CN112209635A - Solid fluorescent carbon dot based on nano porous glass and preparation method thereof - Google Patents
Solid fluorescent carbon dot based on nano porous glass and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of fluorescent carbon nano materials, and particularly discloses a solid fluorescent carbon dot based on nano porous glass and a preparation method thereof, wherein the solid fluorescent carbon dot comprises the following steps: preparing carbon dot powder into a carbon dot solution, soaking a nano porous glass sheet in the carbon dot solution to disperse and dope the carbon dots in the carbon dot solution into nano pores of the nano porous glass, simultaneously inhibiting the aggregation of the carbon dots by the nano pores, and naturally drying the nano porous glass doped with the carbon dots to obtain the solid fluorescent carbon dots based on the nano porous glass. According to the invention, the carbon dots are doped into the nano-porous glass, the method is simple, green and environment-friendly, the nano-porous glass can be prepared in batch, the good compatibility of the carbon dots and the glass is realized, and the prepared solid fluorescent carbon dots have stable luminescence and high fluorescence intensity.
Description
Technical Field
The invention belongs to the field of fluorescent carbon nano materials, and particularly relates to a solid fluorescent carbon dot based on nano porous glass and a preparation method thereof.
Background
The carbon dots are one-dimensional nano materials with fluorescence characteristics, have the advantages of unique optical performance, good water solubility, stable luminescence characteristics, easy synthesis, environmental protection and the like, and are greatly concerned in the fields of biomedicine, sensing detection, luminescence illumination and the like.
However, most of the carbon dots reported in the literature have good luminescence characteristics in a solution, and the solid carbon dots are subject to aggregation quenching effect, so that fluorescence quenching often occurs in a solid state due to pi electron accumulation or energy transfer between carbon cores. At present, although a preparation method of solid carbon dots exists, the preparation method is limited by the problems of complex preparation process, high preparation cost, low carbon dot loading capacity and the like, so that the application of the carbon dots in the fields of illumination and luminescence, energy sources, photoelectric devices and biological medical treatment is limited.
Disclosure of Invention
Aiming at the defects or improvement requirements of the prior art, the invention provides a solid fluorescent carbon dot based on nano-porous glass and a preparation method thereof, and aims to use the nano-porous glass as a matrix and dope the fluorescent carbon dot into the nano-porous glass, so that the prepared solid fluorescent carbon dot has stable luminescence and high fluorescence intensity, is simple to operate, is green and environment-friendly, can be prepared in batches, and realizes good compatibility of the carbon dot and the glass.
In order to achieve the above object, according to an aspect of the present invention, there is provided a method for preparing a solid-state fluorescent carbon dot based on nanoporous glass, comprising the steps of:
preparing carbon dot powder into a carbon dot solution, soaking a nano porous glass sheet in the carbon dot solution to disperse and dope the carbon dots in the carbon dot solution into nano pores of the nano porous glass, simultaneously inhibiting the aggregation of the carbon dots by the nano pores, and naturally drying the nano porous glass doped with the carbon dots to obtain the solid fluorescent carbon dots based on the nano porous glass.
More preferably, the nano-porous glass sheet is soaked in the carbon dot solution for 48 to 96 hours at normal temperature or 30 to 60 minutes at the temperature of 50 to 80 ℃.
More preferably, the nanoporous glass is immersed in the carbon dot solution and subjected to ultrasonic treatment for 20min to 60 min.
As a further preferred method, the nanoporous glass is prepared by the following method: the borosilicate component glass is subjected to phase separation treatment to separate a silicon phase and a boron phase in the borosilicate component glass, and then the borosilicate component glass is cleaned by adopting an acid solution to dissolve the boron phase in the acid solution, so that the glass with a nanometer pore channel, namely the nanometer porous glass, is obtained.
More preferably, the content of silicon dioxide in the nano-porous glass is not less than 96%, and the diameter of the nano-pore channel is 5nm to 30 nm.
More preferably, the concentration of carbon dots in the carbon dot solution is 0.01 mg/mL-1 mg/mL.
As a further preferred method, the carbon dot powder is prepared by the following method: heating and reacting the carbon source molecule precursor to obtain a reactant, cooling the reactant, and dialyzing the reactant to obtain dialysate; the dialysate was frozen and dried under vacuum to give a carbon dot powder.
Preferably, the carbon source molecule precursor reacts for 6-12 hours at a reaction temperature of 160-200 ℃ to obtain a reactant.
More preferably, the reactant is dialyzed by a dialysis bag, the dialysis time is 24-72 hours, and the size of the dialysis bag is 3500D-500D.
According to another aspect of the present invention, there is provided a solid-state fluorescent carbon dot based on nanoporous glass, which is prepared by the above preparation method.
Generally, compared with the prior art, the above technical solution conceived by the present invention mainly has the following technical advantages:
1. according to the invention, the carbon dots are doped into the nano-porous glass, a complex preparation process is not needed, the method is simple, green and environment-friendly, batch preparation can be realized, good compatibility of the carbon dots and the glass is realized, a good preparation method is provided for solid state luminescence, and the prepared solid fluorescent carbon dots have stable luminescence and high fluorescence intensity.
2. According to the invention, the nano-porous glass with abundant nano-pores is adopted to obtain solid carbon dots, the size of the nano-pores is uniform, and the solid carbon dots are dispersed in nano-pores of the nano-porous glass, so that the uniformly distributed solid carbon dots can be obtained; meanwhile, due to the isolation effect of the pore channel, the fluorescence quenching of the carbon dots caused by aggregation can be inhibited, and the enhancement of the carbon dot luminescence in a solid state is realized.
3. According to the invention, the pore size of the nano-porous glass can be adjusted according to the preparation method, so that the nano-porous glass with uniform pore size but adjustable size can be obtained, and carbon dots with different sizes can be doped into the nano-porous glass, thereby realizing the preparation of the solid fluorescent carbon dots.
4. The nano-porous glass with high silicon dioxide content has the characteristics of high light transmittance, high temperature resistance and the like, so that the prepared solid fluorescent carbon dots based on the nano-porous glass have good application prospects in the aspect of optical devices, and can be applied to the fields of solid illumination, ion detection and the like; meanwhile, the invention can realize that the carbon dots obtained by various preparation processes are doped into the nano-porous glass, and realize the preparation of the solid carbon dots in different light emitting areas.
5. The concentration of the carbon dot solution and the time for soaking the nano-porous glass sheet in the carbon dot solution are set, so that the carbon dots in the solution can be fully and uniformly distributed in the pore canal and the pore diameter of the nano-porous glass, uniform doping is realized, and the fluorescence intensity of the solid fluorescent carbon dots is improved; meanwhile, the carbon dots can be accelerated to enter the inside of the pore diameter of the nano porous glass by utilizing high temperature or ultrasonic waves.
6. According to the invention, the precursor of carbon source molecules and the reaction temperature are set, so that the precursor can be promoted to react quickly and sufficiently to obtain a reactant suitable for subsequent dialysis, the yield of the reactant is improved, and the size and the performance of carbon dot powder can be ensured by setting the size of a dialysis bag; in addition, the method adopts a one-step high-temperature method to synthesize the carbon dots in a green way, does not need multi-step heating, has rich carbon source selection and simple preparation process, and can be prepared in large batch.
Drawings
FIG. 1 is a flow chart of a preparation method of a solid-state fluorescent carbon dot based on nano-porous glass according to an embodiment of the present invention;
FIG. 2 is a scanning electron micrograph of nanoporous glass according to an embodiment of the invention;
FIG. 3 is an absorption spectrum of a nanoporous glass without carbon dots incorporated therein according to an embodiment of the invention;
FIG. 4 is a graph showing absorption spectra of carbon dot 1, carbon dot 2 and carbon dot 3 according to an example of the present invention;
FIG. 5 is a graph of solid state carbon dot 1 fluorescence spectra based on nanoporous glass in accordance with an embodiment of the invention;
FIG. 6 is a graph of solid state carbon dot 2 fluorescence spectra based on nanoporous glass in accordance with an embodiment of the invention;
FIG. 7 is a graph of solid state carbon dot 3 fluorescence spectra based on nanoporous glass in accordance with an embodiment of the invention;
FIG. 8 is a graph comparing the fluorescence intensity of solid carbon dots and carbon dot solutions based on nanoporous glass in accordance with an embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The preparation method of the solid-state fluorescent carbon dot based on the nano-porous glass, as shown in fig. 1, specifically comprises the following steps:
s1, uniformly stirring a carbon source molecule precursor in a certain proportion by adopting a one-step high-temperature method, then putting the precursor into a polytetrafluoroethylene hydrothermal kettle inner container, and reacting for 6-12 hours at the reaction temperature of 160-200 ℃ to obtain a reactant;
preferably, the carbon source molecular precursor is p-phenylenediamine and anhydrous aluminum chloride, and the molar ratio of the precursor is 50: 3-25: 6, more preferably 50: 3 or 35: 3 or 25: 6; or the carbon source molecule precursor is citric acid and urea, and the mass ratio of the citric acid to the urea is 1: 1-1: 3, more preferably 1: 2; or the carbon source molecule precursor is citric acid and o-phenylenediamine, and the mass ratio of the citric acid to the o-phenylenediamine is 1: 1-1: 8, more preferably 1: 6, so that the reaction is fully performed.
S2, cooling the reactant to room temperature, and then dialyzing, filtering and purifying the reactant by using a dialysis bag to obtain dialysate;
preferably, the dialysis time is 24-72 hours, and the size of the dialysis bag is 3500D-500D.
S3, freezing the dialyzate and drying the dialyzate in vacuum to obtain carbon dot powder.
S4, preparing carbon dot powder into a carbon dot solution;
preferably, the mass of the carbon dots is 0.1-2 mg, the solvent is absolute ethyl alcohol or deionized water, and the concentration of the carbon dots in the carbon dot solution is 0.01-1 mg/mL.
S5, doping the carbon dot solution into the nano-porous glass, and naturally drying in an ultra-clean room environment to obtain the solid fluorescent carbon dots based on the nano-porous glass;
preferably, the nano-porous glass sheets with different sizes are soaked in the carbon dot solution, the carbon dot solution can be placed in an ultrasonic system for 20-60 min, and the carbon dots are accelerated to enter the inside of the pore diameter of the nano-porous glass by utilizing ultrasonic waves; or putting the nano porous glass into an oven for heating at the high temperature of 50-80 ℃ for 30-60 min, and adding carbon points into the nano porous glass at the high temperature to enter the inside of the pore diameter of the nano porous glass; or naturally soaking at normal temperature for 48-96 h, preferably 72 h; and then placing the carbon dots in an ultra-clean room, and naturally drying for 1 day to ensure that the sample has no external pollution, thereby obtaining the solid-state fluorescent carbon dots based on the nano-porous glass.
Further, the nano-porous glass is prepared by the following method: na with purity of 99.999%2CO3、H3BO3And SiO2The borosilicate component glass is prepared as a raw material, then phase separation is carried out to separate a silicon phase from a boron phase in the borosilicate component glass, and then the borosilicate component glass is cleaned by an acid solution to dissolve the boron phase in the acid solution to obtain the high-transmittance glass with the silicon dioxide content of 96 percent and nano-pores, namely the nano-porous glass, wherein the microstructure of the nano-porous glass consists of nano-pores, and the nano-porous glass can effectively inhibit carbonAnd (4) inducing quenching effect by point aggregation to obtain the fluorescent carbon point in a solid state. Specifically, the size of the nano porous glass is 1 cm-10 cm in length, 1 cm-10 cm in width and 1 mm-1 cm in height (diameter), and the nano porous glass can be cut into different three-dimensional cuboids, cubes or cylinders; in addition, the diameter of the nanometer pore canal of the nanometer porous glass is 5 nm-30 nm, and the diameter size of the pore canal can be adjusted according to the preparation method of the nanometer porous glass.
The nano-porous glass sheet (marked as nano-porous glass) in the invention is in a transparent 3D shape, the size is preferably 1cm by 1mm, the micro-morphology structure of the nano-porous glass sheet is provided with countless nano-pores, as shown in figure 2, the absorption spectrum of the nano-porous glass sheet is as shown in figure 3, the absorption peak at 217nm comes from the self absorption of the glass material, but after 300nm, the nano-porous glass sheet hardly absorbs the excitation light energy, so that the absorption of the carbon dots to the excitation light energy is greatly improved, and the fluorescence intensity of the solid carbon dots based on the nano-porous glass is improved.
The following are specific examples:
example 1
Weighing 1g of citric acid and 2g of urea, placing the citric acid and the urea in a beaker, uniformly grinding, adding 30mL of deionized water, uniformly stirring, placing the mixture in an inner container of a polytetrafluoroethylene reaction kettle, placing the reaction kettle in an oven, setting the reaction temperature to be 160 ℃, and setting the reaction time to be 6 hours; after the reaction is finished, putting the mixture into a 3500D dialysis bag, dialyzing for 36 hours, and further purifying the reactant; and collecting the liquid in the dialysis bag, and putting the liquid into a freeze dryer to obtain a powder sample.
Dissolving 0.0078g of powdered carbon dots in 10ml of deionized water, and performing ultrasonic treatment for 30 minutes to obtain a uniform carbon dot solution; taking 1 nano porous glass sheet, immersing the nano porous glass sheet into the carbon dot solution by adopting a liquid phase method for 72 hours; then, natural drying is carried out for 1 day in an ultra-clean room environment, and solid carbon dots based on the nano-porous glass sheet are obtained.
Example 2
Weighing 0.2g of citric acid and 1.2g of o-phenylenediamine in a beaker, uniformly grinding, putting into an inner container of a polytetrafluoroethylene reaction kettle, putting the reaction kettle into an oven, setting the reaction temperature to be 170 ℃ and the reaction time to be 10 hours; after the reaction is finished, putting the mixture into a 3000D dialysis bag, dialyzing for 48 hours, and further purifying the reactant; and collecting the liquid in the dialysis bag, and putting the liquid into a freeze dryer to obtain a powder sample.
0.018g of powdered carbon dots are dissolved in 20ml of deionized water, and ultrasonic treatment is carried out for 30 minutes to obtain a uniform carbon dot solution; taking 1 nano porous glass sheet, immersing the nano porous glass sheet into the carbon dot solution by adopting a liquid phase method for 72 hours; then, natural drying is carried out for 1 day in an ultra-clean room environment, and solid carbon dots based on the nano-porous glass sheet are obtained.
Example 3
Weighing 5mmol of p-phenylenediamine and 0.3mmol of anhydrous aluminum chloride, placing the materials into a beaker, uniformly grinding the materials, placing the beaker into an inner container of a polytetrafluoroethylene reaction kettle, placing the reaction kettle into a drying oven, setting the reaction temperature to be 180 ℃ and the reaction time to be 8 hours; after the reaction is finished, putting the mixture into a 500D dialysis bag, dialyzing for 24 hours, and further purifying the reactant; the liquid in the dialysis bag was collected and put into a freeze dryer to obtain a powder sample, labeled as carbon dot 1, whose absorption spectrum is shown in fig. 4.
0.00097g of powder carbon dots are dissolved in 20ml of ethanol, and ultrasonic treatment is carried out for 30 minutes to obtain a uniform carbon dot solution; taking 1 nano porous glass sheet, and immersing the nano porous glass sheet into the carbon dot solution by adopting a liquid phase method for 72 hours; and then, naturally drying for 1 day in an ultra-clean room environment to obtain solid carbon dots based on the nano-porous glass sheet, and marking the solid carbon dots as carbon dots 1@ nano-porous glass.
The fluorescence spectrum of the carbon dot 1@ nano-porous glass has a strong fluorescence peak at 598nm (as shown in figure 5), and the fluorescence intensity of the obtained carbon dot 1@ nano-porous glass is increased by 2.4 times compared with that of the carbon dot 1 under the same condition (as shown in a carbon dot 1 bar chart in figure 8).
Example 4
Weighing 5mmol of p-phenylenediamine and 0.6mmol of anhydrous aluminum chloride, placing the materials into a beaker, uniformly grinding the materials, placing the beaker into an inner container of a polytetrafluoroethylene reaction kettle, placing the reaction kettle into a drying oven, setting the reaction temperature to be 160 ℃, and setting the reaction time to be 12 hours; after the reaction is finished, putting the mixture into a 3000D dialysis bag, dialyzing for 24 hours, and further purifying the reactant; the liquid in the dialysis bag was collected and put into a freeze dryer to obtain a powder sample, labeled as carbon dot 2, whose absorption spectrum is shown in fig. 4.
Dissolving 0.0012g of powder carbon dots in 17ml of ethanol, and performing ultrasonic treatment for 30 minutes to obtain a uniform carbon dot solution; taking 1 nano porous glass sheet, immersing the nano porous glass sheet into the carbon dot solution by adopting a liquid phase method for 72 hours; and then, naturally drying for 1 day in an ultra-clean room environment to obtain solid carbon dots based on the nano-porous glass sheet, and marking the solid carbon dots as carbon dots 2@ nano-porous glass.
The fluorescence spectrum of the carbon dot 2@ nano-porous glass has a strong fluorescence peak at 595nm (as shown in figure 6), and compared with the carbon dot 2 under the same condition, the fluorescence intensity of the obtained carbon dot 2@ nano-porous glass is increased by 5.3 times (as shown in a carbon dot 2 bar chart in figure 8).
Example 5
Weighing 5mmol of p-phenylenediamine and 1.2mmol of anhydrous aluminum chloride, placing the materials into a beaker, uniformly grinding the materials, placing the beaker into an inner container of a polytetrafluoroethylene reaction kettle, placing the reaction kettle into a drying oven, setting the reaction temperature to be 200 ℃ and the reaction time to be 12 hours; after the reaction is finished, putting the mixture into a 3500D dialysis bag, dialyzing for 24 hours, and further purifying the reactant; the liquid in the dialysis bag was collected and put into a freeze dryer to obtain a powder sample, labeled as carbon dot 3, whose absorption spectrum is shown in fig. 4.
Dissolving 0.00124g of powder carbon dots in 10ml of deionized water, and carrying out ultrasonic treatment for 30 minutes to obtain a uniform carbon dot solution; taking 1 nano porous glass sheet, immersing the nano porous glass sheet into the carbon dot solution by adopting a liquid phase method for 72 hours; and then, naturally drying for 1 day in an ultra-clean room environment to obtain solid carbon dots based on the nano-porous glass sheet, and marking the solid carbon dots as carbon dots 3@ nano-porous glass.
The fluorescence spectrum of the carbon dot 3@ nano-porous glass has a strong fluorescence peak at 601nm (as shown in figure 7), and the obtained carbon dot 3@ nano-porous glass has the fluorescence intensity increased by 1.4 times compared with the carbon dot 3 under the same condition (as shown in a carbon dot 3 bar chart in figure 8).
Therefore, the solid carbon dots are obtained by adopting the nano-porous glass with rich nano-pores, so that the solid carbon dots are uniformly dispersed in the nano-pores of the nano-porous glass, the fluorescence quenching of the carbon dots caused by aggregation can be inhibited, and the luminescence enhancement of the carbon dots in the solid state is realized, as shown in fig. 8, the fluorescence intensity of the solid carbon dots prepared by adopting the method is far higher than that of the carbon dots in the liquid state.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A preparation method of a solid fluorescent carbon dot based on nano porous glass is characterized by comprising the following steps:
preparing carbon dot powder into a carbon dot solution, soaking a nano porous glass sheet in the carbon dot solution to disperse and dope the carbon dots in the carbon dot solution into nano pores of the nano porous glass, simultaneously inhibiting the aggregation of the carbon dots by the nano pores, and naturally drying the nano porous glass doped with the carbon dots to obtain the solid fluorescent carbon dots based on the nano porous glass.
2. The method for preparing solid-state fluorescent carbon dots based on nano-porous glass as claimed in claim 1, wherein the nano-porous glass sheet is soaked in the carbon dot solution for 48 to 96 hours at normal temperature or 30 to 60 minutes at 50 to 80 ℃.
3. The method for preparing a solid-state fluorescent carbon dot based on nano-porous glass according to claim 1, wherein the nano-porous glass is soaked in the carbon dot solution and subjected to ultrasonic treatment for 20min to 60 min.
4. The method for preparing a solid-state fluorescent carbon dot based on nano-porous glass according to claim 1, wherein the nano-porous glass is prepared by the following method: the borosilicate component glass is subjected to phase separation treatment to separate a silicon phase and a boron phase in the borosilicate component glass, and then the borosilicate component glass is cleaned by adopting an acid solution to dissolve the boron phase in the acid solution, so that the glass with a nanometer pore channel, namely the nanometer porous glass, is obtained.
5. The method for preparing the solid-state fluorescent carbon dot based on the nano-porous glass as claimed in claim 1, wherein the content of silica in the nano-porous glass is not less than 96%, and the diameter of the nano-pore channel is 5nm to 30 nm.
6. The method of claim 1, wherein the concentration of carbon dots in the carbon dot solution is between 0.01mg/mL and 1 mg/mL.
7. The method for preparing a solid fluorescent carbon dot based on nanoporous glass as defined in claim 1, wherein the carbon dot powder is prepared by the following method: heating and reacting the carbon source molecule precursor to obtain a reactant, cooling the reactant, and dialyzing the reactant to obtain dialysate; the dialysate was frozen and dried under vacuum to give a carbon dot powder.
8. The method for preparing the solid fluorescent carbon dots based on the nano-porous glass as claimed in claim 7, wherein the precursor of the carbon source molecule is reacted at the reaction temperature of 160-200 ℃ for 6-12 hours to obtain a reactant.
9. The preparation method of the solid-state fluorescent carbon dot based on the nano-porous glass as claimed in claim 7, wherein a dialysis bag is adopted to dialyze the reactant, the dialysis time is 24-72 hours, and the size of the dialysis bag is 3500D-500D.
10. A solid fluorescent carbon dot based on nanoporous glass, prepared by the method of any one of claims 1 to 9.
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| CN114525128A (en) * | 2022-01-22 | 2022-05-24 | 湖北第二师范学院 | Wavelength-adjustable solid carbon dot and preparation method thereof |
| CN114751397A (en) * | 2022-03-29 | 2022-07-15 | 华南师大(清远)科技创新研究院有限公司 | Fluorescent nano hydroxyapatite and preparation method and application thereof |
| CN116836701A (en) * | 2023-07-04 | 2023-10-03 | 广东药科大学 | Aluminum-doped carbon dot, preparation method, application and Hg removal method 2+ Is a method of (2) |
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