CN110980690A - Method for preparing narrow-band red fluorescent carbon quantum dots by using titanyl phthalocyanine - Google Patents
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Abstract
The invention discloses a method for preparing narrow-band red fluorescent carbon quantum dots by using titanyl phthalocyanine, in particular to red light carbon quantum dots with narrow half-height width of a fluorescent emission peak, belonging to the technical field of nano material preparation. A method for preparing narrow-band red fluorescent carbon quantum dots by using titanyl phthalocyanine comprises the following steps: (1) mixing titanyl phthalocyanine with a solvent, putting the mixture into a reaction kettle, putting the reaction kettle into an oven, and keeping the temperature of the reaction kettle at 175-225 ℃ for more than 4 hours to obtain a reaction product; (2) and (2) naturally cooling the reaction product in the step (1) to room temperature to obtain the red light carbon quantum dots. The preparation process is simple and controllable, and the synthesized red light carbon quantum dots have narrow full width at half maximum of fluorescence peak and high fluorescence quantum yield, and can be widely applied to the fields of display devices, cell markers, biological imaging and the like.
Description
Technical Field
The invention provides a method for preparing narrow-band red fluorescent carbon quantum dots by using titanyl phthalocyanine, in particular to red light carbon quantum dots with narrow half-height width of a fluorescence emission peak, belonging to the field of nano material preparation.
Background
Since the emergence of Carbon Quantum Dots (CQDs) in 2006, the Carbon Quantum Dots (CQDs) are concerned by the scientific and industrial fields and rapidly develop into a novel high-quality fluorescent nano material. The carbon quantum dots have unique photoelectric properties of stronger steady-state fluorescence, longer thermal electron service life, extremely fast electron extraction speed, adjustable band gap width and the like, have superior characteristics of solution-soluble processing, low cost, low toxicity, good biocompatibility and the like, and are suitable for various fields of luminescent devices, luminescent films, high-efficiency Solar Cells (SCs), LED illumination and display devices, lithium ion batteries, supercapacitors, photocatalysis, biological probes, biological imaging and the like.
At present, most of carbon quantum dots prepared by the prior art emit blue-green fluorescence, generally have wide emission characteristics, fewer carbon quantum dots emit red fluorescence, and fewer carbon quantum dots with narrow half-height width of fluorescence emission peak (<30 nm). This greatly limits the application of CQDs to displays and lasers. Although one can prepare red carbon quantum dots by controlling the size of the nucleation of the carbon quantum dots, the surface state and edge state of the carbon quantum dots, or introducing a red luminescent group, the preparation of red carbon quantum dots has been challenging so far. Therefore, the design and preparation of the CQDs with high color purity and fluorescence half-peak width less than 30nm are particularly important for the application of the CQDs in the display field.
Hu et al prepared red luminescent carbon dots through complicated steps, but the QY of red luminescent carbon quantum dots was only 6%. Qu et al reported an orange carbon dot synthesized by a solvothermal method, in which citric acid and urea were used as reaction precursors, DMF was used as a solvent, and modified by NaOH, and its QY was as high as 46%, but its emission peak of the carbon quantum dot was at 580nm, which was orange. Yuan and the like use phloroglucinol as a reaction precursor, sulfuric acid as a catalyst and ethanol as a solvent to synthesize triangular red emission CQDs with the emission peak half-height width of 30nm by a thermal solvent method. However, most preparation processes require the addition of a strong oxidant, the reaction conditions are harsh, or the reaction process is complicated, and it is difficult to obtain red carbon quantum dots with narrow full width at half maximum and large stokes shift. Therefore, the application range of the red light carbon quantum dots in the fields of display devices, cell marking, photodynamic therapy, biological imaging and the like is greatly limited, and therefore, the research and development of the red light carbon quantum dots which are simple and controllable in preparation process, narrow in half-peak width and high in fluorescence quantum yield are urgently needed.
Disclosure of Invention
The invention aims to provide a method for preparing narrow-band red fluorescent carbon quantum dots by using titanyl phthalocyanine; the method has simple process and high efficiency, and can prepare the red light carbon quantum dots with half-height width and excellent fluorescence quantum yield.
The invention discloses a method for preparing narrow-band red fluorescent carbon quantum dots by using titanyl phthalocyanine, which comprises the following steps:
(1) mixing titanyl phthalocyanine with a solvent, putting the mixture into a reaction kettle, putting the reaction kettle into an oven, and keeping the temperature of the reaction kettle at 175-225 ℃ for more than 4 hours to obtain a reaction product;
(2) and (2) naturally cooling the reaction product in the step (1) to room temperature to obtain the narrow-band red fluorescent carbon quantum dot.
Further, the time for ultrasonically mixing the raw materials in the step (1) is 30 min;
further, in the step (1) of the present invention, the oven temperature is set to 180 ℃.
Further, in the step (1) of the present invention, the oven temperature is set to 200 ℃.
Further, in the step (1) of the present invention, the oven temperature is set to 220 ℃.
Furthermore, in the step (1), the heat preservation time is not more than 15 h.
Further, in the step (1), the heat preservation time is 6-12 h.
Further, in the step (1) of the invention, the inner lining of the reaction kettle is made of polytetrafluoroethylene.
Further, the step (2) of the invention is that the reaction product in the step (1) is naturally cooled to room temperature, then filtered by a filter membrane of 220nm, finally eluted by an eluant, and purified by a silica gel chromatographic column to obtain the red light carbon quantum dots.
The solvent is selected from ethanol, N-dimethylformamide and dimethyl sulfoxide; the eluent is ethanol.
The mixing ratio of the oxytitanium phthalocyanine and the solvent in the step (1) of the present invention is mg: ml to 2: 3.
The invention has the beneficial effects that: the invention adopts a one-step solvothermal method to take titanyl phthalocyanine (TiOPc) as a reaction precursor and ethanol as an organic solvent, can prepare the red-light carbon quantum dot with an emission peak at 674nm, a narrow half-height width (23.2nm) of a fluorescence emission peak and a fluorescence Quantum Yield (QY) of 7.54 percent, has simple process, high yield and good repeatability, has larger Stokes shift of the prepared red-light carbon quantum dot, and can be widely applied to the fields of display devices, cell marking, biological imaging and the like.
Drawings
FIG. 1(a) is a TEM image of a narrow-band red fluorescent carbon quantum dot of an embodiment of the present invention, and the inset is a high resolution TEM (HR-TEM) image of R-CQD;
FIG. 1(b) is a diagram illustrating a distribution of the particle size of a narrow-band red fluorescent carbon quantum dot according to an embodiment of the present invention;
FIG. 1(c) is an X-ray diffraction (XRD) pattern of a narrow-band red fluorescent carbon quantum dot in accordance with one embodiment of the present invention;
FIG. 2(a) is an XPS survey of a narrow-band red fluorescent carbon quantum dot according to an embodiment of the present invention;
FIG. 2(b) is a C1s spectrum of a narrow-band red fluorescent carbon quantum dot according to an embodiment of the present invention;
FIG. 2(c) is a spectrum of N1s of a narrow-band red fluorescent carbon quantum dot according to an embodiment of the present invention;
FIG. 2(d) is a diagram of the O1s spectrum of a narrow-band red fluorescent carbon quantum dot according to an embodiment of the present invention;
FIG. 2(e) is a Ti2p spectrum of a narrow-band red fluorescent carbon quantum dot according to an embodiment of the present invention;
FIG. 2(f) is a FT-IR spectrum of a narrow-band red fluorescent carbon quantum dot in accordance with an embodiment of the present invention;
FIG. 3(a) is an absorption spectrum of a narrow-band red fluorescent carbon quantum dot according to an embodiment of the present invention;
FIG. 3(b) is the absorption spectrum, the excitation spectrum and the fluorescence spectrum of a narrow-band red fluorescent carbon quantum dot in accordance with an embodiment of the present invention;
fig. 3(c) shows the fluorescence spectrum of a narrow-band red fluorescent carbon quantum dot according to an embodiment of the present invention: the inset is a photograph of the narrow-band red fluorescent carbon quantum dots under natural light (left) and ultraviolet light irradiation (right);
FIG. 3(d) is a graph showing the fluorescence lifetime of a narrow-band red fluorescent carbon quantum dot under 380nm laser irradiation in accordance with one embodiment of the present invention;
FIG. 4 is a fluorescence emission spectrum of a narrow-band red fluorescent carbon quantum dot according to a second embodiment of the present invention;
FIG. 5 is a fluorescence emission spectrum of three narrow-band red fluorescent carbon quantum dots according to the example of the present invention;
FIG. 6 is a fluorescence emission spectrum of four narrow-band red fluorescent carbon quantum dots according to an embodiment of the present invention.
Detailed Description
The invention is described in further detail below with reference to the figures and the examples, but the scope of the invention is not limited to the description. The following is only an example of a partial test, and is to illustrate the authenticity, the test operability and the technical method of the technical solution of the present invention, and not to limit the protection scope of the present invention.
Example 1
30mg of titanyl phthalocyanine and 60ml of ethanol were placed in a 250ml beaker and ultrasonically dispersed at a frequency of 53KHz for 30 min. And putting the mixed solution after ultrasonic treatment into a 100ml polytetrafluoroethylene lining, screwing the reaction kettle, putting the reaction kettle into an oven, and preserving heat for 6 hours at 180 ℃ to obtain a reaction product.
And naturally cooling the reaction product to room temperature, filtering the reaction product by a filter membrane of 220nm, and finally eluting the silica gel chromatographic column by using ethanol as an eluent to obtain the purified narrow-band red fluorescent carbon quantum dots.
The surface topography of the narrow-band red fluorescent carbon quantum dot in the embodiment is shown in fig. 1(a), the TEM image of the lattice fringes is shown in the inset of fig. 1(a), the particle size distribution diagram measured by TEM is shown in fig. 1(b) and the corresponding X-ray diffraction (XRD) diagram is shown in fig. 1 (c). As can be seen from FIG. 1(a), the narrow-band red fluorescent carbon quantum dot has good dispersibility and crystallinity, the crystal lattice fringes are clear, the spacing between crystal planes is 0.22nm, and the crystal planes correspond to the (100) plane of graphite; the size distribution of the narrow-band red fluorescent carbon quantum dots is 2.1-4.9 nm, and the average particle size is 3.9 nm; the narrow-band red fluorescent carbon quantum dots have a distinct diffraction peak at approximately 25.14 ° due to the (002) plane of graphite.
The X-ray photoelectron spectroscopy (XPS) and fourier transform infrared (FT-IR) spectra of the narrow-band red fluorescent carbon quantum dots of this example are shown in fig. 2(a) - (f). The X-ray photoelectron spectroscopy (XPS) full spectrum of the narrow-band red fluorescent carbon quantum dot shows four peaks at 284.85, 399.20, 531.75 and 457.98eV, corresponding to C1s, N1s, O1s and Ti2p, and the atomic ratios thereof are 86.89%, 3.39%, 9.62% and 0.1%, respectively; the high resolution XPS spectrum of C1s was divided into three peaks at 284.90, 286.18 and 288.18eV, corresponding to C-C/C ═ C, C-O/C-N and C ═ O/C ═ N, respectively; n1s showed three peaks at 398.18, 398.98 and 399.88eV, corresponding to pyrrole N, pyridine N and graphite N, respectively; o1s shows three peaks at 530.48, 531.79 and 532.88eV, corresponding to Ti-O, C ═ O and C-O, respectively; ti2P is Ti2P at 458.08eV3/2Peak and Ti2P at 463.48eV1/2Separation between peaks; fourier transform infrared (FT-IR) spectrum of narrow-band red fluorescent carbon quantum dots shows that stretching vibration of N-H, C-H and C/C-N are respectively positioned at 3344cm -12974 and 2901cm-1And 1655cm-1At least one of (1) and (b); the stretching vibration of lactone structures of C ═ O and C-O-C are respectively positioned at 1250cm-1And 1051cm-1(ii) a C-N at 1394cm-1The vibration of (a) contributes to the amide group; the out-of-plane curvature of the aromatic C-H falls within 881cm-1And 646cm-1(ii) a At 433cm-1There is a weak absorption peak near, corresponding to Ti-O tensile vibration.
The optical properties of the narrow-band red fluorescent carbon quantum dots prepared in this example are shown in fig. 3(a) - (d). The UV-Vis absorption spectrum of the narrow-band red fluorescent carbon quantum dots shows five distinct absorption peaks at about 221, 282, 338, 603 and 667 nm. Strong absorption peaks at 221 and 282nm are due to the pi → pi transition of the aromatic C ═ C bond, weaker absorption peaks at 338, 603, and 667nm are due to the N → pi transition with the aromatic system C ═ O or C-N/C ═ N structure; at the excitation wavelength of 300-420nm, the emission spectrum of the narrow-band red fluorescent carbon quantum dot shows excellent characteristics independent of the excitation wavelength. Under the excitation of the optimal excitation wavelength of 340nm, the strongest emission peak of the narrow-band red fluorescent carbon quantum dot is positioned at 674nm, the fluorescence quantum yield is 7.54%, the half-peak width is 23.2nm, and the peak has larger Stokes shift; the fluorescence spectrum of the time resolution shows that the fluorescence lifetime of the narrow-band red fluorescent carbon quantum dots is 3.9ns, and the fluorescence attenuation curve meets the single exponential attenuation curve.
Example 2
30mg of titanyl phthalocyanine and 60ml of ethanol were placed in a 250ml beaker and ultrasonically dispersed at a frequency of 53KHz for 30 min. And putting the mixed solution after ultrasonic treatment into a 100ml polytetrafluoroethylene lining, screwing the reaction kettle, putting the reaction kettle into an oven, and preserving heat for 12 hours at 180 ℃ to obtain a reaction product.
And naturally cooling the reaction product to room temperature, filtering the reaction product by a filter membrane of 220nm, and finally eluting the silica gel chromatographic column by using ethanol as an eluent to obtain the purified narrow-band red fluorescent carbon quantum dots.
As shown in fig. 4, the emission spectrum of the narrow-band red fluorescent carbon quantum dot prepared in this example shows excellent characteristics independent of the excitation wavelength at the excitation wavelength of 300-640nm, and the emission peaks of the narrow-band red fluorescent carbon quantum dot are at 672nm and 739 nm.
Example 3
30mg of titanyl phthalocyanine and 60ml of N, N-dimethylformamide are placed in a 250ml beaker and ultrasonically dispersed for 30min at a frequency of 53 KHz. And putting the mixed solution after ultrasonic treatment into a 100ml polytetrafluoroethylene lining, screwing the reaction kettle, putting the reaction kettle into an oven, and preserving heat for 6 hours at 180 ℃ to obtain a reaction product.
And naturally cooling the reaction product to room temperature, filtering the reaction product by using a filter membrane of 220nm, and finally eluting the silica gel chromatographic column by using ethanol as an eluent to obtain the purified narrow-band red fluorescent carbon quantum dots.
The emission spectrum of the narrow-band red fluorescent carbon quantum dot in the embodiment is shown in fig. 5, and under the excitation wavelength of 300-640nm, the emission spectrum of the narrow-band red fluorescent carbon quantum dot shows excellent characteristics independent of the excitation wavelength, and the emission peaks of the narrow-band red fluorescent carbon quantum dot are at 675nm and 743 nm.
Example 4
30mg of titanyl phthalocyanine and 60ml of dimethyl sulfoxide were placed in a 250ml beaker and ultrasonically dispersed at a frequency of 53KHz for 30 min. And putting the mixed solution after the ultrasonic treatment into 100ml of polytetrafluoroethylene lining, screwing the reaction kettle, putting the reaction kettle into an oven, and keeping the temperature at 180 ℃ for 6 hours to obtain a reaction product.
And naturally cooling the reaction product to room temperature, filtering the reaction product by a filter membrane of 220nm, and finally eluting the silica gel chromatographic column by using ethanol as an eluent to obtain the purified narrow-band red fluorescent carbon quantum dots.
The emission spectrum of the narrow-band red fluorescent carbon quantum dot in the embodiment is shown in fig. 6, and under the excitation wavelength of 300-660nm, the emission spectrum of the narrow-band red fluorescent carbon quantum dot shows excellent characteristics independent of the excitation wavelength, and the emission peaks of the narrow-band red fluorescent carbon quantum dot are at 700nm and 765 nm.
Example 5
30mg of titanyl phthalocyanine and 60ml of ethanol were placed in a 250ml beaker and ultrasonically dispersed at a frequency of 53KHz for 30 min. And putting the mixed solution after the ultrasonic treatment into 100ml of polytetrafluoroethylene lining, screwing the reaction kettle, putting the reaction kettle into an oven, and keeping the temperature at 175 ℃ for 8 hours to obtain a reaction product.
And naturally cooling the reaction product to room temperature, filtering the reaction product by a filter membrane of 220nm, and finally eluting the silica gel chromatographic column by using ethanol as an eluent to obtain the purified narrow-band red fluorescent carbon quantum dots.
Example 6
30mg of titanyl phthalocyanine and 60ml of N, N-dimethylformamide are placed in a 250ml beaker and ultrasonically dispersed for 30min at a frequency of 53 KHz. And putting the mixed solution after the ultrasonic treatment into 100ml of polytetrafluoroethylene lining, screwing the reaction kettle, putting the reaction kettle into an oven, and preserving the heat for 7 hours at 225 ℃ to obtain a reaction product.
And naturally cooling the reaction product to room temperature, filtering the reaction product by a filter membrane of 220nm, and finally eluting the silica gel chromatographic column by using ethanol as an eluent to obtain the purified narrow-band red fluorescent carbon quantum dots.
Example 7
30mg of titanyl phthalocyanine and 60ml of dimethyl sulfoxide were placed in a 250ml beaker and ultrasonically dispersed at a frequency of 53KHz for 30 min. And putting the mixed solution after the ultrasonic treatment into 100ml of polytetrafluoroethylene lining, screwing the reaction kettle, putting the reaction kettle into an oven, and keeping the temperature for 9 hours at the temperature of 200 ℃ to obtain a reaction product.
And naturally cooling the reaction product to room temperature, filtering the reaction product by a filter membrane of 220nm, and finally eluting the silica gel chromatographic column by using ethanol as an eluent to obtain the purified narrow-band red fluorescent carbon quantum dots.
Example 8
30mg of titanyl phthalocyanine and 60ml of N, N-dimethylformamide are placed in a 250ml beaker and ultrasonically dispersed for 30min at a frequency of 53 KHz. And putting the mixed solution after the ultrasonic treatment into 100ml of polytetrafluoroethylene lining, screwing the reaction kettle, putting the reaction kettle into an oven, and preserving the heat for 10 hours at the temperature of 220 ℃ to obtain a reaction product.
And naturally cooling the reaction product to room temperature, filtering the reaction product by a filter membrane of 220nm, and finally eluting the silica gel chromatographic column by using ethanol as an eluent to obtain the purified narrow-band red fluorescent carbon quantum dots.
Table 1 shows a comparison table of parameters of the preparation process of the narrow-band red fluorescent carbon quantum dots in examples 1 to 4
The above description is only a part of specific embodiments of the present invention, and the present invention belongs to the numerical range, so the embodiments cannot be exhaustive, and the protection scope of the present invention is subject to the numerical range of the present invention and other technical essential ranges. Specific matters or common sense known in the art are not described in detail herein. It should be noted that the above-mentioned embodiments do not limit the present invention in any way, and all technical solutions obtained by means of equivalent substitution or equivalent transformation for those skilled in the art are within the protection scope of the present invention. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (10)
1. A method for preparing narrow-band red fluorescent carbon quantum dots by using oxytitanium phthalocyanine is characterized by comprising the following steps:
(1) mixing titanyl phthalocyanine with a solvent, putting the mixture into a reaction kettle, putting the reaction kettle into an oven, and keeping the temperature of the reaction kettle at 175-225 ℃ for more than 4 hours to obtain a reaction product;
(2) and (2) naturally cooling the reaction product in the step (1) to room temperature to obtain the red light carbon quantum dots.
2. The method for preparing red-light carbon quantum dots by using oxytitanium phthalocyanine according to claim 1, wherein in the step (1), the oven temperature is set to 180 ℃.
3. The method for preparing narrow-band red fluorescent carbon quantum dots by using oxytitanium phthalocyanine according to claim 1, wherein in the step (1), the oven temperature is set to 200 ℃.
4. The method for preparing narrow-band red fluorescent carbon quantum dots by using oxytitanium phthalocyanine according to claim 1, wherein in the step (1), the oven temperature is set to 220 ℃.
5. The method for preparing narrow-band red fluorescent carbon quantum dots by using oxytitanium phthalocyanine according to claim 1, wherein in the step (1), the incubation time is not more than 15 h.
6. The method for preparing the narrow-band red fluorescent carbon quantum dot by using the oxytitanium phthalocyanine according to claim 1, wherein in the step (1), the heat preservation time is 6-12 h.
7. The method for preparing narrow-band red fluorescent carbon quantum dots by using oxytitanium phthalocyanine according to claim 1, wherein in the step (1), the inner lining of the reaction kettle is made of polytetrafluoroethylene.
8. The method for preparing narrow-band red fluorescent carbon quantum dots by using oxytitanium phthalocyanine according to claim 1, wherein the step (2) of the method is that the reaction product obtained in the step (1) is naturally cooled to room temperature, then is filtered by a filter membrane with a pore diameter of 220nm, is finally eluted by an eluent, and is purified by a silica gel chromatographic column to obtain the narrow-band red fluorescent carbon quantum dots.
9. The method for preparing narrow-band red fluorescent carbon quantum dots by using oxytitanium phthalocyanine according to claim 8, wherein the solvent in the step (1) is selected from ethanol, N-dimethylformamide and dimethyl sulfoxide; the eluent is ethanol.
10. The method for preparing a narrow-band red fluorescent carbon quantum dot using oxytitanium phthalocyanine according to claim 1 or 9, wherein the mixing ratio of the oxytitanium phthalocyanine and the solvent in step (1) is mg: ml to 1: 2.
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| CN112516333A (en) * | 2020-12-08 | 2021-03-19 | 四川大学 | Red light carbon dot and nucleic acid compound/nano compound thereof, preparation and application |
| CN112552306A (en) * | 2020-12-30 | 2021-03-26 | 四川轻化工大学 | Metal phthalocyanine loaded fluorescent carbon quantum dot and preparation method and application thereof |
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| CN112552306B (en) * | 2020-12-30 | 2022-03-08 | 四川轻化工大学 | Metal phthalocyanine loaded fluorescent carbon quantum dot and preparation method and application thereof |
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