CN108410455B - Method for simultaneously synthesizing hydrophilic and hydrophobic carbon dots and method for detecting Au by using same3+And application in preparing white light LED - Google Patents

Method for simultaneously synthesizing hydrophilic and hydrophobic carbon dots and method for detecting Au by using same3+And application in preparing white light LED Download PDF

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CN108410455B
CN108410455B CN201810183982.0A CN201810183982A CN108410455B CN 108410455 B CN108410455 B CN 108410455B CN 201810183982 A CN201810183982 A CN 201810183982A CN 108410455 B CN108410455 B CN 108410455B
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carbon dots
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hydrophobic carbon
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CN108410455A (en
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周艳梅
高文莉
祁志冲
刘山虎
徐成功
宋昊翰
王晓
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Henan University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • 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
    • G01N21/6486—Measuring fluorescence of biological material, e.g. DNA, RNA, cells
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    • H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
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    • Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps

Abstract

Method for simultaneously synthesizing hydrophilic and hydrophobic carbon dots and method for detecting Au by using same3+The application in preparing the white light LED belongs to the field of fluorescent carbon nano materials, sulfuric acid is used as a raw material, ethanol is used for dissolving the sulfuric acid, and the mixture is stirred to form a uniform mixed solution; transferring the mixed solution into a polytetrafluoroethylene high-pressure reaction kettle, heating at 200 ℃, and then cooling to room temperature to obtain a black lower layer solution which is hydrophilic carbon dots and a red upper layer solution which is hydrophobic carbon dots.

Description

Simultaneous synthesisMethod for detecting hydrophilic and hydrophobic carbon dots and detection method of Au3+And application in preparing white light LED
Technical Field
The invention belongs to the field of fluorescent carbon nano materials, and particularly relates to a method for simultaneously synthesizing hydrophilic and hydrophobic carbon dots and a method for detecting Au by using the same3+And application in preparing white light LED.
Background
Fluorescent carbon dots have shown great application potential in the fields of sensing, biological imaging, photocatalysis, photovoltaic devices, solar cells and the like due to excellent optical properties, good light stability, lower cytotoxicity and other excellent characteristics.
Most of the carbon dots synthesized at present exhibit hydrophilic properties, and in recent research, hydrophobic carbon dots have been receiving wide attention due to their applications in electronic devices, drug delivery, and the like, but the synthesis of both hydrophilic and hydrophobic carbon dots using low cost and simple steps cannot be achieved in the prior art. Therefore, the selection of low-cost precursors and reasonable techniques for simultaneously preparing hydrophilic and hydrophobic carbon dots are of great significance.
Gold, as a noble metal, plays an important role in the fields of catalysis, biology, medicine, etc., however, the significant increase of gold catalysts and gold nanoparticles, together with Au, is based on3+The associated toxicity is also significantly increased and found to be potentially bio-toxic. Au coating3+Can be tightly combined with various enzymes and DNA, and can cause damage to liver, kidney and peripheral nervous system, but the prior art can not realize visual detection analysis when gold ions in tissues and cells are detected by using carbon points.
The white light emitting diode is a new generation of green light source, has long service life, and is energy-saving and environment-friendly. Semiconductor quantum dots have attracted increasing attention in the field of white light emitting diodes due to their tunable emission, high quantum yield, and narrow emission bandwidth. However, conventional quantum dots usually contain toxic heavy metals, which have toxicity and will cause harm to the environment and human beings, and this will limit their development to some extent, and it will be very meaningful to develop new materials with low cost and low toxicity for preparing white light emitting diodes.
Disclosure of Invention
The method aims to solve the problems that in the prior art, hydrophilic and hydrophobic carbon points cannot be synthesized simultaneously by using lower cost and simple steps, visual detection and analysis cannot be realized when the carbon points detect gold ions in tissues and cells, and quantum dots adopted by a white light emitting diode usually have certain toxicity, so that the environment and human beings are harmed. The invention aims to provide a simple method for simultaneously synthesizing hydrophilic carbon dots and hydrophobic carbon dots, 8mg of methylene blue is added into the raw materials, the prepared hydrophilic carbon dots can be used for manufacturing a white light-emitting diode under the irradiation of 365nm ultraviolet light, and the prepared hydrophilic carbon dots can be used as fluorescent probes to sensitively and selectively detect gold ions, so that visual detection and analysis can be realized on the gold ions in cells.
The above object of the present invention is achieved by the following technical solutions: a method for simultaneously synthesizing hydrophilic and hydrophobic carbon dots, comprising the steps of:
(1) dissolving 0.1mL of concentrated sulfuric acid (standard concentration) by using ethanol, and stirring for 1-2 min to form a uniform mixed solution;
(2) and (2) transferring the mixed solution in the step (1) to a polytetrafluoroethylene high-pressure reaction kettle, heating at 200 ℃ for 6h, and cooling to room temperature to obtain a black lower-layer solution which is hydrophilic carbon dots and a red upper-layer solution which is hydrophobic carbon dots.
Preferably, the upper solution and the lower solution in step (2) are filtered through 0.22 μ M filter membrane to obtain pure hydrophilic and hydrophobic carbon spots.
Preferably, the ethanol solution in step (1) is 10mL, and the polytetrafluoroethylene high-pressure reaction kettle in step (2) is 25 mL.
Preferably, methylene blue is added in the step (1), and the methylene blue and the sulfuric acid are dissolved by ethanol and stirred to form a uniform mixed solution.
Preferably, the methylene blue in step (1) is 8 mg.
The hydrophilic carbon dots are applied to preparing the white light-emitting diode: dissolving 8mg of methylene blue 0.1mL of concentrated sulfuric acid in 10mL of ethanol, and stirring for 1-2 min to form a uniform mixed solution; transferring the obtained mixed solution into a 25mL polytetrafluoroethylene high-pressure reaction kettle, heating at 200 ℃ for 6h, and cooling to room temperature to obtain a black lower layer solution which is hydrophilic carbon dots and a red upper layer solution which is hydrophobic carbon dots. The hydrophilic carbon dots and the hydrophobic carbon dots are dissolved in distilled water and ethanol, the hydrophilic carbon dots show bright white under 365nm ultraviolet light irradiation, and the hydrophobic carbon dots show bright blue fluorescence under 365nm ultraviolet light irradiation. The hydrophilic carbon dots capable of emitting white light and the polyvinyl alcohol composite coating can be used for manufacturing a white light emitting diode on the ultraviolet light emitting diode.
The synthesized hydrophilic carbon dots can be used for detecting gold ions.
Preferably, the hydrophilic carbon dots are used as fluorescent probes to detect gold ions.
Preferably, the method is used for detecting gold ions in the water body.
Preferably, the method is used for detecting gold ions in cells.
Compared with the carbon dots synthesized in the prior art, the invention has the following beneficial effects:
1. the invention provides a method for simultaneously synthesizing hydrophilic carbon dots and hydrophobic carbon dots, which uses sulfuric acid as a raw material and ethanol as a solvent, has the characteristics of low cost, simple synthesis method and the like, and solves the defect that the hydrophilic and hydrophobic carbon dots cannot be simultaneously synthesized by using lower cost and simple steps in the prior art;
2. simultaneously, 8mg of methylene blue is added into the raw materials, the methylene blue and sulfuric acid are used as raw materials, the prepared hydrophilic carbon dots and hydrophobic carbon dots are respectively dissolved in distilled water and ethanol, the hydrophilic carbon dots emit bright white and the hydrophobic carbon dots emit blue fluorescence under the irradiation of 365nm ultraviolet light, and the hydrophilic carbon dots emitting white light and a polyvinyl alcohol composite coating can be used for manufacturing a white light emitting diode on the ultraviolet light emitting diode, so that the problem that the traditional quantum dots usually have certain toxicity and can cause harm to the environment and human beings is solved;
3. the hydrophilic carbon dots prepared by the method can be used as fluorescent probes for sensitively and selectively detecting gold ions, can realize visual detection and analysis on the gold ions in cells, and has the functions of tracking and analyzing tissues and Au in organisms3+The potential application value of the method solves the problem that visual detection and analysis can not be realized when the hydrophilic carbon points are used for detecting gold ions in tissues and cells in the prior art.
Drawings
FIG. 1 provides a transmission electron microscope image and an atomic particle microscope image of hydrophilic and hydrophobic carbon dots;
FIG. 2 provides an X-ray photoelectron spectrum of hydrophilic and hydrophobic carbon dots according to the present invention;
FIG. 3 provides Fourier infrared spectra of hydrophilic and hydrophobic carbon dots;
FIG. 4 provides a fluorescent photograph of hydrophilic and hydrophobic carbon dots under irradiation of 365nm ultraviolet light;
FIG. 5 is a graph showing the selective and competitive fluorescence response of hydrophilic carbon sites to different metal ions according to the present invention;
FIG. 6 shows the hydrophilic carbon dot pairs of the present invention to Au in cells3+Detecting;
FIG. 7 is a graph of the fluorescence emission spectrum of a white light LED prepared by coating an ultraviolet LED with hydrophilic carbon dots and a polyvinyl alcohol compound, a photograph of the white light LED and the color coordinate of the International Commission on illumination.
The specific implementation mode is as follows:
in order to better understand the invention, the following description of the implementation of the example further illustrate the content of the invention, but the content of the invention is not limited to the following embodiments.
Example 1
Method for simultaneously synthesizing hydrophilic and hydrophobic carbon dots and method for detecting Au by using same3+And application in preparing white light LED.
The method for preparing the hydrophilic and hydrophobic carbon dots comprises the following steps:
(1) dissolving 8mg of methylene blue and 0.1mL of sulfuric acid (standard concentrated sulfuric acid is selected) in 10mL of ethanol, and stirring to form a uniform mixed solution;
(2) transferring the mixed solution into a 25mL polytetrafluoroethylene high-pressure reaction kettle, heating for 6h at 200 ℃, and cooling to room temperature to obtain black lower-layer solution which is hydrophilic carbon dots and red hydrophobic carbon dots of upper-layer liquid;
(3) the upper and lower solutions were filtered through 0.22 μ M filters to obtain pure hydrophilic and hydrophobic carbon spots.
And detecting different metal ions by taking the hydrophilic carbon dots as fluorescent probes.
The hydrophilic carbon dots are used as fluorescent probes for Au in cells3+And (6) detecting.
Respectively dissolving the hydrophilic and hydrophobic carbon dots in distilled water and ethanol, and irradiating with 365nm ultraviolet light.
(II) results:
(1) the transmission electron microscope image and the atomic particle microscope image of the hydrophilic and hydrophobic carbon dots obtained in example 1 are shown in FIG. 1: transmission electron micrographs and atomic particle micrographs of the hydrophilic and hydrophobic carbon dots showing that the hydrophilic and hydrophobic carbon dots have a spheroidal structure. Wherein the particle size of the hydrophobic carbon dots is larger than that of the hydrophilic carbon dots.
(2) The X-ray photoelectron spectrum of the hydrophilic and hydrophobic carbon dots obtained in example 1 is shown in FIG. 2: the X-ray photoelectron spectrum of hydrophilic and hydrophobic carbon points shows four distinct peaks at 532.1 eV, 401.9 eV, 284.6 eV and 168.9 eV, corresponding to O1S, N1S, C1S and S2 p. The oxygen content of the hydrophilic and hydrophobic carbon dots is 42.93% and 28.45%, respectively, and the high-resolution energy spectrums of O1s of the hydrophilic and hydrophobic carbon dots show that the hydrophilic carbon dots contain hydrophilic hydroxyl functional groups.
(3) The Fourier infrared spectrum of the hydrophilic and hydrophobic carbon dots obtained in example 1 is shown in FIG. 3: and Fourier infrared spectrum of the hydrophilic and hydrophobic carbon points shows that the surface of the hydrophilic carbon points contains hydrophilic hydroxyl functional groups, and the hydrophobic carbon points do not have hydroxyl functional groups.
(4) The fluorescence spectra of the hydrophilic and hydrophobic carbon dots obtained in example 1 and a fluorescence photograph under 365nm UV lamp are shown in FIG. 4: fluorescence spectra of the hydrophilic and hydrophobic carbon dots, which shows that the hydrophilic and hydrophobic carbon dots have the property that the excitation wavelength depends on the emission wavelength. Fluorescence photographs under UV light irradiation of the hydrophilic and hydrophobic carbon dots show that the hydrophilic and hydrophobic carbon dots show bright white and blue fluorescence, respectively, under 365nm UV light irradiation.
(5) Fluorescence intensity (F/F) of hydrophilic carbon sites obtained in example 1 for selectivity and competitiveness of different metal ions0) The variation is shown in FIG. 5: it shows that hydrophilic carbon dots can specifically detect Au3+And has good selectivity and anti-interference capability.
(6) Hydrophilic carbon sites obtained in example 1 to Au in cells3+See fig. 6: in the figure, a1-e1Is a photograph of PC12 cells in bright field; a is2-e2Adding Au with different concentrations3+Fluorescence photograph of PC12 cells after (0-400. mu.M); a is3-e3Combining the imaging photos; f is Au of different concentrations3+The fluorescence intensity of the cells in the presence of the fluorescent dye. It can be seen that the hydrophilic carbon dots can be used for visual detection of Au in cells3+。
(7) The hydrophilic carbon dots obtained in example 1 can be used with a polyvinyl alcohol composite coating on an ultraviolet light emitting diode to manufacture a white Light Emitting Diode (LED) as shown in FIG. 7: the light-emitting diode prepared by the hydrophilic carbon dots can emit white light, and the color coordinates of the international commission on illumination are (0.29, 0.33), and the coordinates are displayed in a white light area.
Comparative example 1
The method for preparing the hydrophilic and hydrophobic carbon dots comprises the following steps:
(1) dissolving 32 mg of methylene blue and 0.1mL of sulfuric acid (standard concentrated sulfuric acid is selected) in 10mL of ethanol, and stirring to form a uniform mixed solution;
(2) transferring the mixed solution into a 25mL polytetrafluoroethylene high-pressure reaction kettle, heating for 6h at 200 ℃, and cooling to room temperature to obtain black lower-layer solution which is hydrophilic carbon dots and red hydrophobic carbon dots of upper-layer liquid;
(3) the upper and lower solutions were filtered through 0.22 μ M filters to obtain pure hydrophilic and hydrophobic carbon spots.
And detecting different metal ions by taking the hydrophilic carbon dots as fluorescent probes.
The hydrophilic carbon dots are used as fluorescent probes for Au in cells3+And (6) detecting.
Respectively dissolving the hydrophilic and hydrophobic carbon dots in distilled water and ethanol, and irradiating with 365nm ultraviolet light.
Comparative example 2
The preparation method of the hydrophilic and hydrophobic carbon dots comprises the following steps:
(1) dissolving 24 mg of methylene blue and 0.1mL of sulfuric acid (standard concentrated sulfuric acid is selected) in 10mL of ethanol, and stirring to form a uniform mixed solution; a
(2) Transferring the mixed solution into a 25mL polytetrafluoroethylene high-pressure reaction kettle, heating for 6h at 200 ℃, and cooling to room temperature to obtain black lower-layer solution which is hydrophilic carbon dots and red hydrophobic carbon dots of upper-layer liquid;
(3) the upper and lower solutions were filtered through 0.22 μ M filters to obtain pure hydrophilic and hydrophobic carbon spots.
And detecting different metal ions by taking the hydrophilic carbon dots as fluorescent probes.
The hydrophilic carbon dots are used as fluorescent probes for Au in cells3+And (6) detecting.
Respectively dissolving the hydrophilic and hydrophobic carbon dots in distilled water and ethanol, and irradiating with 365nm ultraviolet light.
Comparative example 3
The method for preparing the hydrophilic and hydrophobic carbon dots comprises the following steps:
(1) dissolving 16 mg of methylene blue and 0.1mL of sulfuric acid (standard concentrated sulfuric acid is selected) in 10mL of ethanol, and stirring to form a uniform mixed solution;
(2) transferring the mixed solution into a 25mL polytetrafluoroethylene high-pressure reaction kettle, heating for 6h at 200 ℃, and cooling to room temperature to obtain black lower-layer solution which is hydrophilic carbon dots and red hydrophobic carbon dots of upper-layer liquid;
(3) the upper and lower solutions were filtered through 0.22 μ M filters to obtain pure hydrophilic and hydrophobic carbon spots.
And detecting different metal ions by taking the hydrophilic carbon dots as fluorescent probes.
The hydrophilic carbon dots are used as fluorescent probes for Au in cells3+And (6) detecting.
Respectively dissolving the hydrophilic and hydrophobic carbon dots in distilled water and ethanol, and irradiating with 365nm ultraviolet light.
Comparative example 4
The method for preparing the hydrophilic and hydrophobic carbon dots comprises the following steps:
(4) dissolving 0.1mL of sulfuric acid (standard concentrated sulfuric acid) in 10mL of ethanol, and stirring to form a uniform mixed solution;
(5) transferring the mixed solution into a 25mL polytetrafluoroethylene high-pressure reaction kettle, heating for 6h at 200 ℃, and cooling to room temperature to obtain black lower-layer solution which is hydrophilic carbon dots and red hydrophobic carbon dots of upper-layer liquid;
(6) the upper and lower solutions were filtered through 0.22 μ M filters to obtain pure hydrophilic and hydrophobic carbon spots.
And detecting different metal ions by taking the hydrophilic carbon dots as fluorescent probes.
The hydrophilic carbon dots are used as fluorescent probes for Au in cells3+And (6) detecting.
Respectively dissolving the hydrophilic and hydrophobic carbon dots in distilled water and ethanol, and irradiating with 365nm ultraviolet light.
The probes prepared by the hydrophilic carbon dots synthesized by the preparation methods of the embodiment 1 and the comparative examples 1 to 4 can be used as fluorescent probes for sensitively and selectively detecting gold ions, can realize visual detection and analysis on the gold ions in cells, and has the functions of tracking and analyzing tissues and Au in organisms3+The potential application value of the method solves the problem that visual detection and analysis can not be realized when the hydrophilic carbon points are used for detecting gold ions in tissues and cells in the prior art.
Example 1 and comparative examples were observed simultaneouslyThe color of the fluorescent photograph of the hydrophilic carbon dots in examples 1 to 4 under 365nm ultraviolet irradiation was compared as shown in Table 1
Example 1 Comparative example 1 Comparative example 2 Comparative example 3 Comparative example 4
Colour of fluorescence Bright white color Orange colour Orange colour Orange colour Light orange
TABLE 1 color of fluorescent photographs under 365nm UV irradiation
As shown in Table 1, different hydrophilic carbon spots were synthesized from 0.1mL of sulfuric acid with and without addition of methylene blue in amounts of 8mg, 32 mg, 24 mg, and 16 mg, respectively, to the starting materials. Under 365nm ultraviolet light irradiation, the strongest fluorescence emission peak of the synthesized hydrophilic carbon dots gradually shifts in red along with the increase of the amount of methylene blue, so that orange fluorescence is emitted, when the methylene blue is not added in the raw materials, only weak light orange can be displayed, and only when the methylene blue is 8mg, bright white fluorescence can be emitted, and at the moment, the hydrophilic carbon dots emitted by white light can be used for preparing a diode emitting white light.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical scope of the present invention by equivalent replacement or change according to the technical solution and the inventive concept of the present invention within the technical scope of the present invention.

Claims (6)

1. A method for simultaneously synthesizing hydrophilic and hydrophobic carbon dots is characterized by comprising the following steps:
(1) dissolving 0.1mL of concentrated sulfuric acid and methylene blue in 10mL of ethanol, and stirring for 1-2 min to form a uniform mixed solution;
(2) and (2) transferring the mixed solution in the step (1) into a 25mL polytetrafluoroethylene high-pressure reaction kettle, heating at 200 ℃ for 6h, cooling to room temperature to obtain black hydrophilic carbon dots as a lower layer solution and hydrophobic carbon dots as a red upper layer solution, and filtering the lower layer solution and the upper layer solution by using 0.22 mu M filter membranes respectively to obtain pure hydrophilic and hydrophobic carbon dots.
2. The method for simultaneously synthesizing hydrophilic and hydrophobic carbon dots according to claim 1, wherein the amount of methylene blue used in the step (1) is 8 mg.
3. The use of the synthesized hydrophilic carbon dots according to claim 2 for the preparation of white light emitting diodes, wherein the hydrophilic carbon dots are dissolved in distilled water, and the hydrophilic carbon dots show bright white fluorescence under 365nm ultraviolet light irradiation, and the white light emitting hydrophilic carbon dots can be combined with a polyvinyl alcohol composite coating to prepare white light emitting diodes on the ultraviolet light emitting diodes.
4. Use of the hydrophilic carbon dot according to claim 1 or 2, wherein the hydrophilic carbon dot is used as a fluorescent probe for detecting Au3+。
5. Use of hydrophilic carbon dots according to claim 4 for Au in water bodies3+And (6) detecting.
6. Use of hydrophilic carbon dots according to claim 4 for visualization of Au in cells3+And (6) detecting.
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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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