CN110040719A - A kind of carbon nanotube and its preparation method and application grown on doped graphene matrix - Google Patents
A kind of carbon nanotube and its preparation method and application grown on doped graphene matrix Download PDFInfo
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- CN110040719A CN110040719A CN201910317688.9A CN201910317688A CN110040719A CN 110040719 A CN110040719 A CN 110040719A CN 201910317688 A CN201910317688 A CN 201910317688A CN 110040719 A CN110040719 A CN 110040719A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
- C01B32/16—Preparation
- C01B32/162—Preparation characterised by catalysts
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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
- C01B32/182—Graphene
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The present invention discloses the carbon nanotube and its preparation method and application grown on a kind of doped graphene matrix, and graphene can be automatically assembled into three-dimensional shape graphene in heating stirring, high-temperature process, improve specific surface area;The compound of carbon nanotube and three-dimensional grapheme is realized in the generation of the nickel simple substance catalyzing carbon nanotube generated in reaction, the advantages of by combining two kinds of materials, increases substantially chemical property;Experimental method is safe and non-toxic, low in cost, easy to operate, Yi Shixian and can prepare uniform nanocomposite.Carbon nanotube is grown on prepared doped graphene matrix, can be applied in lithium ion battery, the fields such as supercapacitor and electro-catalysis, method of the invention has broad application prospects.
Description
Technical field
The present invention relates to carbon nanomaterial field, in particular to the carbon nanotube that is grown on a kind of doped graphene matrix and
Preparation method and application.
Background technique
Graphene becomes due to its high electron conduction, good mechanical property and chemical stability, big specific surface area
The only choosing of carbon material.Exotic atom adulterates the application problem that can effectively solve graphene, introduces defect to provide active site.
So increasing active site using the three-dimensional grapheme of N, S codope.The hollow structure of carbon nanotube, hole and tool between managing
Some faults of construction can provide transport channel and memory space abundant for lithium ion, have good embedding lithium characteristic.This
Outside, carbon nanotube has good mechanical property, electrochemical stability can be improved, to improve the chemical property of battery.
If graphene and carbon nanotube progress is compound, their excellent properties can be made full use of, graphene can be carbon nanometer
Pipe provides good support platform, and carbon nanotube can serve as the effect of support for graphene sheet layer, reduce the stacking of lamella.
Summary of the invention
Present invention aims at be to provide carbon nanotube grown on a kind of doped graphene matrix and preparation method thereof and
Using, preparation method is safe and non-toxic, and it is low in cost, it is easy to operate;The carbon nanotube of preparation can be in lithium ion battery, super capacitor
The application of the fields such as device and electro-catalysis.
To achieve the above object, the technical solution adopted by the present invention is that:
A kind of carbon nanotube and its preparation method and application grown on doped graphene matrix, comprising the following steps:
The preparation of the first step, presoma:
It disperses graphene oxide in enough deionized waters, ultrasonic vibration keeps graphene oxide evenly dispersed, obtains oxygen
Graphite alkene dispersion liquid, according to mass ratio 1:(0.3~2.5 of graphene oxide, melamine, trithiocyanuric acid, nickel nitrate):
(0.4~3.5): melamine powder is added to graphene dispersing solution in (1~10), and oil bath stirs evenly, and three polysulfides are then added
The ethanol solution oil bath of cyanic acid stirs evenly, and is eventually adding nickel nitrate and stirs evenly, and freeze-drying obtains presoma;
Second step, heat treatment:
The resulting presoma of the first step is heat-treated, is placed in tube furnace under inert gas protection, with 5~10
DEG C/min is warming up to 600~1000 DEG C, 2~6h is kept the temperature, natural cooling is under protective atmosphere up to carbon nanotube.
Further, the graphene oxide be scattered in graphene oxide dispersion concentration obtained in deionized water be 3~
10mg/ml。
Further, second used in deionized water used in graphene oxide dispersion and configuration trithiocyanuric acid ethanol solution is configured
The volume ratio of alcohol is (1~4): 1.
Further, in the first step triple mixing whipping temp be 60~120 DEG C, each mixing time be 30~
60min。
A kind of application of carbon nanotube as electrode material.
Advantageous effect of the invention is embodied in:
The present invention is by stirring and nickel is catalyzed carbon source generation carbon pipe for subsequent high-temperature calcination and graphene progress is compound,
The carbon nanotube grown on doped graphene matrix is obtained, graphene can primary reconstruction in heating stirring, heat treatment process
At three-dimensional shape graphene, specific surface area is improved;Carbon nanometer is realized in the generation of the nickel simple substance catalyzing carbon nanotube generated in reaction
Pipe is compound with three-dimensional grapheme, by increasing substantially chemical property in conjunction with the advantages of two kinds of materials;Experimental method safety
It is nontoxic, it is low in cost, it is easy to operate, at low cost, Yi Shixian and uniform nanocomposite can be prepared.Prepared mixes
Carbon nanotube is grown in miscellaneous graphene base body, it can be in lithium ion battery, the application of the fields such as supercapacitor and electro-catalysis, this hair
The method of bright offer has broad application prospects.
Detailed description of the invention
Fig. 1 is scanning electron microscopy (SEM) photograph that carbon nanotube is grown on doped graphene matrix prepared by embodiment 2
Piece;
Specific embodiment
Present invention is further described in detail combined with specific embodiments below, but not as a limitation of the invention.
Embodiment 1
(1) it prepares precursor: first dispersing 0.1g graphene oxide in 25ml deionized water, ultrasonic vibration 4h makes
Graphene oxide evenly spreads out to obtain graphene oxide dispersion, then be added 0.06g melamine, 80 DEG C of oil baths stir to
It is completely dissolved, obtains A liquid;Separately 0.17g trithiocyanuric acid is taken to be dissolved in 25ml ethyl alcohol, after obtain B liquid;B liquid is slowly added to A liquid
In, 0.1g nickel nitrate is added after 80 DEG C of oil bath stirring 30min, freeze-drying obtains presoma.
(2) prepared by heat treatment grows carbon nanotube on doped graphene matrix: presoma being placed in tube furnace, is passed to lazy
Property gas shield, is warming up to 650 DEG C of heat preservation 2h with the heating rate of 5 DEG C/min, natural cooling is under protective atmosphere up to carbon nanometer
Pipe.
Embodiment 2
(1) it prepares precursor: first dispersing 0.09g graphene oxide in 30ml deionized water, ultrasonic vibration 4h makes
Graphene oxide evenly spreads out to obtain graphene oxide dispersion, and 0.125g melamine, 80 DEG C of oil bath stirrings are then added
To being completely dissolved, A liquid is obtained;Separately 0.315g trithiocyanuric acid is taken to be dissolved in 25ml ethyl alcohol, after obtain B liquid;B liquid is slowly added to
In A liquid, 0.2g nickel nitrate is added after 80 DEG C of oil bath stirring 60min, freeze-drying obtains presoma.
(2) prepared by heat treatment grows carbon nanotube on doped graphene matrix: presoma being placed in tube furnace, is passed to lazy
Property gas shield, is warming up to 700 DEG C of heat preservation 2h with the heating rate of 5 DEG C/min, natural cooling is under protective atmosphere up to carbon nanometer
Pipe.
Referring to Fig.1, Fig. 1 is the SEM photograph that the present embodiment prepares sample, scans electricity with the S-4800 type of Japan Electronics Corporation
Sub- microscope (SEM) carries out morphology observation, can significantly see the three-dimensional graphite assembled by the graphene of nanometer grade thickness
Alkene, short texture, carbon nanotube are staggeredly grown in graphene base body, and graphene provides the platform of support for carbon nanotube, is
Carbon nano electronic transmitting provides channel, and carbon nanotube is also the effect that graphene sheet layer serves as support.
Embodiment 3
(1) it prepares precursor: first dispersing 0.2g graphene oxide in 60ml deionized water, obtain graphene oxide
Then 0.5g melamine is added in dispersion liquid, 100 DEG C of oil baths are stirred to being completely dissolved, and obtains A liquid;Separately take tri- polysulfide cyanogen of 0.6g
Acid is dissolved in 25ml ethyl alcohol, after obtain B liquid;B liquid is slowly added in A liquid, 0.4g nitre is added after 120 DEG C of oil bath stirring 30min
Sour nickel, freeze-drying, obtains presoma.
(2) prepared by heat treatment grows carbon nanotube on doped graphene matrix: presoma being placed in tube furnace, is passed to lazy
Property gas shield, is warming up to 800 DEG C of heat preservation 2h with the heating rate of 10 DEG C/min, natural cooling is under protective atmosphere up to carbon nanometer
Pipe.
Embodiment 4
(1) it prepares precursor: first dispersing 0.3g graphene oxide in 75ml deionized water, obtain graphene oxide
Then 0.452g melamine is added in dispersion liquid, 80 DEG C of oil baths are stirred to being completely dissolved, and obtains A liquid;Separately take tri- polysulfide of 0.354g
Cyanic acid is dissolved in 25ml ethyl alcohol, after obtain B liquid;B liquid is slowly added in A liquid, 1.5g nitre is added after 80 DEG C of oil bath stirring 60min
Sour nickel, freeze-drying, obtains presoma.
(2) prepared by heat treatment grows carbon nanotube on doped graphene matrix: presoma being placed in tube furnace, is passed to lazy
Property gas shield, is warming up to 800 DEG C of heat preservation 3h with the heating rate of 10 DEG C/min, natural cooling is under protective atmosphere up to carbon nanometer
Pipe.
Embodiment 5
(1) it prepares precursor: first dispersing 0.5g graphene oxide in 100ml deionized water, obtain graphite oxide
Alkene dispersion liquid, is then added 0.526g melamine, and 80 DEG C of stirrings obtain A liquid to being completely dissolved;Separately take tri- polysulfide cyanogen of 0.777g
Acid is dissolved in 25ml ethyl alcohol, after obtain B liquid;B liquid is slowly added in A liquid, 2g nickel nitrate is added after 80 DEG C of stirring 60min, it is cold
It is lyophilized dry, obtains presoma.
(2) prepared by heat treatment grows carbon nanotube on doped graphene matrix: presoma being placed in tube furnace, is passed to lazy
Property gas shield, is warming up to 900 DEG C of heat preservation 2h with the heating rate of 5 DEG C/min, natural cooling is under protective atmosphere up to carbon nanometer
Pipe.
Embodiment 6
(1) it prepares precursor: first dispersing 0.4g graphene oxide in 80ml deionized water, obtain graphene oxide
Dispersion liquid, is then added 0.25g melamine, and 80 DEG C of stirrings obtain A liquid to being completely dissolved;Separately take 0.35g trithiocyanuric acid molten
In 25ml ethyl alcohol, after obtain B liquid;B liquid is slowly added in A liquid, 3.0g nickel nitrate, freezing are added after 120 DEG C of stirring 60min
It is dry, obtain presoma.
(2) prepared by heat treatment grows carbon nanotube on doped graphene matrix: presoma being placed in tube furnace, is passed to lazy
Property gas shield, is warming up to 1000 DEG C of heat preservation 2h with the heating rate of 10 DEG C/min, natural cooling is received under protective atmosphere up to carbon
Mitron.
Embodiment 7
(1) it prepares precursor: first dispersing 0.5g graphene oxide in 50ml deionized water, obtain graphene oxide
Dispersion liquid, is then added 0.15g melamine, and 60 DEG C of stirring 60min obtain A liquid to being completely dissolved;Separately take tri- polysulfide cyanogen of 0.2g
Acid is dissolved in 25ml ethyl alcohol, after obtain B liquid;B liquid is slowly added in A liquid, 5g nickel nitrate is added after 120 DEG C of stirring 30min, it is cold
It is lyophilized dry, obtains presoma.
(2) prepared by heat treatment grows carbon nanotube on doped graphene matrix: presoma being placed in tube furnace, is passed to lazy
Property gas shield, is warming up to 600 DEG C of heat preservation 6h with the heating rate of 8 DEG C/min, natural cooling is under protective atmosphere up to carbon nanometer
Pipe.
Finally it should be noted that: the above examples are only used to illustrate the technical scheme of the present invention rather than its limitations, to the greatest extent
Pipe is described the invention in detail referring to above-described embodiment, it should be understood by those ordinary skilled in the art that: still may be used
With modifications or equivalent substitutions are made to specific embodiments of the invention, and repaired without departing from any of spirit and scope of the invention
Change or equivalent replacement, should all cover in present claims range.
Claims (6)
1. the carbon nanotube and its preparation method and application grown on a kind of doped graphene matrix, it is characterised in that including following
Step:
The preparation of the first step, presoma:
It disperses graphene oxide in enough deionized waters, ultrasonic vibration keeps graphene oxide evenly dispersed, obtains oxidation stone
Black alkene dispersion liquid, according to mass ratio 1:(0.3~2.5 of graphene oxide, melamine, trithiocyanuric acid, nickel nitrate): (0.4
~3.5): melamine powder is added to graphene dispersing solution in (1~10), and oil bath stirs evenly, and trithiocyanuric acid is then added
Ethanol solution oil bath stir evenly, be eventually adding nickel nitrate and stir evenly, freeze-drying obtain presoma;
Second step, heat treatment:
The resulting presoma of the first step is heat-treated, is placed in tube furnace under inert gas protection, with 5~10 DEG C/min
600~1000 DEG C are warming up to, 2~6h is kept the temperature, natural cooling is under protective atmosphere up to carbon nanotube.
2. according to the method described in claim 1, it is characterized by: the graphene oxide is scattered in obtained in deionized water
Graphene oxide dispersion concentration is 3~10mg/ml.
3. according to the method described in claim 1, it is characterized by: configuring deionized water used in graphene oxide dispersion and matching
The volume ratio for setting ethyl alcohol used in trithiocyanuric acid ethanol solution is (1~4): 1.
4. according to the method described in claim 1, it is characterized by: in the first step triple mixing whipping temp be 60~
120 DEG C, each mixing time is 30~60min.
5. the carbon nanotube grown on a kind of doped graphene matrix of the method preparation of any one according to claim 1~4.
6. a kind of application of the carbon nanotube described in claim 5 as electrode material.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105000548A (en) * | 2014-04-22 | 2015-10-28 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of novel three-dimensional nitrogen doped graphene composite material system |
CN105214701A (en) * | 2015-10-10 | 2016-01-06 | 浙江大学 | Iron-carbonide catalyst that in a kind of CNT of aromatic nitro compound hydrogenation, Graphene wraps up and preparation method thereof |
CN106629668A (en) * | 2016-12-27 | 2017-05-10 | 江汉大学 | Preparation method of three-dimensional-structure graphene/carbon nanotube hybrid carbon material |
CN108470890A (en) * | 2018-03-15 | 2018-08-31 | 陕西科技大学 | A kind of application of the preparation method of nitrogen sulphur codope three-dimensional grapheme, its product and the product that prepare |
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2019
- 2019-04-19 CN CN201910317688.9A patent/CN110040719A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105000548A (en) * | 2014-04-22 | 2015-10-28 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of novel three-dimensional nitrogen doped graphene composite material system |
CN105214701A (en) * | 2015-10-10 | 2016-01-06 | 浙江大学 | Iron-carbonide catalyst that in a kind of CNT of aromatic nitro compound hydrogenation, Graphene wraps up and preparation method thereof |
CN106629668A (en) * | 2016-12-27 | 2017-05-10 | 江汉大学 | Preparation method of three-dimensional-structure graphene/carbon nanotube hybrid carbon material |
CN108470890A (en) * | 2018-03-15 | 2018-08-31 | 陕西科技大学 | A kind of application of the preparation method of nitrogen sulphur codope three-dimensional grapheme, its product and the product that prepare |
Non-Patent Citations (1)
Title |
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狄沐昕等: "钴/氮掺杂碳纳米管/石墨烯复合材料的构筑及氧还原催化性能", 《高等学校化学学报》 * |
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Application publication date: 20190723 |