CN111217375B - Boron quantum dot, and stabilizing treatment method and application thereof - Google Patents

Boron quantum dot, and stabilizing treatment method and application thereof Download PDF

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CN111217375B
CN111217375B CN202010071870.3A CN202010071870A CN111217375B CN 111217375 B CN111217375 B CN 111217375B CN 202010071870 A CN202010071870 A CN 202010071870A CN 111217375 B CN111217375 B CN 111217375B
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王慧奇
安铎
李莹
苟立
孙立文
曹红红
王延忠
李宁
常青
薛超瑞
胡胜亮
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North University of China
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Abstract

The invention discloses a boron quantum dot, and a stabilizing treatment method and application thereof, belongs to the technical field of functional materials, relates to a boron quantum dot technology, and solves the technical problem that the boron quantum dot is difficult to stably exist in the air. A boron quantum dot stabilization treatment method comprises the following steps: (1) adding the boron quantum dot solution dispersed in the liquid phase into the carbon nano tube and graphene solution to prepare a mixed solution; (2) stirring the mixed solution, carrying out ultrasonic crushing, and centrifuging to collect precipitates; (3) freeze-drying the precipitate to obtain a composite boron quantum dot sample; (4) and (4) carrying out high-temperature treatment on the sample subjected to freeze drying in the step (3) in an inert environment, so that boron quantum dots stably exist in the carbon nano tube and the graphene. Compared with the prior art, the method can obtain the stable boron quantum dot composite material, so that the boron quantum dots stably exist in the carbon nano tube and the graphene.

Description

Boron quantum dot, and stabilizing treatment method and application thereof
Technical Field
The invention belongs to the technical field of functional materials, relates to a boron quantum dot technology, and particularly relates to a boron quantum dot, and a stabilizing treatment method and application thereof.
Background
The boron quantum dots are a novel boron nano material, have important research significance in the fields of photocatalysis, optical sensing, fluorescence imaging, neutron capture treatment, new energy and the like, and have potential application value in the fields of biology, medicine, energy storage devices, novel semiconductor devices and the like.
The current methods for preparing boron nanostructures mainly focus on magnetron sputtering, chemical vapor deposition, and ultra-high vacuum molecular beam epitaxy. Chinese patent 201910555713.7 discloses a method for preparing high-yield boron quantum dots by high-energy ultrasonic fragmentation assisted liquid phase stripping process at room temperature and normal pressure, which comprises using boron powder as a boron source for preparing fluorescent boron quantum dots, using organic solvents isopropanol and tetrahydrofuran as dual-drive chemical etching agents, and using high-energy ultrasonic fragmentation assisted liquid phase stripping method to obtain boron quantum dots which can be used as secondary battery cathode materials (the theoretical lithium storage capacity of boron is 12395 mA) h g −1 ) And boron-containing drugs for boron neutron capture therapy, and has the potential of large-scale production and wide commercial application prospect. However, the boron quantum dots prepared by the method can only exist in an organic solution stably, and once the boron quantum dots are exposed in the air, the lithium storage performance and the biological activity of the boron quantum dots are greatly reduced, so that the application of the boron quantum dots is greatly limited.
In order to solve the problems existing in the preparation of the boron quantum dots by the method, the invention provides a treatment method capable of stabilizing the boron quantum dots, and the purpose that the boron quantum dots are completely stripped from a liquid phase and exist in a solid phase is achieved.
Disclosure of Invention
The invention provides a boron quantum dot, a stabilizing treatment method and application thereof, aiming at solving the technical problem that the boron quantum dot is difficult to stably exist in the air, and the boron quantum dot is transferred from a liquid phase to a solid phase to prepare the stabilized boron quantum dot.
The invention is realized by the following technical scheme:
a boron quantum dot is prepared through adding the boron quantum dots dispersed in liquid phase to the solution of carbon nanotubes and graphene, ultrasonic breaking, centrifugal separation to collect deposit, freeze drying and high-temp heat treatment.
The invention also provides a boron quantum dot stabilizing treatment method, which comprises the following steps:
(1) adding a boron quantum dot solution with the concentration of 15-50 mg/mL dispersed in a liquid phase into a carbon nano tube and graphene solution with the concentration of 5-15 mg/mL to prepare a mixed solution;
(2) stirring the mixed solution, carrying out ultrasonic crushing, centrifuging for 20-40 min at the centrifugal speed of 8000-10000 rpm, and collecting precipitates;
(3) freeze-drying the precipitate to obtain a composite boron quantum dot sample;
(4) and (4) carrying out high-temperature treatment on the sample subjected to freeze drying in the step (3) in an inert environment, keeping the temperature at 500-1000 ℃ for 2-5 h, and then enabling the boron quantum dots to stably exist in the carbon nano tube and the graphene.
Further, the boron quantum dot solution in the step (1) is isopropanol, ethylene glycol, dimethylformamide, or a mixture of the three as a solvent in any proportion.
The carbon nano-tube in the step (1) is a multi-wall carbon nano-tube, a graphitized carboxyl multi-wall carbon nano-tube, a graphitized multi-wall carbon nano-tube or a mixture of the three in any proportion.
The graphene in the step (1) is single-layer graphene oxide, single-layer graphene or a mixture of the single-layer graphene oxide and the single-layer graphene in any proportion.
The temperature of the freeze drying in the step (3) is-52 to-48 ℃, and the time is 10 to 24 hours.
Furthermore, the invention also discloses application of the boron quantum dots in preparation of a lithium ion battery negative electrode material.
The invention adds the boron quantum dot solution into the carbon nano tube and graphene solution, improves the charge and discharge performance of the carbon nano tube and graphene as electrode materials, meanwhile, boron quantum dots can be stably present in the carbon nano tube and the graphene, specifically, the boron quantum dot solution is added into the carbon nano tube and graphene solution, the structures of the carbon nano tube and the graphene can be opened through ultrasonic crushing, thereby promoting the addition of the boron quantum dots, wherein the freeze drying is to directly change the precipitate from solid state to gas state, and then removing impurities through high-temperature treatment, and promoting the boron quantum dots to be better combined with the carbon nano tubes and the graphene under the high-temperature condition.
In order to verify the effect of the invention, the boron quantum dot doped single-layer graphene oxide and the single-layer graphene oxide prepared in the step (4) are subjected to a TEM image test, the result is shown in fig. 2, and it can be obviously seen from the TEM image of fig. 2 that the boron quantum dot is doped into the single-layer graphene oxide, which indicates that the boron quantum dot is stably existed in a solid phase; the charge and discharge performance of the mixture of the carbon nanotube doped with boron quantum and graphene is tested and compared with the first-circle charge and discharge diagram of graphitized carboxyl multi-walled carbon nanotube and single-layer graphene oxide respectively, and the result is shown in fig. 3, and it can be found from fig. 3 that when boron quantum dots stably exist in the carbon nanotube and graphene, the charge and discharge capacity of the carbon nanotube and graphene is obviously increased compared with that of the simple carbon nanotube and graphene, and the lithium storage performance is obviously improved.
Compared with the prior art, the invention has the beneficial effects that:
(1) the problem that boron quantum dots are difficult to stably exist in the air is solved, and the stable boron quantum dot composite material is obtained;
(2) when boron quantum dots exist in the carbon nano tube and the graphene stably, the lithium storage performance of the carbon nano tube and the graphene is greatly improved.
Drawings
FIG. 1 is a process for boron quantum dot stabilization;
fig. 2 is a TEM image of a monolayer of graphene oxide and a boron quantum dot doped monolayer of graphene oxide;
fig. 3 is a first-turn charge-discharge comparison graph of graphitized carboxyl multi-walled carbon nanotubes, single-layer graphene oxide, boron quantum dot-doped graphitized carboxyl multi-walled carbon nanotubes, and boron quantum dot-doped single-layer graphene oxide.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments and the accompanying drawings, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of protection of the present invention.
Example 1
(1) Adding a boron quantum dot solution with the concentration of 15mg/mL dispersed in a liquid phase into a carbon nano tube and graphene solution with the concentration of 5-15 mg/mL;
(2) stirring the solution in the step (1), carrying out ultrasonic crushing, and then centrifuging at a centrifugation speed of 8000rpm for 20min to obtain a precipitate;
(3) freeze-drying the precipitate in the step (2) at-52 ℃ for 10 hours to obtain a composite boron quantum dot sample;
(4) and (4) carrying out high-temperature treatment on the sample subjected to freeze drying in the step (3) in an inert environment, keeping the temperature for 2 hours at the highest temperature of 500 ℃, and enabling the boron quantum dots to stably exist in the carbon nano tube and the graphene.
The flow diagram of the boron quantum dot stabilization is shown in fig. 1, and the boron quantum dot solution in liquid phase is added into the carbon nanotube and graphene solution, and the stabilized boron quantum dot can be obtained through stirring, ultrasonic centrifugation, freeze drying and high-temperature treatment.
Example 2
(1) Adding a boron quantum dot solution with the concentration of 50mg/mL dispersed in a liquid phase into a graphitized carboxyl multi-walled carbon nanotube solution with the concentration of 15 mg/mL;
(2) stirring the solution in the step (1), performing ultrasonic dispersion, and centrifuging at a centrifugation speed of 10000rpm for 40min to obtain a precipitate;
(3) freeze-drying the precipitate in the step (2) at-48 ℃ for 24 hours to obtain a composite boron quantum dot sample;
(4) and (4) carrying out high-temperature treatment on the sample subjected to freeze drying in the step (3) in an inert environment, keeping the temperature for 5 hours at the maximum temperature of 1000 ℃, so that the boron quantum dots stably exist in the graphitized multi-walled carbon nanotube.
Example 3
(1) Adding a boron quantum dot solution with the concentration of 30mg/mL dispersed in a liquid phase into a graphitized carboxyl multi-walled carbon nanotube solution with the concentration of 10 mg/mL;
(2) stirring the solution in the step (1), performing ultrasonic dispersion, and centrifuging at a centrifugal speed of 9000rpm for 30min to obtain a precipitate;
(3) freeze-drying the precipitate in the step (2) at-50 ℃ for 18h to obtain a composite boron quantum dot sample;
(4) and (4) performing high-temperature treatment on the sample subjected to freeze drying in the step (3) in an inert environment, keeping the temperature at the highest temperature of 800 ℃ for 3 hours, and thus enabling the boron quantum dots to stably exist in the graphitized multi-walled carbon nanotube.
Example 4
(1) Adding a boron quantum dot solution with the concentration of 15mg/mL dispersed in a liquid phase into a single-layer graphene oxide solution with the concentration of 5 mg/mL;
(2) stirring the solution in the step (1), performing ultrasonic dispersion, and centrifuging at a centrifugation speed of 8000rpm for 20min to obtain a precipitate;
(3) freeze-drying the precipitate in the step (2) at-52 ℃ for 10 hours to obtain a composite boron quantum dot sample;
(4) and (4) carrying out high-temperature treatment on the sample subjected to freeze drying in the step (3) in an inert environment, keeping the temperature at the highest temperature of 500 ℃ for 2 hours, and then enabling the boron quantum dots to stably exist in the single-layer graphene oxide.
Example 5
(1) Adding a boron quantum dot solution with the concentration of 50mg/mL dispersed in a liquid phase into a monolayer graphene oxide solution with the concentration of 15 mg/mL;
(2) stirring the solution in the step (1), performing ultrasonic dispersion, and centrifuging at a centrifugation speed of 10000rpm for 40min to obtain a precipitate;
(3) freeze-drying the precipitate in the step (2) at-48 ℃ for 24 hours to obtain a composite boron quantum dot sample;
(4) and (4) carrying out high-temperature treatment on the sample subjected to freeze drying in the step (3) in an inert environment, keeping the temperature for 5 hours at the highest temperature of 1000 ℃, and then enabling boron quantum dots to stably exist in the single-layer graphene oxide.
Example 6
(1) Adding a boron quantum dot solution with the concentration of 30mg/mL dispersed in a liquid phase into a single-layer oxygen sublimation graphene solution with the concentration of 10 mg/mL;
(2) stirring the solution in the step (1), performing ultrasonic dispersion, and centrifuging at a centrifugal speed of 9000rpm for 30min to obtain a precipitate;
(3) freeze-drying the precipitate in the step (2) at the temperature of minus 50 ℃ for 18 hours to prepare a composite boron quantum dot sample;
(4) and (4) carrying out high-temperature treatment on the sample subjected to freeze drying in the step (3) in an inert environment, keeping the temperature at the highest temperature of 800 ℃ for 3 hours, and then enabling the boron quantum dots to stably exist in the single-layer graphene oxide.

Claims (7)

1. A boron quantum dot is characterized in that the boron quantum dot dispersed in a liquid phase is added into a carbon nano tube and graphene solution, and precipitates are collected through centrifugation after ultrasonic crushing, and are obtained through freeze drying and high-temperature heat treatment.
2. A boron quantum dot stabilization treatment method is characterized by comprising the following steps:
(1) adding a boron quantum dot solution with the concentration of 15-50 mg/mL dispersed in a liquid phase into a carbon nano tube and graphene solution with the concentration of 5-15 mg/mL to prepare a mixed solution;
(2) stirring the mixed solution, carrying out ultrasonic crushing, centrifuging for 20-40 min at the centrifugal speed of 8000-10000 rpm, and collecting precipitates;
(3) freeze-drying the precipitate to obtain a composite boron quantum dot sample;
(4) and (4) carrying out high-temperature treatment on the sample subjected to freeze drying in the step (3) in an inert environment, keeping the temperature at 500-1000 ℃ for 2-5 h, and then enabling the boron quantum dots to stably exist in the carbon nano tube and the graphene.
3. The method according to claim 1, wherein the boron quantum dot solution is isopropanol, ethylene glycol, dimethylformamide, or a mixture of the three as a solvent at any ratio.
4. The method according to claim 1 or 2, wherein the carbon nanotubes of step (1) are multi-walled carbon nanotubes, graphitized carboxyl multi-walled carbon nanotubes, graphitized multi-walled carbon nanotubes, or a mixture of the three in any ratio.
5. The boron quantum dot stabilization treatment method according to claim 1 or 2, wherein the graphene in the step (1) is a single-layer graphene oxide, a single-layer graphene, or a mixture of the two in any ratio.
6. The boron quantum dot stabilization treatment method according to claim 1 or 2, wherein the temperature of the freeze drying in the step (3) is-52 to-48 ℃, and the time is 10 to 24 hours.
7. The use of the boron quantum dot of claim 1 in the preparation of a lithium ion battery negative electrode material.
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