AU2021106570A4 - Preparation method of graphene nanoribbon/single walled carbon nanotube intramolecular heterojunction - Google Patents
Preparation method of graphene nanoribbon/single walled carbon nanotube intramolecular heterojunction Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 239000002109 single walled nanotube Substances 0.000 title claims abstract description 83
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 45
- 239000002074 nanoribbon Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 32
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 23
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 13
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 claims abstract description 12
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229960001149 dopamine hydrochloride Drugs 0.000 claims abstract description 11
- 229920001690 polydopamine Polymers 0.000 claims abstract description 11
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 8
- 238000006722 reduction reaction Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 35
- 230000008018 melting Effects 0.000 claims description 27
- 238000002844 melting Methods 0.000 claims description 27
- 229940071870 hydroiodic acid Drugs 0.000 claims description 8
- 239000007853 buffer solution Substances 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000007865 diluting Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 8
- 239000000872 buffer Substances 0.000 abstract description 6
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 229910000043 hydrogen iodide Inorganic materials 0.000 abstract 1
- 239000002041 carbon nanotube Substances 0.000 description 25
- 229910021393 carbon nanotube Inorganic materials 0.000 description 25
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 238000003756 stirring Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000002071 nanotube Substances 0.000 description 5
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 230000003628 erosive effect Effects 0.000 description 3
- 238000009830 intercalation Methods 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- 150000003624 transition metals Chemical class 0.000 description 3
- 238000001237 Raman spectrum Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 229960003638 dopamine Drugs 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 238000001020 plasma etching Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- -1 trihydroxymethyl Chemical group 0.000 description 1
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- 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
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
- C01B32/174—Derivatisation; Solubilisation; Dispersion in solvents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
- C01B32/158—Carbon nanotubes
- C01B32/159—Carbon nanotubes single-walled
-
- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/02—Single-walled nanotubes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/17—Nanostrips, nanoribbons or nanobelts, i.e. solid nanofibres with two significantly differing dimensions between 1-100 nanometer
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a method for preparing a graphene nanoribbon/single-wall carbon
nanotube intramolecular heterojunction, and belongs to the technical field of carbon
nanomaterials. The preparation method includes the following steps: (1) adding single-walled
carbon nanotubes and dopamine hydrochloride to Tris-HCl buffer, reacting in a dark
environment, and filtering to obtain polydopamine-modified single-walled carbon nanotubes;
(2) dispersing the poly-dopamine modified single-walled carbon nanotubes prepared in step
(1) in concentrated sulfuric acid, adding phosphoric acid, heating, adding potassium
permanganate, cooling to room temperature after the reaction is completed, adding hydrogen
peroxide, filtering, and washing with water to neutrality to obtain the melted single-walled
carbon nanotubes; (3) roasting the melted single-walled carbon nanotube obtained in the step
(2), ultrasonically treating the roasted product with hydrochloric acid solution, filtering, adding
hydrogen iodide solution for reduction reaction, and filtering after reaction to prepare the
graphene nanoribbon/single-walled carbon nanotube intramolecular heterojunction.
Description
Preparation method of graphene nanoribbon/single-walled carbon nanotube
intramolecular heterojunction
The invention relates to the technical field of carbon nano materials, in particular
to a preparation method of a graphene nanoribbon/single-walled carbon nanotube
intramolecular heterojunction.
With the development of miniaturization of electronic devices, silicon-based
semiconductor devices have approached their material and physical limits.
Carbon-based molecular devices are gradually considered as the best choice to replace
silicon-based electronic devices. New carbon-based materials, such as graphene and
carbon nanotubes, they are becoming the main force in manufacturing the next
generation of new electronic device materials because of their excellent physical
properties. In recent years, the composite material of graphene and carbon nanotubes
has attracted more and more attention, because it not only has various excellent
properties of graphene and carbon nanotubes, but also shows excellent physical and
chemical properties that graphene and carbon nanotubes do not have, and has been
successfully applied to capacitors, optoelectronic devices, energy storage batteries,
electrochemical sensors and other fields.
The intramolecular heterojunction of graphene nanoribbons (GNR) and
single-walled carbon nanotubes (SWCNT) has been widely studied because of its
unique photoelectric characteristics, which has many potential applications in the future. GNR is a kind of material which depends heavily on width and edge.
According to width and edge, GNR can be either metallic or semiconducting.
According to the difference of chirality, SWCNT can be either metallic or
semiconducting. The flexible adjustability makes the heterojunction composed of
SWCNT and GNR have a good application in the field of devices.
The existing methods for preparing GNR include intercalation stripping melting
carbon nanotubes, chemical erosion melting carbon nanotubes, sonochemical melting
carbon nanotubes, plasma etching melting carbon nanotubes, electrochemical etching
melting carbon nanotubes and transition metal catalytic melting carbon nanotubes.
Among them, plasma etching melting carbon nanotubes method, electrochemical
etching melting carbon nanotubes method and transition metal catalytic melting
carbon nanotubes method have complex steps and high requirements for equipment;
Intercalation stripping melting carbon nanotube method, chemical erosion melting
carbon nanotube method and sonochemical melting carbon nanotube method have
low requirements on equipment, however, there are various shortcomings in the
prepared GNR. For example, the method of intercalating, stripping and melting
carbon nanotubes and the method of chemically eroding and melting carbon
nanotubes will destroy the structure of GNR, resulting in the decrease of its electrical
properties. Although the GNR prepared by sonochemical melting carbon nanotubes
has high performance, the yield is very low, only about 2%. In addition, only
transition metal catalyzed melting of carbon nanotubes can control the degree of
melting of carbon nanotubes. Therefore, it is of great significance for the field to provide a preparation method of graphene nanoribbons/single-walled carbon nanotubes intramolecular heterojunction which is simple and can control the degree of melting.
The purpose of the invention is to provide a preparation method of graphene
nanoribbons/single-walled carbon nanotubes intramolecular heterojunction, which can
prepare graphene nanoribbons/single-walled carbon nanotubes intramolecular
heterojunction with controllable melting degree by a simple method, and has low
requirements on equipment in the preparation process, thus being convenient for
popularization and application of the preparation method.
To achieve the above purpose, the present invention provides the following
technical scheme:
According to one technical scheme of the invention, a preparation method of
graphene nanoribbons/single-walled carbon nanotubes intramolecular heterojunction
is provided, which comprises the following steps:
(1) adding single-walled carbon nanotubes and dopamine hydrochloride into
Tris-HCl buffer solution, reacting in a dark environment, and filtering to obtain
poly-dopamine modified single-walled carbon nanotubes;
(2) dispersing the polydopamine modified single-walled carbon nanotubes
prepared in step (1) in sulfuric acid solution, adding concentrated phosphoric acid,
heating up, adding potassium permanganate, cooling to room temperature after the
reaction is finished, adding hydrogen peroxide, filtering, washing with water to neutrality, and obtaining melted single-walled carbon nanotubes;
(3) roasting the melted single-walled carbon nanotube obtained in step (2),
ultrasonically treating the roasted product with hydrochloric acid solution, filtering,
adding hydroiodic acid solution for reduction reaction, and filtering after reaction to
obtain the graphene nanoribbon/single-walled carbon nanotube intramolecular
heterojunction.
Preferably, the mass ratio of the single-walled carbon nanotube to the dopamine
hydrochloride in step (1) is 1: (0.01-0.2); the mass-volume ratio of the single-walled
carbon nanotube to the Tris-HCl buffer solution is Ig: (10-15) L; the Tris-HCl buffer
solution is prepared by uniformly mixing 10ml of0.1mol/1 trimethylaminomethane
solution with 8ml of 0.1mol/1 hydrochloric acid, and then diluting with water to
1OOOmL.
Preferably, the reaction time in the dark environment in step (1) is 18-24h.
Preferably, the mass-volume ratio of the polydopamine modified single-walled
carbon nanotubes, sulfuric acid solution and concentrated phosphoric acid in step (2)
is Ig: (200-300) ml: (30-35) ml; The sulfuric acid solution is an aqueous sulfuric acid
solution with a mass fraction of 4 0 - 5 0 %.
Preferably, the temperature rise in step (2) is the temperature rise to 75-80°C; the
mass ratio of the potassium permanganate to the polydopamine-modified
single-walled carbon nanotubes is 1:(2-3); the reaction time is 2-3h.
Preferably, it is characterized in that the hydrogen peroxide in step (2) is a 30%
hydrogen peroxide aqueous solution.
Preferably, it is characterized in that the hydrochloric acid solution in step (3) is
an aqueous hydrochloric acid solution with pH=3.0-3.5.
Preferably, the temperature at which the melting single-walled carbon nanotubes
are calcined in step (3) is 450 to 5000C, and the time is 1.5 to 2 h.
Preferably, the hydroiodic acid solution in step (3) is a hydroiodic acid aqueous
solution with a mass fraction of 55-60%; the reduction reaction time is 6-8h.
The second technical scheme of the present invention is to provide a graphene
nanoribbon/single-walled carbon nanotube intramolecular heterojunction prepared
according to the above preparation method.
The beneficial technical effects of the present invention are as follows:
According to the invention, the modified part of the single-walled carbon
nanotube is protected from melting by modifying the poly dopamine, and the
modified degree of the single-walled carbon nanotube can be controlled by
controlling the dosage of dopamine hydrochloride, thereby achieving the effect of
controlling the melting degree of the intramolecular heterojunction of graphene
nanoribbons/single-walled carbon nanotubes.
At the same time, the single-walled carbon nanotubes oxidized and melted by
potassium permanganate were reduced by hydriodic acid solution, and the electrical
properties of the prepared graphene nanoribbons/single-walled carbon nanotubes
intramolecular heterojunction were improved by repairing the edge defects of GNR.
The preparation method provided by the invention has simple steps, and the
prepared graphene nanoribbon/single-walled carbon nanotube intramolecular heterojunction has controllable melting degree and excellent performance; meanwhile, the preparation process has low requirements on equipment, and the disclosed preparation method is convenient for popularization and application.
Various exemplary embodiments of the present invention will now be described
in detail, which should not be regarded as a limitation of the present invention, but
rather as a more detailed description of certain aspects, characteristics and
embodiments of the present invention. It should be understood that the terms
described in the present invention are only for describing specific embodiments, and
are not intended to limit the present invention.
In addition, as for the numerical range in the present invention, it should be
understood that every intermediate value between the upper limit and the lower limit
of the range is also specifically disclosed. Intermediate values within any stated value
or stated range and every smaller range between any other stated value or
intermediate values within the stated range are also included in the present invention.
The upper and lower limits of these smaller ranges can be independently included or
excluded from the range.
Unless otherwise stated, all technical and scientific terms used herein have the
same meanings as commonly understood by those skilled in the art to which the
present invention relates. Although the present invention only describes preferred
methods and materials, any methods and materials similar or equivalent to those
described herein may be used in the practice or testing of the present invention.
As used herein, "including", "comprising", "having", "containing", etc. are all
open terms, which means including but not limited to.
Embodiment 1
The preparation of graphene nanoribbon/single-walled carbon nanotube
intramolecular heterojunction comprises the following steps:
(1) Ig of single-walled carbon nanotubes andO.Olg of dopamine hydrochloride
are added into 10L Tris-HCl buffer (the preparation method of Tris-HCl buffer is as
follows: 100ml of 0.1mol/1 trimethylaminomethane solution is mixed with 80ml of
O.1mol/1 hydrochloric acid, and then diluted to 10L with water). Uniformly stirring,
reacting in a dark environment for 24 hours, filtering, washing the filter residue with
deionized water to be neutral, and drying at 80 DEG C to prepare the polydopamine
modified single-walled carbon nanotube;
(2) taking 0.2g of the polydopamine modified single-walled carbon nanotube
prepared in the step (1), dispersing in 60mL of sulfuric acid aqueous solution with the
mass fraction of 50%, dropwise adding 7mL of concentrated phosphoric acid, stir
uniformly, heat up to 75°C, add 0.5g potassium permanganate, react for 2.5h, cool to
room temperature, add dropwise 300mL of 30% hydrogen peroxide, filter, the filter
residue was washed with deionized water to neutrality, dried at 80°C, and melted
single-walled carbon nanotubes were prepared;
(3) Take 0.1g of the melted single-walled carbon nanotube prepared in step (2),
calcinate at 500°C for 2h, take it out and cool to room temperature, add 50 mL of a
pH 3.0 hydrochloric acid solution, sonicate for 15 minutes, filter, and wash the filter residue with deionized water until it is neutral. The filter residue was added to 50 mL of 60% hydroiodic acid solution and reduced for 8 hours. After the reaction was completed, filter and wash the filter residue. Dry at 80°C to prepare graphene nanoribbons/single-walled carbon nanotube intramolecular heterojunction.
Embodiment 2
The difference from Example 1 is that the amount of dopamine hydrochloride
added in step (1) is adjusted to 0.1 g.
Embodiment 3
The difference from Example 1 is that the amount of dopamine hydrochloride
added in step (1) is adjusted to 0.2g.
Embodiment 4
To prepare graphene nanoribbons/single-walled carbon nanotube intramolecular
heterojunction, the steps are as follows:
(1) Take Ig of single-walled carbon nanotubes and 0.2g of dopamine
hydrochloride and add them to 15L Tris-HCl buffer (the preparation method of
Tris-HCl buffer is: uniformly mixing 150ml of 0.1mol/1 trihydroxymethyl
aminomethane solution with 120ml of 0.1mol/1 hydrochloric acid, and diluting with
water to 15L); stir uniformly, react for 18 hours in a dark environment, filter, wash the
filter residue with deionized water to neutrality, and dry at 80°C to obtain
polydopamine-modified single-walled carbon nanotubes;
(2) Take 0.2 g of the polydopamine-modified single-walled carbon nanotubes
prepared in step (1) and disperse it in 60 mL of a 40% aqueous sulfuric acid solution, and add 6 mL of concentrated phosphoric acid dropwise. Stir uniformly, heat up to
°C, add 0.6g potassium permanganate, react for 2h, cool to room temperature, add
dropwise 300mL of 30% hydrogen peroxide, filter, and wash the filter residue with
deionized water until neutral, drying at 80°C to obtain melted single-walled carbon
nanotubes;
(3) Take O.1g of the melted single-walled carbon nanotube prepared in step (2),
roast it at 500°C for 1.5h, take it out and cool it to room temperature, add 50mL of pH
3.5 hydrochloric acid solution, ultrasound for 15 minutes, filter, wash the filter residue
with deionized water to neutrality, add the filter residue to 50 mL of a 55% hydroiodic
acid solution and reduce it for 8 hours. After the reaction is completed, the filter
residue is filtered, washed, and dried at 80°C, to prepare the graphene
nanoribbons/single-walled carbon nanotube intramolecular heterojunction.
Embodiment 5
To prepare graphene nanoribbons/single-walled carbon nanotube intramolecular
heterojunction, the steps are as follows:
(1) Ig of single-walled carbon nanotubes and 0.2g of dopamine hydrochloride
are added into 15 L Tris-HC buffer solution (the preparation method of Tris-HCl
buffer solution is as follows: 150ml ofO.1mol/1 trimethylaminomethane solution is
mixed with 120ml of 0.1mol/1 hydrochloric acid, and then diluted to 15L with water),
stir uniformly, react in a dark environment for 20 hours, filter, wash the filter residue
with deionized water to neutrality, and dry at 80°C to prepare polydopamine-modified
single-walled carbon nanotubes;
(2) Take 0.2 g of the polydopamine-modified single-walled carbon nanotubes
prepared in step (1), disperse it in 40mL of 50% sulfuric acid aqueous solution, and
add 7mL of concentrated phosphoric acid dropwise. Stir evenly, warm up to 80°C, add
0.4g potassium permanganate, react for 3h, cool to room temperature, add dropwise
300mL of 30% hydrogen peroxide, filter, wash the filter residue with deionized water
to neutrality, and dry at 80°C, the melted single-walled carbon nanotubes are
prepared;
(3) Take 0.1g of the melted single-walled carbon nanotube prepared in step (2),
roast it at 400°C for 2h, take it out and cool to room temperature, add 50mL of a pH
3.5 hydrochloric acid solution, ultrasound for 15 minutes, filter, wash the filter residue
with deionized water to neutrality, add the filter residue to 50 mL of 60% hydroiodic
acid solution and reduce it for 6 hours. After the reaction is completed, the filter
residue is filtered, washed, and dried at 80°C, the graphene nanoribbons/single-walled
carbon nanotube intramolecular heterojunction is prepared.
Comparative Example 1
The difference from Example 1 is that the step of reducing with a hydroiodic
acid solution in step (3) is omitted.
The intramolecular heterojunctions of graphene nanoribbons/single-walled
carbon nanotubes prepared in embodiments 1-5 and Comparative Example 1, and the
single-walled carbon nanotubes and GNR used in the present invention were
characterized by Raman spectrum analyzer. Integrate the D peak at 1329cm-1 and the
G peak at 1584cm-1 of the Raman spectrum respectively, expressed as ID and IG. The
D peak intensity of pure single-walled carbon nanotubes is extremely low. As the
graphene nanoribbons in the intramolecular heterojunction of graphene
nanoribbons/single-wall carbon nanotubes increase, the intensity of the D peak also
increases. Therefore, by calculating ID/IG, the degree of melting of the graphene
nanoribbons/single-walled carbon nanotubes intramolecular heterojunction in the
sample can be reflected, and the calculation results are shown in Table 1.
Table 1 ID/IG Single wall carbon 0.05 nanotube GNR 0.43 Embodiment 1 0.36 Embodiment 2 0.22 Embodiment 3 0.13 Embodiment 4 0.13 Embodiment 5 0.12 Comparative 0.35 Example 1 It can be seen from Table 1 that the technical scheme of the present invention can
prepare graphene nanoribbons/single-walled carbon nanotube intramolecular
heterojunctions. At the same time, as the amount of dopamine hydrochloride increases,
the amount of polydopamine-coated single-walled carbon nanotubes also increases.
The content of graphene nanoribbons in the prepared graphene
nanoribbons/single-wall carbon nanotube intramolecular heterojunction changes
accordingly. Therefore, by changing the mass ratio of the single-walled carbon
nanotubes to the dopamine hydrochloride, the degree of melting of the single-walled
carbon nanotubes can be controlled.
The mobility of the graphene nanoribbons/single-walled carbon nanotube
intramolecular heterojunctions prepared in Embodiment 1 and Comparative Example
1 of the present invention was measured by the carrier measurement method, and the
measurement results are shown in Table 2.
Table 2
Comparative Embodiment 1 Example 1 Mobility (cm 2 V-'s-') 1305 1221
It can be seen from Table 2 that the electrical properties of the intramolecular
heterojunction of graphene nanoribbons/single-walled carbon nanotubes can be
improved by oxidizing and melting the single-walled carbon nanotubes with
potassium permanganate and then reducing them with hydroiodic acid solution.
The above embodiments only describe the preferred mode of the invention, but
do not limit the scope of the invention. On the premise of not departing from the
design spirit of the invention, various modifications and improvements made by
ordinary technicians in the field to the technical scheme of the invention shall fall
within the protection scope determined by the claims of the invention.
Claims (10)
1. A preparation method of graphene nanoribbon/single-walled carbon nanotube
intramolecular heterojunction, characterized by comprising the following steps:
(1) adding single-walled carbon nanotubes and dopamine hydrochloride into
Tris-HCl buffer solution, reacting in a dark environment, and filtering to obtain
poly-dopamine modified single-walled carbon nanotubes;
(2) dispersing the polydopamine modified single-walled carbon nanotubes
prepared in step (1) in sulfuric acid solution, adding concentrated phosphoric acid,
heating up, adding potassium permanganate, cooling to room temperature after the
reaction is finished, adding hydrogen peroxide, filtering, washing with water to
neutrality, and obtaining melted single-walled carbon nanotubes;
(3) roasting the melted single-walled carbon nanotube obtained in step (2),
ultrasonically treating the roasted product with hydrochloric acid solution, filtering,
adding hydroiodic acid solution for reduction reaction, and filtering after the reaction
to prepare the graphene nanoribbon/single-walled carbon nanotube intramolecular
heterojunction.
2. The preparation method of graphene nanoribbon/single-walled carbon
nanotube intramolecular heterojunction according to claim 1, characterized in that, in
the step (1), the mass ratio of the single-walled carbon nanotube to the dopamine
hydrochloride is 1: (0.01-0.2); the mass-volume ratio of the single-walled carbon
nanotube to the Tris-HCl buffer solution is Ig: (10-15) L; the Tris-HCl buffer solution
is prepared by uniformly mixing 10 ml of 0.1 mol/ trimethylaminomethane solution with 8ml of 0.1mol/1 hydrochloric acid, and then diluting with water to 1000 mL.
3. The preparation method of graphene nanoribbon/single-walled carbon
nanotube intramolecular heterojunction according to claim 1, which is characterized
in that the reaction time in the dark environment in step (1) is 18-24 h.
4. The preparation method of graphene nanoribbon/single-walled carbon
nanotube intramolecular heterojunction according to claim 1, characterized in that, the
mass and volume ratio of the polydopamine modified single-walled carbon nanotubes,
sulfuric acid solution and concentrated phosphoric acid in step (2) is ig: (200-300) ml:
(30-35) ml; The sulfuric acid solution is an aqueous sulfuric acid solution with a mass
fraction of 40-50%.
5. The preparation method of graphene nanoribbon/single-walled carbon
nanotube intramolecular heterojunction according to claim 1, characterized in that, the
temperature rise in step (2) is the temperature rise to 75-80°C; the mass ratio of the
potassium permanganate to the polydopamine-modified single-walled carbon
nanotube is 1:(2-3); the reaction time is 2-3h.
6. The method for preparing graphene nanoribbons/single-walled carbon
nanotube intramolecular heterojunction according to claim 1, characterized in that: in
step (2), the hydrogen peroxide is an aqueous solution of hydrogen peroxide with a
mass fraction of 30%.
7. The method for preparing graphene nanoribbons/single-walled carbon
nanotube intramolecular heterojunction according to claim 1, it is characterized in that
the hydrochloric acid solution in step (3) is an aqueous hydrochloric acid solution with pH=3.0-3.5.
8. The method for preparing graphene nanoribbons/single-walled carbon
nanotube intramolecular heterojunction according to claim 1, characterized in that: in
step (3), the melting temperature of the single-walled carbon nanotubes is calcined at
450 to 500°C, and the time is 1.5 to 2 hours.
9. The method for preparing graphene nanoribbons/single-walled carbon
nanotube intramolecular heterojunction according to claim 1, characterized in that in
step (3), the hydroiodic acid solution is an aqueous solution of hydroiodic acid with a
mass fraction of 55-60%; the reduction reaction time is 6-8h.
10. A graphene nanoribbon/single-walled carbon nanotube intramolecular
heterojunction prepared according to the preparation method of any one of claims 1-9.
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| CN114907613B (en) * | 2022-03-23 | 2023-10-31 | 上海工程技术大学 | Carbon nano tube/polydopamine-reduced graphene oxide/three-dimensional interconnected porous silicon rubber composite material, and preparation method and application thereof |
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