CN113337280A - Preparation method of controllable full-spectrum luminescent boron nitride quantum dots - Google Patents
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Abstract
The invention discloses a preparation method of a controllable full-spectrum luminescent boron nitride quantum dot, which comprises the steps of taking a hexagonal boron nitride nanosheet as a precursor, taking an amino compound as a passivating agent, jointly adding the hexagonal boron nitride nanosheet and the amino compound into an organic solvent for hydrothermal reaction, and adjusting the types of the amino compound and the organic solvent to obtain the full-spectrum boron nitride quantum dot in a visible light range. According to the invention, the surface of the boron nitride quantum dot is regulated and controlled for the first time, and the amination degree of the surface of the quantum dot is influenced by the passivating agent and the solvent, so that full-spectrum luminescence of the quantum dot is realized; the boron nitride, the amino compound and the organic solvent used in the preparation method are low in cost, the preparation and purification processes are mild and simple, and the macro-preparation under laboratory conditions can be realized.
Description
Technical Field
The invention belongs to a preparation method of a functionalized nano fluorescent material, and particularly relates to a controllable preparation method of a full-spectrum luminescent boron nitride quantum dot.
Background
In recent years, performance regulation and control can be realized by using a two-dimensional semiconductor material as a precursor to prepare the zero-dimensional quantum dots, and the method is widely applied to the photoelectric fields of LEDs, biological imaging, fluorescence calibration, photocatalysis and the like. At present, zero-dimensional quantum dot materials prepared by taking graphene, black phosphorus and transition metal oxides as precursors realize effective regulation and control of properties such as luminescence, size, band gap and the like, and are successfully applied to the fields of photoelectric display, biomedicine, batteries and the like. With the inspiration, the boron nitride quantum dots are also developed rapidly, and the exploration of optical performance is started. Allwood et al first tried to obtain blue-light boron nitride quantum dots by an ultrasonic method and to realize biological imaging. Then, researchers develop researches on the boron nitride luminescence property and the application field, the quantum yield is continuously improved, and the application field is expanded. However, the boron nitride quantum dots have not realized full spectrum luminescence so far, and the emission wavelength is mainly in the blue region, which hinders further development in the field of photoelectricity. Meanwhile, the research on the surface modification engineering of the boron nitride quantum dots is still blank, and further research and development are needed.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a controllable preparation method of optical boron nitride quantum dots capable of realizing full-spectrum luminescence in a visible light range.
The technical scheme is as follows: the invention discloses a preparation method of a controllable full-spectrum luminescent boron nitride quantum dot, which comprises the steps of taking a hexagonal boron nitride nanosheet as a precursor, taking an amino compound as a passivating agent, adding the hexagonal boron nitride nanosheet and the amino compound into an organic solvent together for hydrothermal reaction, and adjusting the types of the amino compound and the organic solvent to obtain the full-spectrum boron nitride quantum dot in a visible light range.
Further, the amino compound is any one of urea, thiourea or p-phenylenediamine.
Further, the organic solvent is any one of N-methyl pyrrolidone, sulfuric acid, acetone, N-N dimethylformamide and absolute ethyl alcohol.
In the technical scheme, the hexagonal boron nitride is a layered structure consisting of N atoms and B atoms, the hexagonal boron nitride is easily oxidized at the edge under the action of oxygen in the air to form an N-O-B bond, and the amino group in the amino compound and the B atom in the N-O-B bond are coordinated and combined through the mixed reaction of the amino compound and the organic solvent, so that the surface functional modification of the boron nitride is realized. The prepared boron nitride quantum dots influence the surface amination degree of the quantum dots through a passivating agent and an organic solvent, the oxidation degree of the boron nitride quantum dots can be reduced through the functionalization of an amino compound under the action of different organic solvents, the amination degree of hexagonal boron nitride is gradually deepened through different amino functional groups, the surface state is gradually increased, the gradual red shift of a light-emitting spectrum is caused, and the full-spectrum light-emitting of the quantum dots is realized.
Further, the preparation method of the controllable full-spectrum luminescent boron nitride quantum dot comprises the following specific steps:
(1) placing hexagonal boron nitride powder in absolute ethyl alcohol for ultrasonic treatment, and taking an upper suspension after standing;
(2) drying the upper suspension obtained in the step (1) by using a solvent, and then respectively adding an amino compound and an organic solvent to carry out hydrothermal reaction;
(3) and after the reaction is finished, cooling to room temperature to obtain a crude solution product, and separating and purifying to obtain the boron nitride quantum dots.
The hexagonal boron nitride is subjected to solvent ultrasonic treatment, so that flaky hexagonal boron nitride can be obtained and used as a precursor of a hydrothermal reaction, and quantum dots can be formed after the hydrothermal reaction in the next step; the hydrothermal reaction is adopted, the preparation is simple, the reaction condition is controllable, and the effective amination reaction of the boron nitride quantum dots can be realized.
Furthermore, in the step (3), the emission peak wavelength of the boron nitride quantum dots is 420-610 nm. Preferably, the emission peak wavelengths of the boron nitride quantum dots are 420nm, 510nm, 528nm, 575nm and 610nm respectively, which correspond to blue light, green light, yellow-green light, yellow light and red light respectively.
Furthermore, in the step (1), 0.1-1 g of hexagonal boron nitride powder is added into 75mL of absolute ethyl alcohol.
Further, in the step (2), the volume ratio of the upper suspension to the organic solvent is 1: 2 to 4.
Further, in the step (2), 0.05 to 0.1g of an amino compound is added to 15mL of an organic solvent.
Further, in the step (2), the reaction temperature of the hydrothermal reaction is 180-250 ℃, and the reaction time is 8-15 h.
Further, in the step (3), the separation and purification method specifically refers to filtering the crude quantum dot product by using a 220nm PTFE filter.
The principle of the invention is as follows: different amino compounds have different surface energies in the hydrothermal process of boron nitride and have different bonding degrees with the boron nitride; for example, the surface activity of the aminated urea, thiourea and p-phenylenediamine is increased in sequence, and the amination degree is gradually deepened. Meanwhile, the boiling point of the solvent also affects the hydrothermal reaction degree: the lower the boiling point of the solvent during the hydrothermal reaction, the higher the reaction vapor pressure, the greater the degree of reaction: for example, with the same p-phenylenediamine amide deactivation, the boiling points of sulfuric acid, DMF and ethanol decrease in sequence, and the higher the reaction vapor pressure, the greater the degree of amination. Therefore, the amino compound and the solvent can jointly influence the amination degree of the boron nitride quantum dot in the hydrothermal process, so that the surface state is gradually increased to cause spectral red shift, and the full-spectrum luminescence of the boron nitride quantum dot is realized.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: according to the invention, the surface of the boron nitride quantum dot is regulated and controlled by the surface passivating agent and the solvent for the first time, the prepared boron nitride quantum dot influences the surface amination degree of the quantum dot by the passivating agent and the solvent, different amino functional groups enable the amination degree to be gradually deepened, the surface state is gradually increased, and the gradual red shift of a luminescence spectrum is caused, so that the full-spectrum luminescence of the quantum dot is realized, including the visible light range from blue light to red light; the boron nitride, the amino compound and the organic solvent used in the preparation method are low in cost, the preparation and purification processes are mild and simple, and the macro-preparation under laboratory conditions can be realized.
Drawings
FIG. 1 is a fluorescence spectrum of boron nitride quantum dots prepared according to an embodiment of the present invention;
FIG. 2 is a morphology and particle size distribution of the boron nitride quantum dots in the embodiment 1 under a transmission electron microscope;
FIG. 3 is a morphology and particle size distribution of the boron nitride quantum dots in example 3 under a transmission electron microscope;
FIG. 4 is a morphology and particle size distribution of the boron nitride quantum dots in the embodiment 5 under a transmission electron microscope;
fig. 5 is an X-ray photoelectron spectrum of nitrogen element in the boron nitride quantum dot in embodiment 1;
fig. 6 is an X-ray photoelectron spectrum of nitrogen in the boron nitride quantum dots in example 3;
fig. 7 is an X-ray photoelectron spectrum of nitrogen element in the boron nitride quantum dot in example 5;
FIG. 8 is a diagram of a theoretical model structure of the degree of amination on the surface of boron nitride and a calculation of the change of the reaction content in different binding cases by using the density functional theory.
Detailed Description
The technical solution of the present invention is further described in detail with reference to the accompanying drawings and examples.
Example 1
(1) Weighing 0.5g of hexagonal boron nitride powder, placing the hexagonal boron nitride powder in 75ml of absolute ethyl alcohol, carrying out ultrasonic treatment for 12 hours, standing for 24 hours, and taking an upper-layer suspension;
(2) taking 5ml of upper layer suspension in a 25ml of polytetrafluoroethylene reaction kettle, drying the solvent, and adding 0.1g of urea and 15ml of NMP;
(3) placing the reaction kettle in a high-temperature oven for hydrothermal reaction for 10 hours at 180 ℃;
(4) naturally cooling to room temperature after the reaction is finished to obtain a brown solution crude product;
(5) and filtering the crude product of the quantum dots by using a PTFE (polytetrafluoroethylene) filter with the wavelength of 220nm to obtain purified boron nitride quantum dots, wherein the quantum dots emit blue light.
Analyzing the size and aggregation state of the quantum dots by using a transmission electron microscope, dripping the blue light quantum dot solution on a carbon film, scanning by using the transmission electron microscope, and obtaining a test result as shown in figure 2.
And analyzing the chemical structure of nitrogen elements in the quantum dots by using an X-ray photoelectron spectrogram, dropping blue light quanta on a silicon substrate for XPS test, processing the nitrogen element data, wherein the single element chemical structure mainly comprises N-B and N-O-B, and the formation of an N-O-B bond shows that the boron nitride quantum dots realize effective surface functionalization.
Example 2
(1) Weighing 0.8g of hexagonal boron nitride powder, placing the hexagonal boron nitride powder in 75ml of absolute ethyl alcohol, carrying out ultrasonic treatment for 15h, standing for 24h, and taking an upper-layer suspension;
(2) taking 5ml of upper layer suspension liquid in a 25ml of polytetrafluoroethylene reaction kettle, drying the solvent, and adding 0.75g of p-phenylenediamine and 15ml of sulfuric acid solvent;
(3) placing the reaction kettle in a high-temperature oven for hydrothermal reaction for 10 hours at 200 ℃;
(4) naturally cooling to room temperature after the reaction is finished to obtain a brown solution crude product;
(5) and filtering the crude product of the quantum dots by using a PTFE (polytetrafluoroethylene) filter with the wavelength of 220nm to obtain the purified boron nitride quantum dots, wherein the quantum dots are green and luminous.
Example 3
(1) Weighing 0.5g of hexagonal boron nitride powder, placing the hexagonal boron nitride powder in 75ml of absolute ethyl alcohol, carrying out ultrasonic treatment for 18h, standing for 24h, and taking an upper-layer suspension;
(2) taking 5ml of upper layer suspension liquid in a 25ml of polytetrafluoroethylene reaction kettle, drying the solvent, and adding 0.05g of thiourea and 15ml of acetone;
(3) placing the reaction kettle in a high-temperature oven for hydrothermal reaction at 250 ℃ for 15 h;
(4) naturally cooling to room temperature after the reaction is finished to obtain a brown solution crude product;
(5) and filtering the crude product of the quantum dots by using a PTFE (polytetrafluoroethylene) filter with the wavelength of 220nm to obtain the purified boron nitride quantum dots, wherein the quantum dots are yellow-green and luminous.
Analyzing the size and aggregation state of the quantum dots by using a transmission electron microscope, dripping the solution of the yellow-green light quantum dots on a carbon film, scanning by using the transmission electron microscope, and obtaining a test result as shown in figure 3. the size of the quantum dots is 5.5nm, the quantum dots are uniformly dispersed and have no aggregation phenomenon as can be seen from a transmission electron microscope picture of the quantum dots.
Analyzing the chemical structure of nitrogen element in the quantum dot by using an X-ray photoelectron spectrogram, drop-coating yellow green light quantum on a silicon substrate for XPS test, processing the nitrogen element data, and then forming an N-O-B bond, wherein the single element chemical structure mainly comprises N-B and N-O-B, and the formation of the N-O-B bond shows that the boron nitride quantum dot realizes effective surface functionalization; compared with the blue light quantum dots, the reduction of the oxygen-containing bonds shows that the oxidation degree of the boron nitride quantum dots in the solvent ultrasonic or hydrothermal process is reduced, and the amination degree is gradually enhanced.
Example 4
(1) Weighing 1g of hexagonal boron nitride powder, placing the hexagonal boron nitride powder in 75ml of absolute ethyl alcohol, carrying out ultrasonic treatment for 24 hours, standing for 24 hours, and taking an upper layer suspension;
(2) taking 5ml of upper layer suspension in a 25ml of polytetrafluoroethylene reaction kettle, drying the solvent, and adding 0.1g of p-phenylenediamine and 15ml of DMF;
(3) placing the reaction kettle in a high-temperature oven for hydrothermal reaction at 210 ℃ for 24 hours;
(4) naturally cooling to room temperature after the reaction is finished to obtain a brown solution crude product;
(5) and filtering the crude product of the quantum dots by using a PTFE (polytetrafluoroethylene) filter with the wavelength of 220nm to obtain purified boron nitride quantum dots, wherein the quantum dots are yellow and luminous.
Example 5
(1) Weighing 0.1g of hexagonal boron nitride powder, placing the hexagonal boron nitride powder in 75ml of absolute ethyl alcohol, carrying out ultrasonic treatment for 12 hours, standing for 24 hours, and taking an upper-layer suspension;
(2) taking 5ml of upper layer suspension in a 25ml of polytetrafluoroethylene reaction kettle, drying the solvent, and adding 0.1g of p-phenylenediamine and 15ml of absolute ethyl alcohol;
(3) placing the reaction kettle in a high-temperature oven for hydrothermal reaction at 180 ℃ for 8 hours;
(4) naturally cooling to room temperature after the reaction is finished to obtain a brown solution crude product;
(5) and filtering the crude product of the quantum dots by using a PTFE (polytetrafluoroethylene) filter with the wavelength of 220nm to obtain purified boron nitride quantum dots, wherein the quantum dots emit red luminescence.
Analyzing the size and aggregation state of the quantum dots by using a transmission electron microscope, dripping the red light quantum dot solution on a carbon film, scanning by using the transmission electron microscope, and obtaining a test result as shown in figure 4. the quantum dots have the size of 2.5nm, are uniformly dispersed and have no aggregation phenomenon as can be seen from a transmission electron microscope picture of the quantum dots.
Analyzing the chemical structure of nitrogen element in the quantum dot by using an X-ray photoelectron spectrogram, dropping red light quantum on a silicon substrate for XPS test, processing the nitrogen element data, and then forming an N-O-B bond, wherein the single element chemical structure mainly comprises N-B and N-O-B, and the formation of the N-O-B bond shows that the boron nitride quantum dot realizes effective surface functionalization; compared with blue light and yellow green light quantum dots, the gradual reduction of the oxygen-containing bonds shows that the oxidation degree of the boron nitride quantum dots in the solvent ultrasonic or hydrothermal process is reduced, and the amination degree is further deepened, so that the luminescence spectrum is gradually red-shifted.
Experimental example 1
The fluorescence properties of the boron nitride quantum dots of examples 1-5 were tested by fluorescence spectroscopy, and the specific results are shown in fig. 1.
Example 1: taking 1mL of quantum dot stock solution, measuring 5mL of NMP solvent, diluting, and placing in a quartz cuvette. The measurement was carried out using a fluorescence spectrometer at a laser wavelength of 365nm, the emission wavelength being 420 nm.
Example 2: taking 1mL of quantum dot stock solution, measuring 5mL of concentrated sulfuric acid solvent, diluting, and placing in a quartz cuvette. The measurement was carried out using a fluorescence spectrometer at a laser wavelength of 380nm, the emission wavelength being 510 nm.
Example 3: taking 1mL of quantum dot stock solution, measuring 5mL of concentrated sulfuric acid solvent, diluting, and placing in a quartz cuvette. The measurement was carried out using a fluorescence spectrometer at a laser wavelength of 410nm, with an emission wavelength of 528 nm.
Example 4: taking 1mL of quantum dot stock solution, measuring 5mL of concentrated sulfuric acid solvent, diluting, and placing in a quartz cuvette. The measurement was carried out using a fluorescence spectrometer at a laser wavelength of 500nm, the emission wavelength being 575 nm.
Example 5: taking 1mL of quantum dot stock solution, measuring 5mL of concentrated sulfuric acid solvent, diluting, and placing in a quartz cuvette. The measurement was carried out using a fluorescence spectrometer at a laser wavelength of 520nm, the emission wavelength being 610 nm.
The above tests demonstrate that the present invention can realize surface control of boron nitride quantum dots by a surface passivating agent and a solvent, and the full spectrum luminescence of the prepared boron nitride quantum dots includes a visible light range from blue light to red light.
Experimental example 2
The reaction culverts under different combinations of boron nitride and amino functional groups were calculated using the density functional theory, see fig. 8. In theory, the amino functional group is more easily bonded to the B atom at the edge of the boron nitride. Considering that boron nitride is oxidized during the actual solvent ultrasonic and hydrothermal reaction, B atoms are more easily combined with-OH, and N atoms are more easily combined with-H. In such a case, FIG. a shows an amino functional group bonded to the B-O bond at the edge of the oxidized boron nitride; FIG. B shows an amino functional group directly bonded to the oxidized B atom of boron nitride. The calculation results show that the reaction energy of the amino functional group bonded to the B-O bond at the edge of the oxidized boron nitride is-3.34 eV, and the reaction energy of the amino functional group directly bonded to the B atom of the oxidized boron nitride is 1.87eV, which indicates that the amino functional group is bonded to the B-O bond at the edge of the oxidized boron nitride and the functional group after the amination exists in the form of B-O-N in the actual reaction process.
Claims (10)
1. A method for preparing controllable full-spectrum luminescent boron nitride quantum dots is characterized by comprising the following steps: the method comprises the steps of taking a hexagonal boron nitride nanosheet as a precursor, taking an amino compound as a passivating agent, adding the hexagonal boron nitride nanosheet and the amino compound into an organic solvent together for hydrothermal reaction, and adjusting the types of the amino compound and the organic solvent to obtain the full-spectrum boron nitride quantum dot in a visible light range.
2. The method for preparing the controllable full-spectrum luminescent boron nitride quantum dot as claimed in claim 1, wherein: the amino compound is any one of urea, thiourea or p-phenylenediamine.
3. The method for preparing the controllable full-spectrum luminescent boron nitride quantum dot as claimed in claim 1, wherein: the organic solvent is any one of N-methyl pyrrolidone, sulfuric acid, acetone, N-N dimethylformamide and absolute ethyl alcohol.
4. The method for preparing the controllable full-spectrum luminescent boron nitride quantum dot according to any one of claims 1 to 3, which is characterized by comprising the following specific steps:
(1) placing hexagonal boron nitride powder in absolute ethyl alcohol for ultrasonic treatment, and taking an upper suspension after standing;
(2) drying the upper suspension obtained in the step (1) by using a solvent, and then respectively adding an amino compound and an organic solvent to carry out hydrothermal reaction;
(3) and after the reaction is finished, cooling to room temperature to obtain a crude solution product, and separating and purifying to obtain the boron nitride quantum dots.
5. The method for preparing the controllable full-spectrum luminescent boron nitride quantum dot as claimed in claim 4, wherein the method comprises the following steps: in the step (3), the emission peak wavelength of the boron nitride quantum dots is 420-610 nm.
6. The method for preparing the controllable full-spectrum luminescent boron nitride quantum dot as claimed in claim 4, wherein the method comprises the following steps: in the step (1), 0.1-1 g of hexagonal boron nitride powder is added into 75mL of absolute ethyl alcohol.
7. The method for preparing the controllable full-spectrum luminescent boron nitride quantum dot as claimed in claim 4, wherein the method comprises the following steps: in the step (2), the volume ratio of the upper suspension to the organic solvent is 1: 2 to 4.
8. The method for preparing the controllable full-spectrum luminescent boron nitride quantum dot as claimed in claim 4, wherein the method comprises the following steps: in the step (2), 0.05-0.1 g of an amino compound is added to 15mL of an organic solvent.
9. The method for preparing the controllable full-spectrum luminescent boron nitride quantum dot as claimed in claim 4, wherein the method comprises the following steps: in the step (2), the reaction temperature of the hydrothermal reaction is 180-250 ℃, and the reaction time is 8-15 h.
10. The method for preparing the controllable full-spectrum luminescent boron nitride quantum dot as claimed in claim 4, wherein the method comprises the following steps: in the step (3), the separation and purification method specifically refers to filtering the crude quantum dot product by using a 220nm PTFE filter.
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| CN113845902A (en) * | 2021-09-18 | 2021-12-28 | 山东大学 | Carbon-oxygen co-doped boron nitride quantum dot with green fluorescence and preparation method and application thereof |
| CN115465844A (en) * | 2022-08-25 | 2022-12-13 | 东南大学 | Preparation method of white light emitting boron nitride quantum dots |
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| CN105060262A (en) * | 2015-07-03 | 2015-11-18 | 复旦大学 | Water-soluble boron nitride quantum dot and preparation method thereof |
| CN108529574A (en) * | 2018-07-16 | 2018-09-14 | 青岛大学 | A kind of preparation method of ultrathin boron nitride nanosheet and its dispersion liquid |
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| CN105060262A (en) * | 2015-07-03 | 2015-11-18 | 复旦大学 | Water-soluble boron nitride quantum dot and preparation method thereof |
| CN108529574A (en) * | 2018-07-16 | 2018-09-14 | 青岛大学 | A kind of preparation method of ultrathin boron nitride nanosheet and its dispersion liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113845902A (en) * | 2021-09-18 | 2021-12-28 | 山东大学 | Carbon-oxygen co-doped boron nitride quantum dot with green fluorescence and preparation method and application thereof |
| CN115465844A (en) * | 2022-08-25 | 2022-12-13 | 东南大学 | Preparation method of white light emitting boron nitride quantum dots |
| CN115465844B (en) * | 2022-08-25 | 2024-04-05 | 东南大学 | Preparation method of white light-emitting boron nitride quantum dot |
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