CN109609123B - Red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot and preparation and application thereof - Google Patents
Red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot and preparation and application thereof Download PDFInfo
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Abstract
The invention provides a red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot and preparation and application thereof. The method comprises the following steps: s1, dispersing L-cystine and o-phenylenediamine in ethanol to obtain a precursor solution; s2, reacting the precursor solution in a reaction kettle, and cooling the reaction solution to room temperature after the reaction is finished to obtain a dark red carbon dot solution; s3, filtering and purifying the dark red carbon dot solution; and S4, removing the solvent from the filtrate and drying to obtain the red/yellow double-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot solid. The method has the advantages of few required raw materials, few intermediate products and byproducts, high reaction speed, economy, environmental protection, good dispersibility of the obtained fluorescent carbon quantum dots, uniform granularity, little toxicity, excellent reversible pH performance, higher fluorescence quantum yield and good stability.
Description
Technical Field
The invention belongs to the field of nano materials. In particular to a red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot and preparation and application thereof.
Background
Carbon is the basis of all known lives on the earth and plays a significant role in the development of modern science and technology. Most carbon quantum dots are mainly composed of amorphous carbon to crystallized carbon core with sp2Mainly hybridized carbon, and the lattice spacing of the carbon quantum dots is consistent with the structure of graphitic carbon or amorphous layered carbon. Carbon quantum dots (Carbon dots) are a fluorescent nano material with the particle size of less than 10nm, mainly comprise Carbon elements, do not contain heavy metal elements, are a novel nano material, are used as substitutes of traditional semiconductor quantum dots, and appear and attract great attention in the past decade. Its excellent properties include low toxicity, simple and low cost synthesis process, biocompatibility and excellent fluorescence properties. The properties enable the carbon dots to have wide application prospects in the aspects of detection probes, biomedical imaging, sensing, catalysis, anti-counterfeiting, drug delivery, photovoltaic devices, energy conversion and the like.
In recent years, many scientists have tried to develop various methods for synthesizing carbon quantum dots and to master the control of their optical properties. Most of the studies are centered around blue, green and yellow fluorescent carbon quantum dots, and the synthesis method of red fluorescent carbon dots is rarely reported.
Disclosure of Invention
The invention aims to provide a red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot and preparation and application thereof. The method has the advantages of few required raw materials, few intermediate products and byproducts, high reaction speed, economy, environmental protection, good dispersibility of the obtained fluorescent carbon quantum dots, uniform granularity, little toxicity, excellent reversible pH performance, higher fluorescence quantum yield and good stability.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dots, which comprises the following steps:
s1, dispersing L-cystine and o-phenylenediamine in ethanol to obtain a precursor solution;
s2, reacting the precursor solution in a reaction kettle, and cooling the reaction solution to room temperature after the reaction is finished to obtain a dark red carbon dot solution;
s3, filtering and purifying the dark red carbon dot solution;
and S4, removing the solvent from the filtrate and drying to obtain the red/yellow double-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot solid.
The red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot with high fluorescent quantum yield is obtained by one-step synthesis through a solvothermal method.
Wherein the L-cystine as sulfur source is a sulfur-containing amino acid containing-S-S-disulfide bond.
The nitrogen source and the carbon source o-phenylenediamine contain benzene rings and amino groups, and can perform substitution reaction on the rings.
Preferably, the mass ratio of L-cystine to o-phenylenediamine in the precursor solution in S1 is 1: 0.1-1: 10; for example, 1:0.1, 1:1, 1:4, or 1: 10. When the mass ratio of L-cystine to o-phenylenediamine is 1:4, the fluorescence intensity value is the largest, the quantum yield is the highest, and the fluorescence intensity value is obviously reduced when the mass ratio is lower than or higher than 1: 4. Therefore, the mass ratio of the L-cystine to the o-phenylenediamine is preferably 1:4, so as to ensure that the obtained red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dots have the optimal fluorescent effect.
Preferably, L-cystine and o-phenylenediamine are dispersed in ethanol in S1, and a precursor solution is obtained after ultrasonic treatment; because L-cystine is not dissolved in ethanol solution, the precursor solution obtained after ultrasonic treatment is white suspension. Preferably, the sonication time is 5 min. The precursor can be fully and completely dispersed in ethanol by adding ultrasonic operation, so that a uniform precursor solution can be obtained.
Preferably, the reaction vessel in S2 is a stainless steel autoclave lined with polytetrafluoroethylene.
Preferably, the temperature of the reaction in S2 is 160-240 ℃, preferably 220 ℃; the reaction time is 8 hours or more, for example, 8 hours, 10 hours, 12 hours, 14 hours, 16 hours, and preferably 12 hours.
Preferably, the filtration purification in S3 is performed using a cylindrical membrane separation filter. And (4) filtering for many times to remove large particles, wherein the filtrate is the carbon point solution.
Further preferably, the cylindrical membrane separation filter has a molecular weight cut-off of one or a combination of 3kDa, 5kDa, 10kDa, 20kDa and 30 kDa. The carbon dots are of a small size and a filter head with an excessive molecular weight cut-off cannot be selected to avoid the failure to remove part of the impurities.
In addition, the filtration purification described in S3 can also filter the prepared carbon dot solution multiple times using a 0.22 μm filter head.
Preferably, the step of removing the solvent from the filtrate and drying in S4 includes: and (3) carrying out rotary evaporation on the solution at the temperature of 30-40 ℃ to remove the solvent, and then drying the solution at the temperature of 50-80 ℃ for 0.5-1 h. As will be readily understood by those skilled in the art, there are many options for the solvent removal and drying means, such as vacuum drying, lyophilization, and the like, and the present invention is not limited thereto, but only the solvent removal and drying effects are achieved.
The invention also provides the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot prepared by the preparation method. The carbon quantum dots prepared by the method have high fluorescence quantum yield, less raw materials and high fluorescence intensity.
Preferably, the size of the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot is 2-5 nm.
The invention also provides the application of the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot, which specifically comprises the application in Ag+Detection, pH detection, cell detection or identification of rock fractures.
Further, the present invention provides a method of identifying a rock fracture, the method comprising the steps of:
1) adding the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dots into a solvent to prepare a carbon quantum dot solution; preferably, the solvent is an ethanol solution.
2) And dripping the carbon quantum dot solution on the surface of the rock.
3) The rock was observed under an ultraviolet lamp to identify cracks. Compared with the prior art, the invention has the following beneficial effects:
the preparation method can prepare the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot by only one-step reaction, has high reaction speed, few byproducts, little raw material consumption and low cost, and the obtained carbon quantum dot has high light intensity, low toxicity and high fluorescent quantum yield, and is successfully applied to Ag+And pH detection, and has wide application prospect in cell detection and other aspects.
Drawings
Fig. 1 is a transmission electron microscope image of the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot prepared in example 1 of the present invention.
Fig. 2 is an atomic force microscope spectrum of the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot prepared in example 1 of the present invention.
Fig. 3 is a fluorescence spectrum of the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot prepared in example 1 in ethanol.
Fig. 4 is a fluorescence spectrum of the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot prepared in example 1 of the present invention in an acid solution with a pH of 1.
FIG. 5 is an FTIR spectrum of the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot prepared in example 2 of the invention.
Fig. 6 is a peak spectrum of C1s of the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot prepared in example 2 of the present invention.
FIG. 7 is a peak separation spectrum of N1s of the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot prepared in example 2 of the present invention.
FIG. 8 is a peak-splitting spectrum of O1s of the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot prepared in example 2 of the present invention.
Fig. 9 is a peak separation spectrum of S2p of the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot prepared in example 2 of the present invention.
FIG. 10 shows that Ag with different concentrations is added to red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dots prepared in example 2 of the present invention+Curve of the intensity of the post photoluminescence.
Fig. 11 is a graph of fluorescence intensity curves of red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dots prepared in example 2 of the present invention at 540ex, after the pH changes from 1.0 to 13.0 and then to 1.0, which was repeated 10 times.
Fig. 12 is a toxicity test of the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot prepared in example 2 of the present invention.
FIG. 13 is a rock surface observed under an ultraviolet lamp in example 2 of the present invention.
FIG. 14 shows that in example 2 of the present invention, after the carbon quantum dot solution is dripped on the rock surface, the rock gap is observed under an ultraviolet lamp.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below in connection with preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
Example 1
(a) Taking L-cystine (0.0625g) and o-phenylenediamine (0.25g) to disperse in 10mL ethanol, and then carrying out ultrasonic treatment for 5min to obtain a precursor solution.
(b) Placing the obtained precursor solution into a 50mL stainless steel autoclave with a polytetrafluoroethylene lining, sealing, reacting for 12h at 220 ℃, and naturally cooling to room temperature to obtain a dark red carbon dot solution;
(c) the dark red carbon spot solution was filtered through a 3kDa cut-off cylindrical membrane separation filter, and the filtrate was collected and 20uL of the filtrate was diluted to 2mL with ethanol.
Referring to fig. 1, it is a transmission electron microscope image of the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot prepared in this example, and the carbon quantum dot is in a regular monodisperse sphere shape. The average particle size obtained from the test in FIG. 1 was 2.97nm, and the lattice spacing was about 0.203nm, reflecting the (100) crystal planes of graphite.
Referring to fig. 2, which is an atomic force microscope (afm) spectrum of the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot prepared in this example, it can be seen from fig. 2 that the size of the carbon quantum dot is between 2nm and 5 nm.
Referring to fig. 3 and 4, there are shown fluorescence spectra of the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dots prepared in this example diluted in ethanol and an acid solution with pH of 1; as can be seen from the figure, when the fluorescent material is diluted in ethanol, the strongest fluorescence intensity can be obtained when the excitation wavelength is 540nm, and the peak positions of the fluorescence emission spectrum are 595nm and 648 nm; when diluted in hydrochloric acid of pH 1, the strongest fluorescence intensity was obtained at an excitation wavelength of 580nm, and the peak positions of fluorescence emission spectra were 628nm and 675 nm. This indicates that different environmental conditions have a significant impact on the optical properties of nitrogen and sulfur co-doped carbon quantum dots and that the emission sites of CD are more sensitive to solvent polarity due to their smaller size. Obviously, the photoluminescence properties of nitrogen and sulfur co-doped carbon quantum dots remain almost unchanged, indicating that their unique photoluminescence properties can be used for various applications in these solvent systems.
Example 2
(a) Taking 0.0625g of L-cystine and 0.25g of o-phenylenediamine, dispersing in 10mL of ethanol, and carrying out ultrasonic treatment for 5min to obtain a precursor solution.
(b) And placing the obtained precursor solution into a 50mL stainless steel autoclave lined with polytetrafluoroethylene, sealing, reacting for 12h at 220 ℃, and naturally cooling to room temperature to obtain a dark red carbon dot solution.
(c) And filtering the dark red carbon dot solution by using a cylindrical membrane separation filter with the molecular weight cutoff of 3kDa, collecting filtrate, and performing rotary evaporation and drying to obtain carbon quantum dot solid powder with high fluorescence yield. The carbon quantum dot obtained in the embodiment has the luminous intensity of 2.09/10e under the irradiation of 540nm light6(a.u.)。
Referring to fig. 5, FTIR spectra of the red/yellow dual wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dots prepared in this example further confirm the presence of oxygen-containing groups (O-H, -COO-, C ═ O) and C-S, C ═ C, and C-N.
Referring to fig. 6 to 9, XPS peak profiles of the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dots prepared in this example show that the surfaces of the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dots contain a large amount of C, O, N, S elements.
Referring to fig. 10, Ag with different concentrations is added to the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dots prepared in this example+Graph of the variation of the post photoluminescence intensity. Prepared nitrogen and sulfur co-doped carbon quantum dot fluorescence in Ag+Sharp and fast response in solution and with Ag in solution+The fluorescence intensity of the nitrogen and sulfur co-doped carbon quantum dots is gradually reduced when the concentration is increased.
Fig. 11 is a graph of fluorescence intensity curves of the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dots prepared in this example, under 540nm excitation light, the pH changes from 1.0 to 13.0 and then to 1.0, and the process is repeated 10 times. It can be seen that the carbon dot has good pH response characteristic and reversible characteristic under 540nm excitation light.
FIG. 12 is a toxicity test of the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot prepared by the implementation of the invention. The survival rate of the cells is over 80 percent when the carbon point concentration is 0-1000 mg/L.
Fig. 13 and 14 show the application of the red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dots prepared by the implementation of the invention in rock crack identification. As can be seen from the figure, the carbon dots can be obviously observed in rock gaps under an ultraviolet lamp after being dripped on the surface of the rock.
Example 3
(a) Taking 0.0625g of L-cystine and 0.25g of o-phenylenediamine, dispersing in 10mL of ethanol, and carrying out ultrasonic treatment for 5min to obtain a precursor solution;
(b) placing the obtained precursor solution into a 50mL stainless steel autoclave with a polytetrafluoroethylene lining, sealing, reacting for 8h at 220 ℃, and naturally cooling to room temperature to obtain a dark red solution;
(c) and filtering the dark red solution by using a cylindrical membrane separation filter with the molecular weight cutoff of 3kDa, collecting filtrate, and performing rotary evaporation and drying to obtain carbon quantum dot solid powder with high fluorescence yield. The carbon quantum dot obtained in the embodiment has the luminous intensity of 1.32/10e under the irradiation of 540nm light6(a.u.)。
Example 4
(a) Taking 0.0625g of L-cystine and 0.25g of o-phenylenediamine, dispersing in 10mL of ethanol, and carrying out ultrasonic treatment for 5min to obtain a precursor solution.
(b) And placing the obtained precursor solution into a 50mL stainless steel autoclave lined with polytetrafluoroethylene, sealing, reacting for 12h at the temperature of 180 ℃, and naturally cooling to room temperature to obtain a dark red carbon dot solution.
(c) And filtering the dark red carbon dot solution by using a cylindrical membrane separation filter with the molecular weight cutoff of 3kDa, and collecting filtrate. The carbon quantum dot obtained in the embodiment has the luminous intensity of 1.15/10e under the irradiation of 540nm light6(a.u.)。
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention, and it will be obvious to those skilled in the art that other variations or modifications may be made on the basis of the above description, and all embodiments may not be exhaustive, and all obvious variations or modifications may be included within the scope of the present invention.
Claims (10)
1. A preparation method of red/yellow dual-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dots is characterized by comprising the following steps:
s1, dispersing L-cystine and o-phenylenediamine in ethanol to obtain a precursor solution;
s2, reacting the precursor solution in a reaction kettle, and cooling the reaction solution to room temperature after the reaction is finished to obtain a dark red carbon dot solution;
s3, filtering and purifying the dark red carbon dot solution;
and S4, removing the solvent from the filtrate and drying to obtain the red/yellow double-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot solid.
2. The preparation method according to claim 1, wherein the mass ratio of L-cystine to o-phenylenediamine in the precursor solution in S1 is 1: 0.1-1: 10.
3. The method according to claim 1, wherein the precursor solution is obtained by dispersing L-cystine and o-phenylenediamine in ethanol in S1 and subjecting the mixture to ultrasonic treatment.
4. The method according to claim 1, wherein the reaction vessel in S2 is a stainless steel autoclave lined with polytetrafluoroethylene.
5. The method according to claim 1, wherein the temperature of the reaction in S2 is 160 to 240 ℃; the reaction time is more than 8 h.
6. The method according to claim 1, wherein the filtration purification in S3 is performed using a cylindrical membrane separation filter.
7. The method according to claim 6, wherein the cylindrical membrane separation filter has a molecular weight cut-off of 3kDa, 5kDa, 10kDa, 20kDa, or 30 kDa.
8. The method according to claim 1, wherein the step of removing the solvent from the filtrate and drying in S4 comprises:
and (3) carrying out rotary evaporation on the solution at the temperature of 30-40 ℃ to remove the solvent, and then drying the solution at the temperature of 50-80 ℃ for 0.5-1 h.
9. Red/yellow double-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot prepared by the preparation method of any one of claims 1-8 in Ag+Detection, pH detection, cell detection or identification of rock fractures.
10. A method of identifying a rock fracture, the method comprising the steps of:
1) adding the red/yellow double-wavelength nitrogen and sulfur co-doped fluorescent carbon quantum dot prepared by the preparation method of any one of claims 1-8 into a solvent to prepare a carbon quantum dot solution;
2) dripping the carbon quantum dot solution on the surface of the rock;
3) the rock was observed under an ultraviolet lamp to identify cracks.
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