CN104649260A - Preparation method of graphene nano fibers or nanotubes - Google Patents
Preparation method of graphene nano fibers or nanotubes Download PDFInfo
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- CN104649260A CN104649260A CN201510067911.0A CN201510067911A CN104649260A CN 104649260 A CN104649260 A CN 104649260A CN 201510067911 A CN201510067911 A CN 201510067911A CN 104649260 A CN104649260 A CN 104649260A
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Abstract
The invention discloses a preparation method of nano fibers or nanotubes. The preparation method comprises the following steps: preparing graphene oxide from natural graphite used as a raw material; ultrasonically dispersing the graphene oxide uniformly in a solvent to obtain a graphene oxide dispersion solution; adding a solute to obtain a mixed solution; and performing electro-spinning, pre-oxidation and carbonization, and then treating by adopting free ammonia to obtain the nano fibers or nanotubes, wherein the solvent is an organic solvent or water, when the solvent is the organic solvent, the added solute is polyacrylonitrile, and when the solvent is water, the added solute is a water-soluble macromolecular substance. The preparation method disclosed by the invention is simple in process and can be used for realizing unlimited link of graphene nano-sheets.
Description
Technical field
The invention belongs to the package technique field of graphene nanometer sheet, particularly the preparation method of a kind of graphene nano fiber or nanotube.
Background technology
Because Graphene has the physics-chem characteristic of a series of uniqueness, electronic mobility excellent under the physical strength of such as superelevation, high Young's modulus, room temperature, very high thermal conductivity, excellent optical absorption characteristic and the complete pressuretightness to any gas, be subject to extensive concern since AndreGeim and the Konstantin Novoselov of Univ Manchester UK in 2004 utilizes scotch tape to prepare.Graphene is more single as its structure formation of flaky material of a kind of two dimension, but multiple change can occur its macrostructure form, as the macrostructure of two-dimensional film and three-dimensional, has widened the Application Areas of Graphene.
Electrostatic spinning is a kind of novel spining technology, it develops based on the principle of charged liquid ionogen high-velocity jet in high tension electrostatic field, its core is charged liquid flow deformation in high tension electrostatic field, then solidify through melt cooling or solvent evaporates, thus obtain the submicron even fibrous material of Nano grade, have the advantages that cost is low, large quantities ofly can prepare nanofiber, being widely used in preparing high polymer nanometer fiber, is the focus of Recent study.But also report electrostatic spinning technique does not directly prepare the graphene nano fiber of continuous print, endless at present.This continuous fibre not only as the carrier of various catalyzer, and all can have great application prospect in the person in electronics such as nano-device, field emission effect.But so far but without utilizing electrostatic spinning technique to prepare the such technology report of graphene nano fiber.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide the preparation method of a kind of graphene nano fiber or nanotube, can make dispersion, the graphene nanometer sheet of shape irregularity at high temperature makes it be connected with each other by nitrogen-atoms, utilizes carbon nanofiber to become continuous print graphene nano fiber or nanotube as template simultaneously.
To achieve these goals, the technical solution used in the present invention is:
The preparation method of a kind of graphene nano fiber or nanotube, be that graphene oxide prepared by raw material with natural graphite, in solvent ultrasonic disperse evenly after obtain graphene oxide dispersion, add solute and obtain mixing solutions, after carrying out electrospinning, preoxidation, carbonization, ammonia process is adopted to obtain graphene nano fiber or nanotube, wherein said solvent is organic solvent or water, when for organic solvent, the solute added is polyacrylonitrile, when for water, the solute added is water-soluble high-molecular substance.
Described organic solvent is DMF or N,N-dimethylacetamide or the arbitrary proportion mixture of the two.
Described water-soluble high-molecular substance is polyvinyl alcohol, polyvinylpyrrolidone or hydroxypropylcellulose.
In the mixing solutions of described acquisition, the quality of graphene oxide accounts for 15 ~ 35% of total Solute mass, and the solution of the quality preparation different concns of adjustment solute and solvent, its concentration range is 8% ~ 20%.
Described electrospinning is that the mixing solutions electrospinning of described acquisition is become composite fiber precursor by high-voltage electrostatic spinning technology.Afterwards by electrospinning gained composite fiber precursor preoxidation 0 ~ 120 minute; 950 ~ 1100 DEG C are warming up under inert atmosphere protection; after constant temperature, pass into ammonia carry out reaction 10 ~ 60 minutes; reaction terminates rear closedown ammonia and furnace cooling after passing into rare gas element, and described rare gas element is nitrogen, argon gas or helium.
Described natural graphite is natural micro crystal graphite or natural flake graphite.
Compared with prior art, in step of the present invention, the concentration of solution and the relative content of GO have directly important impact to the diameter of graphene nano fiber, pattern.Because carbon nanofiber connects in the process of pipe at Graphene and serves template and confinement effect, so the diameter of nanofiber directly determines the diameter of graphene nano pipe, and the diameter of nanofiber is decided by the concentration of electrospun solution.Electrospun solution concentration is too low, and owing to cannot form the direct drip of charged drop at collecting board, strength of solution is too high, causes strength of solution to increase, and can resist the stretching of spinning jet.Summing up through test of many times can the upper limit of electrostatic spinning PAN strength of solution and lower limit, and general strength of solution can form comparatively uniform nano-fiber filaments 8% ~ 20%.
The compound precursor that electrospinning of the present invention obtains by after carbonizing treatment under high temperature, then adopts ammonia (NH
3) process.The main purpose introducing ammonia has two: the first to be that ammonia at high temperature (about 1000 DEG C) meeting have strong corrasion to the carbon nanofiber of polyacrylonitrile-radical, makes it consume further thus only retains the composition of Graphene; Second is that the introducing of ammonia simultaneously just can introduce a large amount of nitrogen (N) atoms, the carbon atom that first these nitrogen-atoms at high temperature comparatively can enliven with graphene edge place reacts, reaction result be the carbon atom that nitrogen-atoms will replace graphene edge place and comparatively enlivens, the carbon atom of its both sides is coupled together, simultaneously due to the confinement effect of carbon nanofiber, graphene sheet layer just can form graphene nano fiber or nanotube.
Accompanying drawing explanation
Fig. 1 is the microscopic sdIBM-2+2q.p.approach figure of graphene oxide.Fig. 1 a is transmission electron microscope (TEM) shape appearance figure of graphene oxide; Fig. 1 b is the atomic force microscope microscopic appearance figure of graphene oxide, can know the size finding out lamella.
Fig. 2 is the shape appearance figure after the composite nano fiber preoxidation of PAN and GO.
Fig. 3 is that composite nano fiber is through NH
3the SEM shape appearance figure of the graphene nano fiber obtained after process.Fig. 3 a is continuous graphite alkene nanofiber shape appearance figure, and 3c is the partial enlargement SEM shape appearance figure of 3d.Can find out through NH relative to Fig. 2
3after process, the diameter of graphene fiber declines all to some extent.
Fig. 4 is graphene nano pipe SEM shape appearance figure.The graphene nano pipe of Fig. 4 a to be the concentration of electrospun solution be diameter that 15wt% (PAN:0.7g+GO:0.3g+DMF:5.6g) prepares is approximately 400 ~ 500nm; Fig. 4 b is the partial enlargement shape appearance figure of Fig. 4 a.
Fig. 5 is transmission electron microscope (TEM) shape appearance figure of graphene nano pipe.Fig. 5 b is that the surface of 5a and edge high resolution TEM scheme.In Fig. 5 a, illustration is the selected area electron diffraction figure (SAD) of graphene nano tube-surface.
Embodiment
By the composite nano fiber regulating the concentration of electrospun solution can prepare different diameter, thus graphene nano fiber or the nanotube of different diameter can be obtained.Below in conjunction with following examples and accompanying drawing, the present invention is further described.
Embodiment one
The present embodiment comprises the following steps:
Step one, be raw material with natural flake graphite, adopt chemical method to obtain graphene oxide, then 0.24g graphene oxide is dissolved in 8.8gDMF and carries out supersound process and within 2 hours, obtain graphene oxide (GO) dispersion liquid.Fig. 1 is the microscopic sdIBM-2+2q.p.approach figure to GO.
The preparation of step 2, electrospun solution.Added by the PAN of 0.96g in above-mentioned mixing solutions and heat in the water-bath of 65 DEG C and stir 24 hours, namely this can form the electrospun solution of 12%.Wherein the quality of graphene oxide accounts for the massfraction of solute is 20%.
Step 3, gained solution electrostatic spinning is realized the preparation of nanofiber compound precursor, in electrostatic spinning process, voltage is 25kv, and the distance of syringe needle distance substrate is 25cm, and solution rate of feed is 1ml/h.
Step 4, the composite nano fiber precursor of preparation is carried out preoxidation, temperature is 280 DEG C, and the time is 2 hours.Fig. 2 is the shape appearance figure after the composite nano fiber preoxidation of PAN and GO.Afterwards the composite nano fiber after preoxidation is carried out carbonization and NH
3process obtains graphene nano fiber.Ammonia (NH
3) treatment condition: temperature 1000 DEG C, the time is 30min, can obtain graphene nano fiber after this end of processing.Fig. 3 is the SEM shape appearance figure of graphene nano fiber, can see that diameter is approximately 200 ~ 300nm.
Embodiment two
The present embodiment comprises the following steps:
Step one, be raw material with natural graphite, adopt chemical method to obtain graphene oxide, then 0.12g graphene oxide is dissolved in 3.9g water and carries out supersound process and obtain GO in 2 hours, and then ultrasonic disperse obtains graphene oxide (GO) dispersion liquid.
The preparation of step 2, electrospun solution.After the PVA of 0.22g added in above-mentioned dispersion liquid heat in the water-bath of 65 DEG C and stir 24 hours, namely this can form the electrospun solution of 8%.Wherein the quality of graphene oxide accounts for the massfraction of solute is 35%.
Step 3, gained solution electrostatic spinning is realized the preparation of nanofiber compound precursor, in electrostatic spinning process, voltage is 25kv, and the distance of syringe needle distance substrate is 25cm, and solution rate of feed is 1ml/h.
Step 4, the composite nano fiber precursor of preparation is carried out carbonization and NH
3process obtains graphene nano fiber.Ammonia (NH
3) treatment condition: temperature 950 DEG C, the time is 30min, can obtain graphene nano fiber after this end of processing.
Embodiment three
The present embodiment comprises the following steps:
Step one, with natural micro crystal graphite for raw material, adopt chemical method to obtain graphene oxide, then 0.3g graphene oxide be dissolved in 9g DMF and carry out supersound process and within 2 hours, obtain graphene oxide (GO) dispersion liquid.
The preparation of step 2, electrospun solution.Added by the PAN of 0.7g in above-mentioned dispersion liquid and heat in the water-bath of 65 DEG C and stir 24 hours, namely this can form the electrospun solution of 10%.
Step 3, gained solution electrostatic spinning is realized the preparation of nanofiber precursor, in electrostatic spinning process, voltage is 25kv, and the distance of syringe needle distance substrate is 25cm, and solution rate of feed is 1ml/h.
Step 4, the composite nano fiber precursor of preparation is carried out preoxidation, temperature is 280 DEG C, and the time is 1 hour.Afterwards the composite nano fiber after preoxidation is carried out carbonization and NH
3graphene nano pipe is prepared in process.Carbonization temperature is 1000 DEG C of times is 10min, and the atmosphere of tube furnace is nitrogen (N
2), carbonization process terminates rear horse back and carries out activation treatment: tube furnace is switched to ammonia (NH
3) atmosphere closes N simultaneously
2, temperature-resistant, soak time is 20min, can obtain graphene nano open tube after this end of processing.The SEM shape appearance figure of the graphene nano pipe that Fig. 4 a and 4b is strength of solution to be prepared when being 15%, can see that diameter is approximately 400 ~ 500nm.Fig. 5 is transmission electron microscope (TEM) shape appearance figure of graphene nano pipe.
Embodiment four
The present embodiment comprises the following steps:
Step one, be raw material with natural graphite, adopt chemical method to obtain graphene oxide, then 0.12g graphene oxide is dissolved in 5.8g water and carries out supersound process and obtain GO in 2 hours, and then ultrasonic disperse obtains graphene oxide (GO) dispersion liquid.
The preparation of step 2, electrospun solution.After the polyvinylpyrrolidone of 0.68g added in above-mentioned dispersion liquid heat in the water-bath of 65 DEG C and stir 24 hours, namely this can form the electrospun solution of 12%.Wherein the quality of graphene oxide accounts for the massfraction of solute is 15%.
Step 3, gained solution electrostatic spinning is realized the preparation of nanofiber compound precursor, in electrostatic spinning process, voltage is 25kv, and the distance of syringe needle distance substrate is 25cm, and solution rate of feed is 1ml/h.
Step 4, the composite nano fiber precursor of preparation carried out carbonization and NH3 process obtains graphene nano fiber.Ammonia (NH
3) treatment condition: temperature 950 DEG C, the time is 30min, can obtain graphene nano fiber after this end of processing.
Claims (7)
1. the preparation method of a graphene nano fiber or nanotube, it is characterized in that, be that graphene oxide prepared by raw material with natural graphite, in solvent ultrasonic disperse evenly after obtain graphene oxide dispersion, add solute and obtain mixing solutions, after carrying out electrospinning, preoxidation, carbonization, ammonia process is adopted to obtain graphene nano fiber or nanotube, wherein said solvent is organic solvent or water, when for organic solvent, the solute added is polyacrylonitrile, and when for water, the solute added is water-soluble high-molecular substance.
2. the preparation method of graphene nano fiber or nanotube according to claim 1, is characterized in that, described organic solvent is DMF or N,N-dimethylacetamide or the arbitrary proportion mixture of the two.
3. the preparation method of graphene nano fiber or nanotube according to claim 1, it is characterized in that, described water-soluble high-molecular substance is polyvinyl alcohol, polyvinylpyrrolidone or hydroxypropylcellulose.
4. the preparation method of graphene nano fiber or nanotube according to claim 1, it is characterized in that, in the mixing solutions of described acquisition, the quality of graphene oxide accounts for 15 ~ 35% of total Solute mass, the solution of the quality preparation different concns of adjustment solute and solvent, its concentration range is 8% ~ 20%.
5. the preparation method of graphene nano fiber or nanotube according to claim 1, it is characterized in that, described electrospinning is that the mixing solutions electrospinning of described acquisition is become composite fiber precursor by high-voltage electrostatic spinning technology.
6. the preparation method of graphene nano fiber or nanotube according to claim 1; it is characterized in that; by electrospinning gained composite fiber precursor preoxidation 0 ~ 120 minute; 950 ~ 1100 DEG C are warming up under inert atmosphere protection; after constant temperature, pass into ammonia carry out reaction 10 ~ 60 minutes; reaction terminates rear closedown ammonia and furnace cooling after passing into rare gas element, and described rare gas element is nitrogen, argon gas or helium.
7. the preparation method of graphene nano fiber or nanotube according to claim 1, it is characterized in that, described natural graphite is natural micro crystal graphite or natural flake graphite.
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Cited By (12)
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| CN105498821A (en) * | 2015-12-17 | 2016-04-20 | 苏州大学 | Composite material used for catalyzing and degrading nitrogen oxide and preparation method and application thereof |
| CN105776189A (en) * | 2016-01-30 | 2016-07-20 | 山西大学 | Method for preparing high-purity small oxidized graphene |
| CN106521719A (en) * | 2016-11-10 | 2017-03-22 | 过冬 | Graphene-based carbon nanofiber preparation method |
| CN106784683A (en) * | 2016-12-20 | 2017-05-31 | 中国科学技术大学 | Graphene composite nano-line, its preparation method and application |
| CN107082417A (en) * | 2017-06-06 | 2017-08-22 | 烟台市烯能新材料股份有限公司 | A kind of preparation method of low granularity graphene |
| CN107475793A (en) * | 2016-06-08 | 2017-12-15 | 南京理工大学 | A kind of preparation method of graphene oxide parcel polyacrylonitrile composite nano fiber |
| CN108163842A (en) * | 2018-01-23 | 2018-06-15 | 内蒙古农业大学 | A kind of preparation method and application of graphene nano pipe |
| CN108597889A (en) * | 2018-04-13 | 2018-09-28 | 北京化工大学 | A kind of transition metal hydrotalcite-reduced graphene nanotube fibers electrode material and preparation method thereof and a kind of ultracapacitor |
| CN109369185A (en) * | 2018-09-26 | 2019-02-22 | 南通大学 | A kind of preparation method of nitrogen-doped graphene complex carbon material |
| CN109423702A (en) * | 2017-09-05 | 2019-03-05 | 中国石油化工股份有限公司 | A kind of high-intensitive, graphene-based carbon fiber of high weight of hydrogen and preparation method thereof |
| CN110067035A (en) * | 2019-05-14 | 2019-07-30 | 中国科学院沈阳应用生态研究所 | A kind of electrostatic spinning and preparation method thereof of hydrophobic graphene composite high-molecular fiber |
| CN110760946A (en) * | 2019-11-07 | 2020-02-07 | 黑龙江黑大生物质新材料科技有限公司 | Graphene-based composite fiber, and preparation method and application thereof |
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Cited By (16)
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| US20170173571A1 (en) * | 2015-12-17 | 2017-06-22 | Soochow University | Composite material used for catalyzing and degrading nitrogen oxide and preparation method and application thereof |
| CN105498821B (en) * | 2015-12-17 | 2018-06-12 | 苏州大学 | It is a kind of for composite material of catalytic degradation nitrogen oxides and its preparation method and application |
| CN105498821A (en) * | 2015-12-17 | 2016-04-20 | 苏州大学 | Composite material used for catalyzing and degrading nitrogen oxide and preparation method and application thereof |
| US10441945B2 (en) * | 2015-12-17 | 2019-10-15 | Soochow University | Composite material used for catalyzing and degrading nitrogen oxide and preparation method and application thereof |
| CN105776189A (en) * | 2016-01-30 | 2016-07-20 | 山西大学 | Method for preparing high-purity small oxidized graphene |
| CN107475793A (en) * | 2016-06-08 | 2017-12-15 | 南京理工大学 | A kind of preparation method of graphene oxide parcel polyacrylonitrile composite nano fiber |
| CN106521719A (en) * | 2016-11-10 | 2017-03-22 | 过冬 | Graphene-based carbon nanofiber preparation method |
| CN106784683A (en) * | 2016-12-20 | 2017-05-31 | 中国科学技术大学 | Graphene composite nano-line, its preparation method and application |
| CN107082417A (en) * | 2017-06-06 | 2017-08-22 | 烟台市烯能新材料股份有限公司 | A kind of preparation method of low granularity graphene |
| CN109423702A (en) * | 2017-09-05 | 2019-03-05 | 中国石油化工股份有限公司 | A kind of high-intensitive, graphene-based carbon fiber of high weight of hydrogen and preparation method thereof |
| CN108163842A (en) * | 2018-01-23 | 2018-06-15 | 内蒙古农业大学 | A kind of preparation method and application of graphene nano pipe |
| CN108597889A (en) * | 2018-04-13 | 2018-09-28 | 北京化工大学 | A kind of transition metal hydrotalcite-reduced graphene nanotube fibers electrode material and preparation method thereof and a kind of ultracapacitor |
| CN108597889B (en) * | 2018-04-13 | 2019-11-15 | 北京化工大学 | A kind of transition metal hydrotalcite-reduced graphene nanotube fibers electrode material and preparation method thereof and a kind of supercapacitor |
| CN109369185A (en) * | 2018-09-26 | 2019-02-22 | 南通大学 | A kind of preparation method of nitrogen-doped graphene complex carbon material |
| CN110067035A (en) * | 2019-05-14 | 2019-07-30 | 中国科学院沈阳应用生态研究所 | A kind of electrostatic spinning and preparation method thereof of hydrophobic graphene composite high-molecular fiber |
| CN110760946A (en) * | 2019-11-07 | 2020-02-07 | 黑龙江黑大生物质新材料科技有限公司 | Graphene-based composite fiber, and preparation method and application thereof |
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Application publication date: 20150527 |