CN105129781A - Preparation method of graphene nanoribbon - Google Patents
Preparation method of graphene nanoribbon Download PDFInfo
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- CN105129781A CN105129781A CN201510491338.6A CN201510491338A CN105129781A CN 105129781 A CN105129781 A CN 105129781A CN 201510491338 A CN201510491338 A CN 201510491338A CN 105129781 A CN105129781 A CN 105129781A
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- mixed solution
- carbon nanotube
- sediment
- graphene nanobelt
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000002074 nanoribbon Substances 0.000 title abstract 5
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 31
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 19
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000006185 dispersion Substances 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims description 29
- 239000002127 nanobelt Substances 0.000 claims description 26
- 239000013049 sediment Substances 0.000 claims description 19
- 238000005119 centrifugation Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract 2
- 238000004108 freeze drying Methods 0.000 abstract 1
- 238000001132 ultrasonic dispersion Methods 0.000 abstract 1
- 238000000137 annealing Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000002048 multi walled nanotube Substances 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 239000002082 metal nanoparticle Substances 0.000 description 2
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 239000002079 double walled nanotube Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- -1 graphite alkene Chemical class 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000013528 metallic particle Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000817 safety factor Toxicity 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002109 single walled nanotube Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Abstract
The invention provides a preparation method of a graphene nanoribbon. The method includes: taking a carbon nanotube as the raw material, introducing ozone into a sulfuric acid dispersion liquid of carbon nanotube continuously, carrying out ultrasonic dispersion, centrifugal separation and freeze drying, thus obtaining the graphene nanoribbon. The method provided by the invention has the characteristics of simplicity, convenient operation and low production cost, can reduce the energy consumption of production, and is convenient for actual popularization and application in production. The graphene nanoribbon prepared by the method provided by the invention has complete structure and high electric conductivity, and can realize effective regulation of the graphene nanoribbon size by selecting carbon nanotubes of different tube diameters.
Description
Technical field
The invention belongs to carbon nanomaterial technical field, be specifically related to the preparation method of graphene nanobelt.
Background technology
Graphene (Graphene) refers to the graphite with a carbon atom thickness, by sp between C-C
2covalent linkage is hexagonal network aspect, decomposes the soccerballene that can become zero dimension, the curling carbon nanotube that can form one dimension, and superposition can form three-dimensional graphite.In order to give single-layer graphene, certain is electrical, according to special style cutting graphite alkene, can form graphene nanobelt (Graphenenanoribbon).According to the difference of graphene nano belt edge, graphene nanobelt can be divided into armchair and Z-type two kinds, and wherein Z-type nano belt is conductor, and armchair nano belt is semi-conductor.The structure of graphene nanobelt has high conductivity, high heat conductance, lower noise, and the another kind that these fine qualities impel graphene nanobelt to become integrated circuit interconnection material is selected, and likely substitutes copper metal.
The preparation method of existing graphene nanobelt, normally utilize metal nanoparticle can etch Graphene along preferential direction in annealing process, under described Graphene shape border confinement effect, metal nanoparticle is "the" shape track etching, thus forms graphene nanobelt and array thereof.Concrete implementation step comprises: (1) prepares Graphene on substrate; (2) at Graphene edge fixing metal particle; (3) at Ar
2/ H
2anneal in atmosphere, temperature remains on 700 DEG C ~ 1000 DEG C.The main drawback of the method is: technique relative complex, and the quality of the preparation of experiment mid-early stage Graphene and the preparation of metallic particles directly affects the quality of follow-up graphene nanobelt, there is larger randomness and uncertain factor; At Ar
2/ H
2atmosphere and temperature remains on 700 DEG C ~ 1000 DEG C annealing, the requirement for equipment is higher, production cost and energy consumption too high, and there is safety factors scarcely.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of graphene nanobelt.It is simple, easy to operate that the method has technique, and production cost is low, less demanding to experimental installation, is suitable for the advantages such as large-scale production.
The technical scheme adopted for realizing the object of the invention is such, and a kind of preparation method of graphene nanobelt, is characterized in that, comprises the following steps:
1) dispersion of carbon nanotube:
By carbon nanotube dispersed in the vitriol oil, obtain the carbon nano tube dispersion liquid A that carbon nanotube concentration is 1.0 ~ 5.0g/L;
2) ozone oxidation:
To step 1) continue to pass into ozone 1 ~ 2h in the carbon nano tube dispersion liquid A that obtains, and constantly stir, obtain mixing solutions B;
3) ultrasonic disperse:
By step 2) in gained mixing solutions B under ultrasonic output frequency is 100Hz ~ 5MHz, carry out ultrasonic disperse 30 ~ 60min, obtain mixed solution C;
4) centrifugation:
Adopt the method for centrifugation, from step 3) isolate solid sediment the mixed solution C that obtains;
5) lyophilize:
To step 4) add deionized water in the sediment collected, obtain mixed solution D, mixed solution D is carried out lyophilize and obtain pressed powder and be graphene nanobelt.
Further, step 1) in, described carbon nanotube is the carbon nanotube of single wall, double-walled or many walls.
Further, step 2) in, described ozone concn is 60 ~ 100%, and gas flow rate is: 0.1 ~ 5.0m
3/ h.
Further, step 4) in, mixed solution C, centrifugal 30 ~ 60min under rotating speed is 4000 ~ 10000rpm, carries out solid-liquid separation, collects sediment.
Further, step 5) in, after described sediment and ionized water mix, obtain mixed solution D through ultrasonic disperse, in mixed solution D, the concentration of described sediment is 1.0 ~ 5.0g/L.
After the present invention adopts technique scheme, mainly contain following effect:
(1) the inventive method prepare the size of graphene nanobelt can by effective adjustment of selecting the carbon nanotube of different tube diameters can realize graphene nanobelt size, this product has the performances such as high conductivity, high thermal conductivity, high electromagnetic wave absorbability;
(2) the inventive method only adopts mechanical stirring, ozone oxidation, ultrasonic disperse and centrifugation etc., and process is simple, and without the need to high temperature annealing, production energy consumption is low;
(3) present invention process is simple, and easy to operate, production unit is few, thus reduces production cost further, is convenient to actual applying, is suitable for large-scale production.
Accompanying drawing explanation
Fig. 1 is the multi-walled carbon nano-tubes raw material under scanning electronic microscope;
Fig. 2 is the graphene nanobelt (this patent method prepares) under scanning electronic microscope;
Fig. 3 is the Electronic Speculum figure that the graphene nanobelt in Fig. 2 is opened in longitudinal shear.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described, but should not be construed the above-mentioned subject area of the present invention and be only limitted to following embodiment.Without departing from the idea case in the present invention described above, according to ordinary skill knowledge and customary means, make various replacement and change, all should be included in protection scope of the present invention.
Embodiment 1:
1) dispersion of carbon nanotube:
Single Walled Carbon Nanotube being scattered in concentration is in the vitriol oil of 98%, obtains the carbon nano tube dispersion liquid A that carbon nanotube concentration is 1.0g/L;
2) ozone oxidation:
To step 1) continue to pass into ozone 1h in the carbon nano tube dispersion liquid A that obtains, and constantly stir, obtain mixing solutions B; Ozone concn is 100%, and flow velocity is: 0.1m
3/ h.
3) ultrasonic disperse:
By step 2) in gained mixing solutions B under ultrasonic output frequency is 5MHz, carry out ultrasonic disperse 30min, obtain mixed solution C;
4) centrifugation:
Adopt the method for centrifugation, from step 3) isolate solid sediment the mixed solution C that obtains; By mixed solution C centrifugal 3min under rotating speed is 10000rpm, carry out solid-liquid separation, collect sediment.
5) lyophilize:
Get step 4) collect sediment 10mg, add deionized water 10mL, ultrasonic disperse, obtain mixed solution D, mixed solution D is carried out lyophilize, obtain pressed powder and be graphene nanobelt.
Embodiment 2:
1) dispersion of carbon nanotube:
It is in the vitriol oil of 98% that multi-walled carbon nano-tubes (see Fig. 1) is scattered in concentration, obtains the carbon nano tube dispersion liquid A that carbon nanotube concentration is 5.0g/L;
2) ozone oxidation:
To step 1) continue to pass into ozone 2h in the carbon nano tube dispersion liquid A that obtains, and constantly stir, obtain mixing solutions B; Ozone concn is 60%, and flow velocity is: 5.0m
3/ h.
3) ultrasonic disperse:
By step 2) in gained mixing solutions B under ultrasonic output frequency is 5MHz, carry out ultrasonic disperse 60min, obtain mixed solution C;
4) centrifugation:
Adopt the method for centrifugation, from step 3) isolate solid sediment the mixed solution C that obtains; By mixed solution C centrifugal 30min under rotating speed is 4000rpm, carry out solid-liquid separation, collect sediment.
5) lyophilize:
Get step 4) collect sediment 150mg, add deionized water 30mL, ultrasonic disperse, obtain mixed solution D, mixed solution D is carried out lyophilize, obtain pressed powder and be graphene nanobelt.The Electronic Speculum figure of this graphene nanobelt is see Fig. 2.In addition, to be multi-walled carbon nano-tubes open from longitudinally carrying out shearing and obtain Fig. 3.
Embodiment 3:
1) dispersion of carbon nanotube:
Double-walled carbon nano-tube being scattered in concentration is in the vitriol oil of 98%, obtains the carbon nano tube dispersion liquid A that carbon nanotube concentration is 3.0g/L;
2) ozone oxidation:
To step 1) continue to pass into ozone 2h in the carbon nano tube dispersion liquid A that obtains, and constantly stir, obtain mixing solutions B; Ozone concn is 80%, and flow velocity is: 3m
3/ h.
3) ultrasonic disperse:
By step 2) in gained mixing solutions B under ultrasonic output frequency is 100Hz, carry out ultrasonic disperse 60min, obtain mixed solution C;
4) centrifugation:
Adopt the method for centrifugation, from step 3) isolate solid sediment the mixed solution C that obtains; By mixed solution C centrifugal 15min under rotating speed is 10000rpm, carry out solid-liquid separation, collect sediment.
5) lyophilize:
Get step 4) collect sediment 30mg, add deionized water 15mL, ultrasonic disperse, obtain mixed solution D, mixed solution D is carried out lyophilize, obtain pressed powder and be graphene nanobelt.
Claims (2)
1. a preparation method for graphene nanobelt, is characterized in that, comprises the following steps:
1) dispersion of carbon nanotube:
By carbon nanotube dispersed in the vitriol oil, obtain the carbon nano tube dispersion liquid A that carbon nanotube concentration is 1.0 ~ 5.0g/L;
2) ozone oxidation:
To step 1) continue to pass into ozone 1 ~ 2h in the carbon nano tube dispersion liquid A that obtains, and constantly stir, obtain mixing solutions B;
3) ultrasonic disperse:
By step 2) in gained mixing solutions B under ultrasonic output frequency is 100Hz ~ 5MHz, carry out ultrasonic disperse 30 ~ 60min, obtain mixed solution C;
4) centrifugation:
Adopt the method for centrifugation, from step 3) isolate solid sediment the mixed solution C that obtains;
5) lyophilize:
To step 4) add deionized water in the sediment collected, obtain mixed solution D, mixed solution D is carried out lyophilize and obtain pressed powder and be graphene nanobelt.
2. the preparation method of a kind of graphene nanobelt according to claim 1, is characterized in that:
Step 1) in, described carbon nanotube is the carbon nanotube of single wall, double-walled or many walls.
Step 2) in, described ozone concn is 60 ~ 100%, and gas flow rate is: 0.1 ~ 5.0m
3/ h.
Step 4) in, mixed solution C, centrifugal 10 ~ 30min under rotating speed is 4000 ~ 10000rpm, carries out solid-liquid separation, collects sediment.
Step 5) in, after described sediment and deionized water mix, obtain mixed solution D through ultrasonic disperse, in mixed solution D, the concentration of described sediment is 1.0 ~ 5.0g/L.
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|---|---|---|---|
| CN201510491338.6A CN105129781A (en) | 2015-08-10 | 2015-08-10 | Preparation method of graphene nanoribbon |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510491338.6A CN105129781A (en) | 2015-08-10 | 2015-08-10 | Preparation method of graphene nanoribbon |
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|---|---|
| CN105129781A true CN105129781A (en) | 2015-12-09 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101575095A (en) * | 2009-05-26 | 2009-11-11 | 北京大学 | Method for preparing graphene |
| CN103224227A (en) * | 2012-01-30 | 2013-07-31 | 深圳市润麒麟科技发展有限公司 | Microwave preparation method of graphene sheet and carbon nanotube/graphene sheet composite material |
| CN103359723A (en) * | 2012-04-05 | 2013-10-23 | 清华大学 | Preparation method of narrow graphene nanoribbons |
| CN103879991A (en) * | 2012-12-20 | 2014-06-25 | 海洋王照明科技股份有限公司 | Preparation method of graphene nanobelt |
| US20150013896A1 (en) * | 2013-07-12 | 2015-01-15 | Florida State University Research Foundation, Inc. | Graphene Nanoribbons and Methods |
| CN104709899A (en) * | 2013-12-17 | 2015-06-17 | 国家纳米科学中心 | Graphene nanoribbon carbon fiber and preparation method thereof |
-
2015
- 2015-08-10 CN CN201510491338.6A patent/CN105129781A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101575095A (en) * | 2009-05-26 | 2009-11-11 | 北京大学 | Method for preparing graphene |
| CN103224227A (en) * | 2012-01-30 | 2013-07-31 | 深圳市润麒麟科技发展有限公司 | Microwave preparation method of graphene sheet and carbon nanotube/graphene sheet composite material |
| CN103359723A (en) * | 2012-04-05 | 2013-10-23 | 清华大学 | Preparation method of narrow graphene nanoribbons |
| CN103879991A (en) * | 2012-12-20 | 2014-06-25 | 海洋王照明科技股份有限公司 | Preparation method of graphene nanobelt |
| US20150013896A1 (en) * | 2013-07-12 | 2015-01-15 | Florida State University Research Foundation, Inc. | Graphene Nanoribbons and Methods |
| CN104709899A (en) * | 2013-12-17 | 2015-06-17 | 国家纳米科学中心 | Graphene nanoribbon carbon fiber and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| DMITRY V. KOSYNKIN ET AL: "Longitudinal unzipping of carbon nanotubes to form graphene nanoribbons", 《NATURE》 * |
| KUN XU ET AL: "Theoretical Study on the Oxidation Mechanism and Dynamics of the Zigzag Graphene Nanoribbon Edge by Oxygen and Ozone", 《THE JOURNAL OF PHYSICAL CHEMISTRY C》 * |
| S.R. DHAKATE ET AL: "The production of multi-layer graphene nanoribbons from thermally reduced unzipped multi-walled carbon nanotubes", 《CARBON》 * |
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