CN111100631A - Multicolor luminous solid silicon dot powder and multifunctional application of preparation method thereof - Google Patents
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Abstract
The invention belongs to the technical field of synthesis of fluorescent nano materials, and discloses multicolor luminous solid silicon dot powder, a preparation method and multifunctional application thereof. The emission peak position of the multicolor luminous solid silicon dot powder extends from blue light to orange red light, and the multicolor luminous solid silicon dot powder has good thermal stability and photobleaching resistance. The invention also discloses application of the multicolor luminous solid silicon dot powder in the fields of solid illumination and agricultural light conversion films. Compared with the prior art, the reaction raw materials are simple and easy to obtain, the reaction conditions are mild, and the reaction can be obtained only through one-step high-temperature annealing treatment. Due to the unique multicolor emission characteristic of the multicolor luminous solid silicon dot powder, a related multicolor light-emitting diode device and a light conversion film are obtained so as to explore the application prospect of the multicolor light-emitting diode device in the fields of solid illumination and agricultural light conversion films. The invention solves the problem that the existing photoelectronic device field and sensing field cannot be produced in scale due to the lack of a preparation process of multicolor solid luminescent silicon dots.
Description
Technical Field
The invention belongs to the technical field of synthesis of fluorescent nano materials, and particularly relates to multicolor luminous solid silicon dot powder, a preparation method and multifunctional application thereof.
Background
Compared with the traditional organic dye, the semiconductor quantum dot has the advantages of wide absorption wavelength range, narrow fluorescence spectrum, high fluorescence quantum efficiency, chemical bleaching resistance and the like. They have wide application prospects in the aspects of optoelectronic devices, sensing and biological imaging. However, the high toxicity of the quantum dots containing cadmium and lead limits the practical application of the quantum dots.
The silicon dots are spherical silicon-based nano materials with the volume less than 5nm, have the advantages of high abundance, no toxicity or low toxicity, high fluorescence quantum efficiency, good light stability and the like, and are expected to become substitutes of quantum dots containing cadmium and lead. These advantages have brought silicon dots to widespread attention and have stimulated their potential applications in the fields of optoelectronics, sensing, bio-imaging and light conversion.
However, the method and mechanism for producing the multicolor luminescent solid silicon dot powder are not clear. These disadvantages limit their widespread use because solid-state fluorescence colors from blue to red are necessary for optoelectronic devices and sensing applications.
At present, most of researches are focused on regulating the fluorescence color of a silicon dot solution, and the solid-state fluorescence of silicon dot powder is rarely reported. Although there is a report mentioning single blue solid state fluorescence of silicon dot powders, no mechanism is provided to explain why silicon dot powders are resistant to aggregation-induced self-quenching, let alone to build multi-color solid state luminescent silicon dot powders.
In class IV luminescent nanoparticles, solid-state fluorescence of carbon dots has been a focus of research. But carbon spots often appear as self-quenching fluorescence due to excessive energy resonance transfer and direct pi-pi interactions. In addition, carbon dot powders are generally difficult to obtain because of their hygroscopic nature. Compared with carbon dot powder, silicon dot powder has the characteristic of no deliquescence and is easy to obtain. However, obtaining a multi-color luminescent solid-state silicon dot powder remains a challenging task due to lack of sufficient experimental and theoretical knowledge.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention mainly aims to provide multicolor luminous solid silicon dot powder; the multicolor luminous solid silicon dot powder has good thermal stability and photobleaching resistance, and the fluorescence effect is obvious; it is expected to become a novel material in the fields of solid-state illumination and agricultural light conversion films.
The invention also aims to provide a preparation method of the multicolor luminous solid silicon dot powder; the preparation method is simple and rapid.
The invention also aims to provide multifunctional application of the multicolor luminous solid silicon dot powder, and solves the problem that the existing multicolor luminous solid silicon dot preparation process is lacked in the fields of solid illumination and agricultural light conversion films, so that large-scale production cannot be realized.
The purpose of the invention is realized by the following technical scheme:
a multicolor luminous solid silicon dot powder has an average particle size of 100nm, and emits blue light, green light, yellow light and orange red light under excitation of an excitation wavelength of 400nm, and has emission peak positions of 455nm, 534nm, 593nm and 613 nm.
The preparation method of the multicolor luminous solid silicon dot powder comprises the following operation steps:
(1) adding a silane coupling agent into an aqueous solution of a reducing agent under the condition of introducing nitrogen, fully mixing, reacting at the temperature of 150-220 ℃ for 6-16h, cooling the obtained mixed system to room temperature after the reaction is finished, and dialyzing to obtain a fluorescent silicon dot solution;
(2) freeze-drying the fluorescent silicon dot solution obtained in the step (1) to obtain solid silicon dot powder;
(3) and (3) annealing the solid silicon dot powder obtained in the step (2) at the high temperature of 100-400 ℃ for 10min, or annealing at the high temperature of 200 ℃ for 2-180min to obtain the multicolor luminous solid silicon dot powder.
The reducing agent in the step (1) is sodium citrate, citric acid, ascorbic acid, sodium ascorbate, folic acid, maleic acid, aminophenol or catechol.
The silane coupling agent in the step (1) is at least one of N- (β -aminoethyl-gamma-aminopropyl) trimethoxysilane (DAMO), N-aminoethyl-gamma-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane and methyltriethoxysilane.
In the step (1), the dosage ratio of the reducing agent to the silane coupling agent is 1-3 g: 5-10 mL.
The average particle size of the fluorescent silicon dot solution in the step (1) is 1.7nm, and the fluorescent silicon dot solution is yellow when observed by naked eyes under a fluorescent lamp and bright blue when irradiated by a 365nm ultraviolet lamp; excitation is carried out by 368nm excitation wavelength, the emission wavelength is 380-600nm, and larger fluorescence emission intensity is obtained at 445 nm; the fluorescence quantum yield was 66% with quinoline sulfate as a reference.
The average particle size of the solid silicon dot powder in the step (2) is 100 nm; the solid powder shows yellow when observed by naked eyes under a fluorescent lamp, and shows blue-yellow dual emission under the irradiation of a 365nm ultraviolet lamp; the blue and yellow emission peak positions are respectively at 439nm and 564nm, and the fluorescence quantum efficiency is respectively 26.35% and 10.91%.
The application of the multicolor luminous solid silicon point powder in the field of solid lighting.
The multicolor luminous solid silicon dot powder is blue light solid silicon dot powder, and is combined with carboxymethyl cellulose to form the miniature agricultural light conversion film.
The multicolor luminous solid silicon dot powder is blue light solid silicon dot powder, and the agricultural light conversion film is constructed by the multicolor luminous solid silicon dot powder and polyethylene, so that the growth and development of a cabbage heart are promoted.
According to the invention, a reducing agent and a silane coupling agent are utilized to synthesize the self-quenching-resistant fluorescent silicon dots in a solid state by one-step hydro-thermal synthesis; the solid silicon dot powder is utilized to synthesize a series of multi-color luminous solid silicon dot powder at high temperature, so that the thermal stability and the photobleaching resistance of the silicon dot powder are enhanced while the good optical performance of the silicon dot powder is kept; thereby promoting the application of the multi-color luminous solid silicon dot powder in the fields of solid illumination and agricultural light conversion films.
Compared with the prior art, the invention has the following advantages and effects:
(1) according to the invention, the solid-state self-quenching-resistant fluorescent silicon dot is synthesized by a simple hydrothermal method, and the solid-state silicon dot has blue-yellow dual-emission performance.
(2) The method has the advantages of simple and easily obtained reaction raw materials and mild reaction conditions, and a series of multi-color luminous solid silicon dot powder can be obtained only by one-step high-temperature annealing treatment; due to the unique multicolor emission characteristic of the multicolor luminous solid silicon dot powder, a related multicolor light-emitting diode device and a light conversion film are obtained so as to explore the application prospect of the multicolor light-emitting diode device and the light conversion film in the fields of solid illumination and agricultural light conversion films; the invention solves the problem that the existing photoelectronic device field and sensing field cannot be produced in scale due to the lack of a preparation process of multicolor solid luminescent silicon dots.
(3) The multicolor luminous solid silicon dot powder is successfully applied to the fields of solid illumination and agricultural light conversion films.
Drawings
FIG. 1 is a transmission electron microscope photograph of Si NPs-1 in example 1;
FIG. 2 is a graph showing an ultraviolet absorption spectrum and a fluorescence spectrum of Si NPs-1 in example 1;
FIG. 3 is a transmission electron microscope photograph of Si NPs-2 in example 1;
FIG. 4 is a fluorescence spectrum of Si NPs-2 in example 1;
FIG. 5 is a transmission electron microscope photograph and a particle size distribution chart of the multicolor luminescent solid silicon dot powder (B-SSF, G-SSF, Y-SSF, and O-SSF) in example 1; wherein (a), (B), (c) and (d) are B-SSF, G-SSF, Y-SSF and O-SSF scanning electron microscopy images and particle size distribution plots, respectively.
FIG. 6 is a fluorescence spectrum of multicolor luminescent solid-state silicon dot powder (B-SSF, G-SSF, Y-SSF, and O-SSF) in example 1;
FIG. 7 is a blue, green, yellow, and orange-red LED device of example 11; wherein (I) is a fluorescence image of a light emitting diode based on B-SSF (a), G-SSF (B), Y-SSF (c), and O-SSF (d), (II) is a CIE chromaticity coordinate based on B-SSF (a), G-SSF (B), Y-SSF (c), and O-SSF (d), (III) is a PL emission spectrum based on B-SSF (a), G-SSF (B), Y-SSF (c), and O-SSF (d).
FIG. 8 is a scanning electron microscope photograph of the B-SSF-based cellulose film and the pure cellulose film in example 12; wherein (a) and (B) are scanning electron micrographs of the pure cellulose film at different magnifications, and (c) and (d) are scanning electron micrographs of the B-SSF-based cellulose film at different magnifications.
FIG. 9 is a graph showing the light conversion properties of the B-SSF-based cellulose film of example 12.
Detailed description of the invention
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
The preparation of the multi-color luminous solid silicon dot powder comprises the following steps:
(1) introducing nitrogen into the sodium citrate aqueous solution with the mass fraction of 4.44% for 5min to remove oxygen in the solution;
(2) adding DAMO into the sodium citrate aqueous solution while stirring, and keeping introducing nitrogen for 20min to form a precursor solution; the dosage ratio of the sodium citrate to the DAMO is 1g to 6 mL;
(3) putting the precursor solution obtained in the step (2) into a reaction kettle, carrying out hydrothermal reaction at 200 ℃ for 12h, cooling the obtained mixed system to room temperature after the reaction is finished, carrying out dialysis to obtain a yellow silicon-point solution (Si NPs-1), and observing and testing the prepared Si NPs-1, wherein the result is shown in a figure 1 and a figure 2;
(4) freeze-drying the silicon dot solution obtained in the step (3) to form yellow solid powder (Si NPs-2), and observing and testing the prepared Si NPs-2, wherein the results are shown in a figure 3 and a figure 4;
(5) and (3) respectively annealing the yellow solid powder obtained in the step (4) at the high temperature of 200 ℃ for 2, 10, 120 and 180min to obtain a series of multi-color luminous solid silicon dot powder (blue light solid silicon dot powder B-SSF, green light solid silicon dot powder G-SSF, yellow light solid silicon dot powder Y-SSF and orange light solid silicon dot powder O-SSF). The prepared B-SSF, G-SSF, Y-SSF and O-SSF were observed and tested, and the results are shown in FIGS. 5 and 6.
Example 2
The preparation method is the same as that of example 1, except that in the step (5), the yellow solid powder obtained in the step (4) is respectively annealed at high temperature of 100, 200, 300 and 400 ℃ for 10min to obtain a series of multi-color light-emitting solid silicon dot powders (blue light solid silicon dot powder B-SSF, green light solid silicon dot powder G-SSF, yellow light solid silicon dot powder Y-SSF and orange light solid silicon dot powder O-SSF).
Example 3
The preparation method was the same as example 1, except that in step (2), 3-aminopropyl-triethoxysilane, 3-aminopropyl-trimethoxysilane and 3- [2- (2-aminoethylamino) ethylamino ] propyl-trimethoxysilane were used respectively instead of DAMO in example 1, to prepare three different fluorescent silicon dot solutions with amino groups.
Example 4
The preparation method is the same as example 1, except that in step (2), sodium ascorbate, ascorbic acid, citric acid or folic acid are respectively used to replace the sodium citrate in example 1, and four different fluorescent silicon dot solutions with amino groups are prepared.
Example 5
The preparation method was the same as in example 1, except that in step (2), the amount ratio of sodium citrate to the silane coupling agent DAMO was 1g:3 mL.
Example 6
The preparation method was the same as in example 1, except that in step (2), the amount ratio of sodium citrate to the silane coupling agent DAMO was 2g:3 mL.
Example 7
The preparation method was the same as in example 1, except that in step (3), the hydrothermal reaction time was 8 hours.
Example 8
The preparation method was the same as in example 1, except that in the step (3), the hydrothermal temperature was 150 ℃.
Example 9
The preparation method is the same as example 1, except that in the step (3), the microwave-assisted method is used instead of the hydrothermal method; the microwave reaction condition is 750W, 15 min.
Example 10
The preparation method was the same as in example 1, except that, in the step (5), the temperatures of the high-temperature annealing treatment were replaced with 100 ℃ and 300 ℃ respectively.
Example 11
The multicolor luminous solid silicon dot powder of example 1 was applied in the field of solid state lighting by the following method:
(1) a certain amount of epoxy resin and solid silicon dot powder are taken and uniformly stirred, 10 mu L of ethylenediamine (curing agent) is added, and finally the mixture is integrated on an LED chip.
(2) And drying in an oven at 50 ℃ for 3h to obtain the blue, green, yellow and orange-red LED devices, as shown in FIG. 7.
Example 12
The blue solid silicon dot powder (B-SSF) prepared in example 1 is applied to the field of light conversion films, and the method comprises the following steps:
(1) under the condition of 60 ℃ water bath, 0.8g of carboxymethyl cellulose is dissolved in 50mL of deionized water; uniformly stirring the cellulose solution and B-SSF (0.02, 0.04, 0.06, 0.08, 0.10 and 0.12g) with different masses to obtain a mixed solution; and finally, forming the B-SSF-based cellulose film at 40 ℃ for 4 h.
(2) Except that B-SSF powder is not added, a similar synthesis process is adopted to prepare the pure cellulose film. The obtained B-SSF-based cellulose film and pure cellulose film were subjected to observation and light conversion property tests, and the results are shown in FIGS. 8 and 9.
Example 13
The procedure was as in example 12, except that O-SSF was used in place of B-SSF in example 12.
Example 14
The field of application was the same as in example 12, except that in step (1), polyethylene was used instead of carboxymethyl cellulose. The specific implementation method comprises the following steps:
(1) a blend of Low Density Polyethylene (LDPE) and Linear Low Density Polyethylene (LLDPE) in a 4:1 mass ratio was synthesized.
(2) And (2) uniformly mixing the mixture obtained in the step (1) with B-SSF (0.02, 0.04, 0.06, 0.08, 0.10 and 0.12g) with different masses, and using the obtained mixed sample for instrument film blowing.
(3) Pure polyethylene films were prepared using a similar synthesis procedure except that no B-SSF powder was added.
(4) Applying the B-SSF-based polyethylene film obtained in the step (2) to promote the growth of the cabbage heart. The comparison of the physiological index data of the flowering Chinese cabbage is shown in Table 1.
TABLE 1 physiological index test results of cabbage heart samples
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A multicolor luminous solid silicon dot powder is characterized in that: the average particle size of the multicolor luminous solid silicon dot powder is 100nm, under the excitation of excitation wavelength of 400nm, the multicolor luminous solid silicon dot powder respectively emits blue light, green light, yellow light and orange red light, and the emission peak positions are 455nm, 534nm, 593nm and 613nm respectively.
2. The method for preparing a multicolor luminous solid silicon dot powder according to claim 1, characterized by comprising the following steps:
(1) adding a silane coupling agent into an aqueous solution of a reducing agent under the condition of introducing nitrogen, fully mixing, reacting at the temperature of 150-220 ℃ for 6-16h, cooling the obtained mixed system to room temperature after the reaction is finished, and dialyzing to obtain a fluorescent silicon dot solution;
(2) freeze-drying the fluorescent silicon dot solution obtained in the step (1) to obtain solid silicon dot powder;
(3) and (3) annealing the solid silicon dot powder obtained in the step (2) at the high temperature of 100-400 ℃ for 10min, or annealing at the high temperature of 200 ℃ for 2-180min to obtain the multicolor luminous solid silicon dot powder.
3. The method of claim 2, wherein: the reducing agent in the step (1) is sodium citrate, citric acid, ascorbic acid, sodium ascorbate, folic acid, maleic acid, aminophenol or catechol.
4. The method according to claim 2, wherein the silane coupling agent in the step (1) is at least one selected from the group consisting of N- (β -aminoethyl- γ -aminopropyl) trimethoxysilane, N-aminoethyl- γ -aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, and methyltriethoxysilane.
5. The method of claim 2, wherein: in the step (1), the dosage ratio of the reducing agent to the silane coupling agent is 1-3 g: 5-10 mL.
6. The method of claim 2, wherein: the average particle size of the fluorescent silicon dot solution in the step (1) is 1.7nm, and the fluorescent silicon dot solution is yellow when observed by naked eyes under a fluorescent lamp and bright blue when irradiated by a 365nm ultraviolet lamp; excitation is carried out by 368nm excitation wavelength, the emission wavelength is 380-600nm, and larger fluorescence emission intensity is obtained at 445 nm; the fluorescence quantum yield was 66% with quinoline sulfate as a reference.
7. The method of claim 2, wherein: the average particle size of the solid silicon dot powder in the step (2) is 100 nm; the solid powder shows yellow when observed by naked eyes under a fluorescent lamp, and shows blue-yellow dual emission under the irradiation of a 365nm ultraviolet lamp; the blue and yellow emission peak positions are respectively at 439nm and 564nm, and the fluorescence quantum efficiency is respectively 26.35% and 10.91%.
8. Use of a polychromatic luminescent solid silicon dot powder according to claim 1 in the field of solid state lighting.
9. Use of a multicolor luminous solid silicon dot powder according to claim 1 in an agricultural light conversion film, characterized in that: the multicolor luminous solid silicon dot powder is blue light solid silicon dot powder, and is combined with carboxymethyl cellulose to construct a miniature agricultural light conversion film.
10. Use of a multicolor luminous solid silicon dot powder according to claim 9 in an agricultural light conversion film, characterized in that: the multicolor luminous solid silicon dot powder is blue light solid silicon dot powder, and an agricultural light conversion film is constructed by the blue light solid silicon dot powder and polyethylene, so that the growth and development of the cabbage heart are promoted.
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