN109777407A (en) * | 2019-02-18 | 2019-05-21 | 东北林业大学 | A kind of double transmitting carbon quantum dots and its organic compound film, preparation method and application with pH sensibility |
| CN109991200B (en) * | 2019-04-08 | 2021-09-14 | 皖西学院 | Polyethyleneimine modified ascorbic acid carbon nanodot as well as preparation method and application thereof |
| CN109991200A (en) * | 2019-04-08 | 2019-07-09 | 皖西学院 | The amine-modified ascorbic acid carbon nano dot of polyethyleneimine, preparation method and application |
| CN112461807A (en) * | 2020-11-26 | 2021-03-09 | 山西大学 | Application of carbon quantum dots in targeted nucleolus wash-free imaging |
| CN113201332A (en) * | 2021-04-27 | 2021-08-03 | 晋中学院 | Preparation method of green fluorescent carbon quantum dot hydrogel |
| CN113201332B (en) * | 2021-04-27 | 2023-11-28 | 晋中学院 | Preparation method of green fluorescent carbon quantum dot hydrogel |
| CN114806554A (en) * | 2022-04-13 | 2022-07-29 | 中国科学院苏州生物医学工程技术研究所 | Phosphorescent carbon dot, application thereof in anti-counterfeiting and information encryption and LED lamp bead based on phosphorescent carbon dot |
| CN115159506A (en) * | 2022-07-12 | 2022-10-11 | 苏州大学 | Branched polyethyleneimine-based nitrogen-doped multicolor fluorescent carbon dot and preparation method thereof |
| CN115322776A (en) * | 2022-07-12 | 2022-11-11 | 公安部物证鉴定中心 | Fingerprint developing agent based on nitrogen-doped multicolor fluorescent carbon dots, preparation method and application |
| CN115322776B (en) * | 2022-07-12 | 2024-08-13 | 公安部物证鉴定中心 | Fingerprint developing agent based on nitrogen-doped multicolor fluorescent carbon dots, preparation method and application |
| CN115820250A (en) * | 2022-12-20 | 2023-03-21 | 珠海科技学院 | Method for simultaneously synthesizing hydrophilic carbon quantum dots and hydrophobic carbon quantum dots |
| CN115820250B (en) * | 2022-12-20 | 2023-10-17 | 珠海科技学院 | Method for simultaneously synthesizing hydrophilic carbon quantum dots and hydrophobic carbon quantum dots |
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