CN111484004B - Preparation method of graphene quantum dots - Google Patents
Preparation method of graphene quantum dots Download PDFInfo
- Publication number
- CN111484004B CN111484004B CN201910074574.6A CN201910074574A CN111484004B CN 111484004 B CN111484004 B CN 111484004B CN 201910074574 A CN201910074574 A CN 201910074574A CN 111484004 B CN111484004 B CN 111484004B
- Authority
- CN
- China
- Prior art keywords
- inert gas
- treatment
- nano tube
- plasma treatment
- graphene quantum
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
Abstract
The invention provides a preparation method of graphene quantum dots, which comprises the following steps: providing an initial carbon nanotube, and performing oxidation treatment on the initial carbon nanotube to obtain a first carbon nanotube; calcining the first carbon nano tube to obtain a second nano tube; and carrying out inert gas plasma treatment on the second carbon nano tube to obtain the graphene quantum dot. According to the preparation method, the graphene quantum dot material with stable photoelectric performance and high quantum efficiency is prepared through oxidation, cutting and other processes. The graphene quantum dots prepared by the method are stable in batch, high in production efficiency and suitable for industrial production, and have wide application prospects in the fields of photoelectric display devices, photovoltaic devices and biomedicine.
Description
Technical Field
The invention relates to the field of materials, in particular to a preparation method of graphene quantum dots.
Background
Graphene (Graphene) is a planar two-dimensional nanomaterial consisting of a single layer of carbon atoms. The carbon atoms in the graphene are all sp 2 The rail hybridization is carried out in the mode, so that the graphene has the characteristics of high heat conductivity coefficient, high electric conductivity coefficient, high structural strength and the like.
In recent years, graphene quantum dots have attracted attention from researchers as a novel fluorescent material. When two-dimensional graphene sheets are broken down to the nanoscale (typically less than 10 nm), graphene exhibits semiconductor properties; under photon excitation, fluorescence is emitted. Graphene quantum dots have attracted extensive research interest since their discovery. Similar to the semiconductor quantum dots, the graphene quantum dots have the advantages of adjustable fluorescence emission, higher light stability, wide excitation spectrum, small size and the like. In addition, the graphene quantum dot has the advantages of good biocompatibility, low toxicity, easiness in surface functionalization and the like. The advantages make up the defects of the semiconductor quantum dots and the traditional organic dyes, so that the semiconductor quantum dots have wide application prospects in the fields of photoelectric display devices, photovoltaic devices, biomedicine and the like.
At present, researchers have developed a plurality of methods for synthesizing graphene quantum dots, but the methods have certain problems, such as low synthesis efficiency, poor fluorescence performance of the obtained graphene quantum dots, concentration of fluorescence emission wavelength in a blue light region, low fluorescence quantum efficiency and the like. Therefore, how to efficiently prepare graphene quantum dots excellent in quantum efficiency is a hot spot of current researchers.
Disclosure of Invention
In view of the defects in the prior art, the invention provides a preparation method of graphene quantum dots.
The preparation method of the graphene quantum dot comprises the following steps:
providing an initial carbon nanotube, and performing oxidation treatment on the initial carbon nanotube to obtain a first carbon nanotube; calcining the first carbon nano tube to obtain a second nano tube; and carrying out inert gas plasma treatment on the second carbon nano tube to obtain the graphene quantum dot.
According to the preparation method, the graphene quantum dot material with stable photoelectric performance and high quantum efficiency is prepared through oxidation, calcination (cutting of the carbon nano tube), argon plasma treatment (cutting of the carbon nano tube) and other processes. The graphene quantum dot prepared by the method meets the actual quantum dot size requirement, has stable batch, uniform size distribution and high production efficiency, is suitable for industrial production, and has wide application prospects in the fields of photoelectric display devices, photovoltaic devices and biomedicine.
Drawings
Fig. 1 is a flow chart of a process for preparing graphene quantum dots according to some embodiments of the present invention.
Detailed Description
The invention provides a preparation method of graphene quantum dots, which is used for making the purposes, technical schemes and effects of the invention clearer and more definite, and is further described in detail below. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
As shown in fig. 1, some embodiments of the present invention provide a method for preparing graphene quantum dots, which includes the following steps:
s10, providing an initial carbon nanotube, and carrying out oxidation treatment on the initial carbon nanotube to obtain a first carbon nanotube;
s20, calcining the first carbon nanotubes to obtain second nanotubes;
s30, performing inert gas plasma treatment on the second carbon nano tube to obtain the graphene quantum dot.
According to the preparation method, the graphene quantum dot material with stable photoelectric performance and high quantum efficiency is prepared through oxidation, calcination (cutting of the carbon nano tube), argon plasma treatment (cutting of the carbon nano tube) and other processes. The graphene quantum dot prepared by the method meets the actual quantum dot size requirement, has stable batch, uniform size distribution and high production efficiency, is suitable for industrial production, and has wide application prospects in the fields of photoelectric display devices, photovoltaic devices and biomedicine.
Specifically, in some embodiments, in the step S10, the initial carbon nanotubes are single-walled carbon nanotubes, and compared with multi-walled nanotubes, graphene quantum dots with suitable dimensions (3-10 nm) and uniform distribution are more easily realized through subsequent oxidation, cutting and cutting processes. Therefore, the obtained graphene quantum dot has more stable photoelectric performance and higher quantum efficiency.
In some embodiments, in the step S10, the initial nanotubes may be oxidized by a conventional method to attach oxidized groups (e.g., carboxyl groups) to the surfaces of the carbon nanotubes, and these groups may escape as small molecules and form defects on the surfaces of the carbon nanotubes during the calcination in the subsequent step S02.
In some embodiments, in the step S10, a certain amount of initial carbon nanotube powder, deionized water, and concentrated nitric acid are added into a three-necked flask, stirred uniformly, and heated in a water bath. And transferring the obtained initial carbon nanotube treatment liquid into a centrifuge tube after heating in a water bath, centrifuging at 8000 rpm, pouring out the supernatant, redispersing the precipitate in deionized water, and repeatedly centrifuging until the pH of the supernatant is 6-7. And (3) drying the treated initial carbon nano tube in vacuum to obtain oxidized initial carbon nano tube powder. In the process, the concentrated nitric acid water bath is used for treating the initial carbon nano tube to oxidize part of carbon atoms, so that oxidized groups (such as carboxyl groups) are introduced to the surface of the initial carbon nano tube, the dispersion performance of the initial carbon nano tube is improved, and in the subsequent calcining process of step S02, the groups can escape in the form of small molecules and form defects on the surface of the carbon nano tube.
In some specific embodiments, in the step S10, the concentrated nitric acid may be replaced by a strong oxidizing water-soluble substance such as potassium permanganate, a mixed solution of concentrated nitric acid and potassium permanganate, and the like.
In some specific embodiments, in the step S10, the ratio of the initial carbon nanotube to the deionized water is in the range of 1:50-500, the ratio of the initial carbon nanotube to the deionized water is too small, the concentration of the initial carbon nanotube is low, the treatment efficiency is slow, and the ratio of the initial carbon nanotube to the deionized water is too large, so that the initial carbon nanotube cannot be completely immersed into the deionized water, and the carboxylation process of the initial carbon nanotube is affected; the ratio of deionized water to concentrated nitric acid is 1:1-5, the ratio of the deionized water to the concentrated nitric acid is too small, the nitric acid content is too high, nitrogen dioxide is generated by the solution in the reaction process, the influence on the environment is large, the ratio of the deionized water to the concentrated nitric acid is too large, the oxidizing property of the reaction solution is too small, and the initial carbon nano tube cannot be effectively oxidized.
In some specific embodiments, in the step S10, the water bath temperature is 70-90 ℃, the temperature is too low, the initial carbon nanotube carboxylation time is long, the production efficiency is reduced, the temperature is too high, nitric acid is decomposed in a large amount, the oxidizing property of the reaction solution is reduced, and the initial carbon nanotube cannot be carboxylated effectively; the initial carbon nano tube carboxylation time range is 2-6 h, the time is too short, the initial carbon nano tube cannot be effectively oxidized, the time is too long, the production period is prolonged, and the industrial production is not facilitated.
In some specific embodiments, in the step S10, the rotational speed of the centrifugal treatment is 5000 rpm, the time is 3-5 min, the rotational speed of the centrifugal treatment is too low, the initial carbon nanotubes cannot be completely settled due to too short centrifugal time, the yield is reduced, the rotational speed of the centrifugal treatment is too high, the energy consumption is increased due to too long centrifugal time, and the production cost is increased.
In some embodiments, in the step S20, a certain amount of the first carbon nanotube powder is taken and placed in a quartz boat, the quartz boat is transferred into a tubular muffle furnace, inert gas is introduced, air in the tubular muffle furnace is removed, the temperature is quickly increased to 800-1500 ℃ for first calcination treatment, water vapor is introduced after the treatment for 15-60 min, second calcination treatment is performed at 800-1000 ℃ for 10-30 min, and the cut second carbon nanotubes are obtained.
In some embodiments, the first calcination treatment is performed by heating to 800-1500 ℃ to make the organic functional groups on the surface of the first carbon nanotube escape in the form of small molecules and form defects on the surface of the carbon nanotube. The subsequent steam introduction is to utilize water molecules to react with carbon atoms at high temperature to further etch and fracture the carbon nanotubes, so as to achieve the aim of cutting the carbon nanotubes. Because the reactivity of the carbon atoms at the defect is relatively high, water molecules can react with the carbon atoms preferentially, so that the defect can be gradually enlarged under the action of the water molecules, and finally the carbon nano tube is broken.
In some embodiments, the moving speed of the inert gas in the tubular muffle furnace is 20 cm-50 cm/min, the moving speed is too high, the gas is wasted, the cost is increased, the certain speed is too low, the risk of air penetrating into the muffle furnace is increased, and the inert environment of the reaction system cannot be effectively ensured;
in some embodiments, the first calcination treatment temperature is 800 ℃ to 1500 ℃, the temperature is too high, energy is wasted, the cost is increased, the temperature is too low, organic functional groups cannot effectively escape, the etching effect of the carbon nano tube is poor, and the subsequent reaction is affected; the first calcination treatment time is 15-60 min, the time is too short, organic functional groups cannot effectively escape, the etching effect of the carbon nano tube is poor, the subsequent reaction is affected, the time is too long, the preparation period is long, and the production is not facilitated.
In some embodiments, the second calcination treatment is performed in a mixed atmosphere with a volume ratio of water vapor to inert gas of 100:5-20, so that a large amount of carbon nanotubes react with water molecules, the production efficiency is reduced, the water vapor content is too low, the etched carbon nanotubes are relatively small, the carbon nanotubes cannot be cut into carbon nanotube short tubes smaller than 10nm, and further, quantum dots with proper sizes are difficult to prepare.
In some embodiments, the temperature of the second calcination treatment is 800-1000 ℃, the temperature is too high, energy is wasted, the cost is increased, the temperature is too low, the reaction of the carbon nano tube and water molecules is slow, the preparation period is long, and the production is not facilitated; the second calcination treatment time is 10-30 min, the time is too short, the etched carbon nano tube amount is small, the carbon nano tube cannot be cut into carbon nano short tubes smaller than 10nm, the subsequent reaction is affected, the time is too long, the preparation period is long, and the production is not facilitated.
In some embodiments, in the step S30, the second carbon nanotube short tube is placed in a fluidized bed reactor equipped with a plasma generating device (the reaction device is a pair of parallel electrodes connected in a fluidized bed reaction chamber, a high-energy arc is generated between the parallel electrodes after a power supply is turned on, and inert gas is ionized into inert gas plasma when passing through the parallel electrodes), and the flow of the inert gas is regulated to a certain range, so that the second carbon nanotube forms a stable fluidized state. And simultaneously, adjusting the positions of the parallel electrodes in the fluidized bed, and enabling the second carbon nano tubes in the fluidized state to be positioned between the parallel electrodes. After the air in the fluidized bed is completely exhausted, a power supply is started, an electric arc is generated between the positive electrode and the negative electrode, and when inert gas passes through the area between the positive electrode and the negative electrode, ionization occurs under the action of the electric arc, so that inert gas plasma is generated. And after the carbon nano tube is bombarded by the inert gas plasma for 30-60 min, turning off a power supply, continuously introducing the inert gas to the reactor, cooling to room temperature, and taking out the product in the reactor to obtain graphene quantum dot powder.
In some embodiments, the second carbon nanotube is subjected to an inert gas plasma treatment selected from argon plasma treatment, helium plasma treatment, neon plasma treatment, krypton plasma treatment, or xenon plasma treatment.
In some embodiments, the moving speed of the inert gas in the fluidized bed reactor is 50-100 cm/min, the moving speed of the inert gas is too low, the carbon nano tube is deposited at the bottom of the reactor, a fluidized state cannot be formed, the energy utilization rate is low, the prepared product is non-uniform, the moving speed of the inert gas is too high, the carbon nano tube is easily carried out of the reactor by airflow, and the production efficiency of the graphene quantum dot is obviously reduced;
in some embodiments, further, the second carbon nanotubes in the fluidized state need to be located between the parallel electrodes as much as possible, otherwise, the inert gas plasma generated between the electrodes cannot act on the carbon nanotubes completely and effectively, so that the carbon nano short tubes cannot be cut into graphene quantum dots with uniform sizes.
In some embodiments, the evacuation operation is because during the generation of the plasma, if air is present in the reactor, multiple plasmas are generated, affecting the purity and yield of the reaction products.
In some embodiments, the plasma generator has a power discharge frequency of 40KHz, 13.56MHz, 2.45GHz, and other frequencies are not allowed due to wireless communication.
In some embodiments, the practical voltage of the plasma generator is 380V, the discharge current is 5-20A, the current is too small, the production period of inert gas ionization efficiency is long, industrial production is not facilitated, the current is too large, damage to positive and negative electrodes is large, parallel electrodes need to be replaced frequently, and production cost is increased.
In some embodiments, the distance between the parallel electrodes (positive electrode and negative electrode) is 2-20 mm, the distance is too short, the inert gas plasma generation efficiency is low, the synthesis efficiency is low, the production period is prolonged, the distance is too long, and the arc condition between the electrodes becomes severe, so that the arc condition is difficult to realize.
In some embodiments, the reaction time of the carbon nano short tube in the fluidized bed is 30-60 min, the time is too short, the carbon nano short tube cannot be fully opened due to the fact that the carbon nano short tube is bombarded by inert gas plasma, the graphene quantum dot material is obtained, the purity of the material is affected, the time is too long, the production period is prolonged, energy is wasted, and the production cost is increased.
According to the preparation method provided by the embodiment of the invention, the graphene quantum dot material with stable photoelectric performance and high quantum efficiency is prepared through oxidation, calcination (cutting of the carbon nano tube), argon plasma treatment (cutting of the carbon nano tube) and other processes. The graphene quantum dot prepared by the method meets the actual quantum dot size requirement, has stable batch, uniform size distribution and high production efficiency, is suitable for industrial production, and has wide application prospects in the fields of photoelectric display devices, photovoltaic devices and biomedicine.
The present invention will be described in detail with reference to examples.
Example 1
(1) Single wall carbon nanotube oxidation
2 g single-wall carbon nano tube powder, 200 ml deionized water and 400 ml concentrated nitric acid are respectively added into a 1000 ml three-neck flask, uniformly stirred, and heated in a water bath at 80 ℃ for 3 h. After the water bath heating is completed, transferring the obtained single-walled carbon nanotube treatment liquid into 8 50 ml centrifuge tubes, centrifuging at 8000 rpm, pouring out the upper liquid, re-dispersing the precipitate into deionized water, and repeatedly centrifuging until the pH value of the upper liquid is 6-7. And (3) drying the treated single-walled carbon nanotubes in vacuum to obtain carboxylated single-walled carbon nanotube powder.
(2) Cutting single-wall carbon nano tube
Placing the oxidized single-walled carbon nanotube powder into a quartz boat, transferring the quartz boat into a tubular muffle furnace, introducing inert gas (argon) at a flow rate of 50 cm/min, exhausting for 30min, removing air in the tubular muffle furnace, regulating the flow rate of the inert gas (argon) to 20 cm/min, rapidly heating to 1000 ℃, and performing constant-temperature treatment for 30min. Then cooling to 800 ℃, introducing water vapor with the quantity of 10% of inert gas (argon), reacting for 15 min at constant temperature, closing a muffle furnace, cooling to room temperature, and taking out the cut single-walled carbon nano short tube.
(3) Single-walled carbon nanotube cutting
Placing the cut carbon nano tube short tube into a fluidized bed reactor provided with a plasma generating device, exhausting for 30min at the flow rate of 100cm/min inert gas (argon), adjusting the flow rate of the inert gas (argon) to 60 cm/min after the air in the fluidized bed is completely removed, adjusting the positions of parallel electrodes to enable the parallel electrodes to be in the fluidized state range of the carbon nano tube short tube, starting a power supply, discharging at the frequency of 40KHz by using 5A current to generate electric arcs, ionizing the inert gas (argon) flow, closing the power supply after the inert gas (argon) plasma bombards the carbon nano tube short tube for 30min, continuously introducing the inert gas (argon) to the reactor, and taking out products in the reactor after the reactor is cooled to room temperature to obtain graphene quantum dot powder.
Example 2
(1) Single wall carbon nanotube oxidation
2 g single-wall carbon nano tube powder, 200 ml deionized water and 400 ml concentrated nitric acid are respectively added into a 1000 ml three-neck flask, uniformly stirred, and heated in a water bath at 80 ℃ for 3 h. After the water bath heating is completed, transferring the obtained single-walled carbon nanotube treatment liquid into 8 50 ml centrifuge tubes, centrifuging at 8000 rpm, pouring out the upper liquid, re-dispersing the precipitate into deionized water, and repeatedly centrifuging until the pH value of the upper liquid is 6-7. And (3) drying the treated single-walled carbon nanotubes in vacuum to obtain carboxylated single-walled carbon nanotube powder.
(2) Cutting single-wall carbon nano tube
Placing the oxidized single-walled carbon nanotube powder into a quartz boat, transferring the quartz boat into a tubular muffle furnace, introducing inert gas (argon) at a flow rate of 50 cm/min, exhausting for 30min, removing air in the tubular muffle furnace, regulating the flow rate of the inert gas (argon) to 20 cm/min, rapidly heating to 1000 ℃, and performing constant-temperature treatment for 30min. Then cooling to 800 ℃, introducing water vapor with the quantity of 10% of inert gas (argon), reacting for 15 min at constant temperature, closing a muffle furnace, cooling to room temperature, and taking out the cut single-walled carbon nano short tube.
(3) Single-walled carbon nanotube cutting
Placing the cut carbon nano tube short tube into a fluidized bed reactor provided with a plasma generating device, exhausting for 30min at the flow rate of 100cm/min inert gas (argon), adjusting the flow rate of the inert gas (argon) to 60 cm/min after the air in the fluidized bed is completely removed, adjusting the positions of parallel electrodes to enable the parallel electrodes to be in the fluidized state range of the carbon nano tube short tube, starting a power supply, discharging at the frequency of 13.56MHz by using 5A current to generate electric arcs, ionizing the flow of the inert gas (argon), closing the power supply after the inert gas (argon) plasma bombards the carbon nano tube short tube for 30min, continuously introducing the inert gas (argon) to the reactor, cooling to room temperature, and taking out products in the reactor to obtain graphene quantum dot powder.
Example 3
(1) Single wall carbon nanotube oxidation
2 g single-wall carbon nano tube powder, 200 ml deionized water and 400 ml concentrated nitric acid are respectively added into a 1000 ml three-neck flask, uniformly stirred, and heated in a water bath at 80 ℃ for 3 h. After the water bath heating is completed, transferring the obtained single-walled carbon nanotube treatment liquid into 8 50 ml centrifuge tubes, centrifuging at 8000 rpm, pouring out the upper liquid, re-dispersing the precipitate into deionized water, and repeatedly centrifuging until the pH value of the upper liquid is 6-7. And (3) drying the treated single-walled carbon nanotubes in vacuum to obtain carboxylated single-walled carbon nanotube powder.
(2) Cutting single-wall carbon nano tube
Placing the oxidized single-walled carbon nanotube powder into a quartz boat, transferring the quartz boat into a tubular muffle furnace, introducing inert gas (argon) at a flow rate of 50 cm/min, exhausting for 30min, removing air in the tubular muffle furnace, regulating the flow rate of the inert gas (argon) to 20 cm/min, rapidly heating to 1000 ℃, and performing constant-temperature treatment for 30min. Then cooling to 800 ℃, introducing water vapor with the quantity of 10% of inert gas (argon), reacting for 15 min at constant temperature, closing a muffle furnace, cooling to room temperature, and taking out the cut single-walled carbon nano short tube.
(3) Single-walled carbon nanotube cutting
Placing the cut carbon nano tube short tube into a fluidized bed reactor provided with a plasma generating device, exhausting for 30min at the flow rate of 100cm/min inert gas (argon), adjusting the flow rate of the inert gas (argon) to 60 cm/min after the air in the fluidized bed is completely removed, adjusting the positions of parallel electrodes to enable the parallel electrodes to be in the fluidized state range of the carbon nano tube short tube, starting a power supply, discharging at the frequency of 40KHz by 15A current to generate electric arcs, ionizing the inert gas (argon) flow, closing the power supply after the inert gas (argon) plasma bombards the carbon nano tube short tube for 30min, continuously introducing the inert gas (argon) to the reactor, and taking out products in the reactor after the reactor is cooled to room temperature to obtain graphene quantum dot powder.
Claims (7)
1. The preparation method of the graphene quantum dot is characterized by comprising the following steps of:
providing an initial carbon nanotube, and performing oxidation treatment on the initial carbon nanotube to obtain a first carbon nanotube;
calcining the first carbon nano tube to obtain a second carbon nano tube;
performing inert gas plasma treatment on the second carbon nano tube to obtain the graphene quantum dot;
the step of calcining the first carbon nanotubes comprises the following steps: performing first calcination treatment on the first carbon nano tube under the condition of inert gas; performing a second calcination treatment under the condition of a mixed atmosphere containing water vapor and inert gas;
after the first carbon nano tube is subjected to first calcination treatment under the condition of inert gas, continuously introducing inert gas and water vapor, and performing second calcination treatment under the condition of mixed atmosphere containing water vapor and inert gas, wherein the volumes of the water vapor and the inert gas are 100:5-20;
the temperature of the first calcination treatment is 800-1500 ℃;
the time of the first calcination treatment is 15-60 min;
the temperature of the second calcination treatment is 800-1000 ℃;
the second calcination treatment time is 10-30 min.
2. The method of claim 1, wherein the initial carbon nanotubes are single-walled carbon nanotubes.
3. The method of claim 1, wherein the graphene quantum dots have a size of 3-10 nm.
4. The preparation method of claim 1, wherein the graphene quantum dots are obtained by performing inert gas plasma treatment on the calcined carbon nanotubes under the condition that the second carbon nanotubes are in a fluidized state.
5. The method according to claim 4, wherein the second carbon nanotubes are placed in a fluidized bed reactor equipped with a plasma generator, a fluidized inert gas is introduced to convert the calcined carbon nanotubes into a fluidized state, and the second carbon nanotubes in the fluidized state are placed between a pair of electrodes of the plasma generator, and an inert gas plasma treatment is performed by applying an electric current.
6. The method according to claim 5, wherein the inert gas plasma treatment is performed by energizing the plasma generator at a power discharge frequency of 40KHz, 13.56MHz or 2.45 GHz; and/or the number of the groups of groups,
energizing to perform inert gas plasma treatment under the condition that the practical voltage of the plasma generating device is 380V and the discharge current is 5-20A; and/or the number of the groups of groups,
the flow speed of the flowing inert gas is 50-100 cm/min; and/or the number of the groups of groups,
the time for carrying out inert gas plasma treatment is 30-60 min; and/or the number of the groups of groups,
the pair of electrodes are parallel electrodes, and the distance between the two electrodes is 2-20 mm.
7. The method according to claim 1, wherein the second carbon nanotube is subjected to an inert gas plasma treatment selected from the group consisting of an argon plasma treatment, a helium plasma treatment, a neon plasma treatment, a krypton plasma treatment, and a xenon plasma treatment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910074574.6A CN111484004B (en) | 2019-01-25 | 2019-01-25 | Preparation method of graphene quantum dots |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910074574.6A CN111484004B (en) | 2019-01-25 | 2019-01-25 | Preparation method of graphene quantum dots |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111484004A CN111484004A (en) | 2020-08-04 |
| CN111484004B true CN111484004B (en) | 2023-05-09 |
Family
ID=71796193
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910074574.6A Active CN111484004B (en) | 2019-01-25 | 2019-01-25 | Preparation method of graphene quantum dots |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111484004B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114348992B (en) * | 2021-12-15 | 2024-01-19 | 中国科学院金属研究所 | Method for efficiently and controllably chopping carbon nano tube in gas phase |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102616770A (en) * | 2012-03-28 | 2012-08-01 | 福州大学 | Method for preparing grapheme nano belts by etching carbon nano tubes through water vapor |
| CN103738941A (en) * | 2013-11-14 | 2014-04-23 | 盐城增材科技有限公司 | Graphene quantum dot preparation method |
| WO2017077381A2 (en) * | 2016-11-17 | 2017-05-11 | Research Institute Of Petroleum Industry (Ripi) | Formulation for the synthesis of thermal nanofluid based on carbon nanodots |
-
2019
- 2019-01-25 CN CN201910074574.6A patent/CN111484004B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102616770A (en) * | 2012-03-28 | 2012-08-01 | 福州大学 | Method for preparing grapheme nano belts by etching carbon nano tubes through water vapor |
| CN103738941A (en) * | 2013-11-14 | 2014-04-23 | 盐城增材科技有限公司 | Graphene quantum dot preparation method |
| WO2017077381A2 (en) * | 2016-11-17 | 2017-05-11 | Research Institute Of Petroleum Industry (Ripi) | Formulation for the synthesis of thermal nanofluid based on carbon nanodots |
Non-Patent Citations (1)
| Title |
|---|
| 胡超凡.石墨烯量子点.《光学功能化石墨烯基纳米材料》.2016,第38-39页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111484004A (en) | 2020-08-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Chen et al. | Oxygen functionalization of multiwall carbon nanotubes by Ar/H2O plasma treatment | |
| JP7156648B2 (en) | Carbon nanostructured material and method of forming carbon nanostructured material | |
| US20150135993A1 (en) | Treating Particles | |
| Choi et al. | Bandgap engineering of nanosized carbon dots through electron-accepting functionalization | |
| CN108821331A (en) | A kind of preparation method and product of gallium oxide nanometer rods | |
| CN111484004B (en) | Preparation method of graphene quantum dots | |
| WO2017196198A2 (en) | Process, reactor and system for fabrication of freestanding two-dimensional nanostructures using plasma technology | |
| JP5732636B2 (en) | Method for producing aligned carbon nanotubes | |
| CN106115639A (en) | A kind of crimping blade shape nano lamellar g C3n4preparation method | |
| JP2006036593A (en) | Method and apparatus for manufacturing monolayer carbon nanotube | |
| JP2006070089A (en) | Environment-preservative nano silicon solution and nano silicon powder, and manufacturing method of the same | |
| JP3372751B2 (en) | Field electron emission device and method of manufacturing the same | |
| CN108033443A (en) | A kind of method that combination of ultrasound microwave prepares graphene quantum dot | |
| JP5449987B2 (en) | Method for concentrating semiconducting single-walled carbon nanotubes | |
| JP5032042B2 (en) | Plasma CVD apparatus and film forming method | |
| JP4863590B2 (en) | Carbon nanotube modification method, carbon nanotube and electron emission source | |
| JP3952476B2 (en) | Single-walled carbon nanotube and method for producing the same | |
| CN111441106A (en) | Method for preparing high-quality graphene fibers by high-energy microwave irradiation | |
| CN110627038A (en) | Method for preparing carbon tube by arc discharge and chemical purifying carbon tube | |
| JP2006305554A (en) | Method of forming catalyst and method of manufacturing carbon film using the same | |
| CN113462384B (en) | Method for preparing fluorescent carbon quantum dots by gas-liquid two-phase plasma technology | |
| Wu et al. | Increasing the semiconducting component in transparent conducting films of single-walled carbon nanotubes | |
| CN113697812B (en) | Preparation method of silicon carbide nanotube based on high-frequency electromagnetic field excitation | |
| CN117049520B (en) | Wall number regulating and controlling method of carbon nano tube, single-wall carbon nano tube and preparation method thereof | |
| Shen et al. | Selective removal of metallic single-walled carbon nanotubes by microwave-assisted treatment of SWCNTs with nitronium ions |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information | ||
| CB02 | Change of applicant information |
Address after: 516006 TCL science and technology building, No. 17, Huifeng Third Road, Zhongkai high tech Zone, Huizhou City, Guangdong Province Applicant after: TCL Technology Group Co.,Ltd. Address before: 516006 Guangdong province Huizhou Zhongkai hi tech Development Zone No. nineteen District Applicant before: TCL Corp. |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant |