CN110203911A - A kind of graphene fiber and preparation method - Google Patents
A kind of graphene fiber and preparation method Download PDFInfo
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- CN110203911A CN110203911A CN201910619443.1A CN201910619443A CN110203911A CN 110203911 A CN110203911 A CN 110203911A CN 201910619443 A CN201910619443 A CN 201910619443A CN 110203911 A CN110203911 A CN 110203911A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- 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
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
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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
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
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Abstract
The present invention relates to a kind of graphene fiber and preparation methods, and generally, the present invention is using graphene oxide colloid as presoma, using hydro-thermal reaction, and handled by drying at room temperature, obtain a kind of graphene fiber that conductivity is controllable, modification scope 345.58-443.41S/m.The invention reside in propose a kind of lamella size by regulating and controlling oxidation of precursor graphene, by one-dimensional limited hydro-thermal assemble method, without adding reducing agent, binder and other conductive materials, the graphene fiber that conductivity is controllable, regular gully pattern is presented in surface can be prepared by.This method preparation cost is cheap, and favorable repeatability, operating process is simple, and impurity introduces few.The graphene fiber prepared has broad application prospects in the fields such as energy storage and conversion, bio-medical, environmental protection and multifunctional material.
Description
Technical field:
The present invention relates to a kind of graphene fiber that conductivity is controllable and preparation methods, and generally, the present invention is with oxygen
Graphite alkene colloid is presoma, is handled using hydro-thermal reaction, and by drying at room temperature, obtains that diameter dimension is uniform, surface is in
The conductivity of the graphene fiber of existing parallel orientation gender gap gully structure, graphene fiber can be by changing stannic oxide/graphene nano
The lateral dimension of piece regulates and controls.
Background technique:
Since Geim in 2004 et al. obtains single-layer graphene for the first time from pyrolytic graphite with adhesive tape stripping method, graphite
Alkene is with its unique two-dimensional nanostructure and excellent physical chemistry and biological property, increasingly in physics, chemistry, material
Cause concern in the fields such as, biology.Graphene fiber (including graphene oxide fiber or redox graphene fiber) is
Graphene-based nanometer sheet is not necessarily to carrier by the methods of wet spinning technology, film shrunk method, limited hydro-thermal method, template auxiliary
Under conditions of addition binder, in axial direction self assembly arranges the structure function of new generation one to form macroscopic three dimensional structure
Change carbon based fibers material；The excellent performance of graphene is transferred to graphene fiber, to obtain the characteristics such as high conductivity.With
Intrinsic graphene nanometer sheet is compared, and the graphene fiber of three-dimensional structure has the characteristics that lightweight, is easier to manipulation, is expected to possess single
Special nature not available for graphene nanometer sheet or traditional material.
The graphene nano fiber that the country is reported at present mostly uses electrospinning process to prepare, and also has using hydrothermal synthesis
Method prepares the report of redox graphene micrometer fibers, such as patent publication No. CN 106592007B: graphene micron is fine
Dimension, preparation method, nerve fiber bracket and repair system, it is consistent that rule is presented in prepared graphene-based micrometer fibers surface
Nano-porous structure, but do not have certain directionality；The raising of electric conductivity is by mixing conductive polymer poly ethylene two
Oxygen thiophene is realized.
The invention reside in a kind of lamella size by regulating and controlling oxidation of precursor graphene is proposed, restricted water supply by one-dimensional
Hot assemble method can be prepared by that conductivity is controllable, rule are presented in surface without adding reducing agent, binder and other conductive materials
The then graphene fiber of gully pattern.In summary the application field referred to, High conductivity graphene fiber proposed by the present invention
There is huge practical prospect.
Summary of the invention:
The invention proposes a kind of graphene fiber and preparation methods, compared with prior art, the outstanding advantages of this method
It is that the present invention is directly prepared using various sizes of stannic oxide/graphene nano piece not over means such as other compound or doping
The controllable micrometer fibers of conductivity, material preparation cost is cheap, and favorable repeatability, operating process is simple, and impurity introduces few.
Specific step is as follows for a kind of graphene fiber and preparation method:
1) improved Hummers method is used, graphite oxide colloid is prepared；
2) the graphite oxide colloid of 5-12mg/ml, ultrasonic disperse are configured using ultrapure water, time 20-100min is obtained
Uniformly mixed graphene oxide colloid；
3) graphene oxide colloid is injected to diameter with syringe is to close capillary in the capillary of 0.2-1.2mm,
Hydro-thermal reaction is carried out, then drying at room temperature obtains graphene fiber.
In the present invention, step 1) selection prepares the crystalline flake graphite of graphene oxide colloid, granularity 20-350 mesh.
In the present invention, step 2) ultrasonic power is 50-500w.
In the present invention, the hydro-thermal reaction time in step 3) is 30-480min.
In the present invention, graphene fiber drying is completed in a glass tube in step 3).
A kind of graphene fiber, which is characterized in that in conjunction with atomic force microscope, Fourier Transform Infrared Spectroscopy test, sweep
Retouch the electric conductivity of electron microscope observation and the linear voltammetric scan method measurement fiber of electrochemical workstation, graphene fiber diameter ruler
Very little distribution is uniform, and parallel orientation gender gap gully structure is presented in surface, and gully size and conductivity range can be by changing precursor oxygen
Graphite alkene lamella size regulation, stannic oxide/graphene nano piece with a thickness of 1nm within, the big minor control field of lamella be 2.12~
9.22 μm, for the range of gully size at 0.81~1.73 μm, conductivity range is 345.58~443.41S/m.
Detailed description of the invention:
Fig. 1 .1 and Fig. 1 .2 are the atomic force microscopy diagrams of graphene oxide presoma in embodiment.
Fig. 2 is graphene oxide presoma scanning electron microscope diagram in embodiment.
Fig. 3 .1 and Fig. 3 .2 are the scanning electron microscope diagrams on graphene fiber surface in embodiment.
Fig. 4 is graphene oxide presoma and graphene fiber Fourier Transform Infrared Spectroscopy figure in embodiment.
Fig. 5 is the graphene fiber VA characteristic curve measured with electrochemical workstation in embodiment.
Specific embodiment:
Embodiment:
A kind of graphene fiber and the experiment condition and parameter of preparation method are as follows:
1) 32 mesh crystalline flake graphite 2g are weighed, are poured into the 96ml concentrated sulfuric acid (98%wt), 2g sodium nitrate is added, is sufficiently stirred
Afterwards, after being slowly added to 12g potassium permanganate, ice-water bath processing is carried out, 90min is stirred, temperature is then risen to 35 DEG C, is stirred for
2h；280ml ultrapure water is slowly added in two times in above-mentioned mixed liquor, hydrogen peroxide (30%wt) to bubble-free is slowly added dropwise and produces
It is raw；Solution is after centrifuge high speed centrifugation, three times through 10% dilute hydrochloric acid eccentric cleaning, is finally cleaned using deionized water to pH value
It is in neutrality, obtains graphite oxide colloid.
2) it is diluted with ultrapure water, configures the graphite oxide colloid of 8mg/ml, choose 120w power, ultrasonic 30min obtains oxygen
Graphite alkene colloid.
3) graphene oxide colloid is injected to diameter with syringe is to close capillary both ends in the capillary of 1.0mm,
Hydro-thermal reaction is carried out, fiber room temperature is dried to obtain graphene fiber by time 120min.
The method lifted according to foregoing invention can prepare graphene fiber, its feature is as follows:
1) AFM Analysis is carried out to prepared stannic oxide/graphene nano piece.The result shows that graphene oxide
Lamella has apparent fold, as shown in Fig. 1 .1；Available graphene oxide layer thickness, about 1nm are few from Fig. 1 .2
Layer graphene oxide.
2) electron microscope observation, such as Fig. 2 are scanned to prepared stannic oxide/graphene nano piece.Statistical result table
Bright, graphene oxide particle size is 5.81 ± 3.42 μm.
3) electron-microscopic analysis is scanned to prepared graphene fiber.As can be seen that fiber is straight from Fig. 3 .1
Diameter is about 63.19 ± 1.32 μm；It can see the pleated structure of graphene oxide from Fig. 3 .2, and fiber surface presents and determines
To the gully pattern of arrangement, the size in gully is 1.70 ± 0.48 μm, and stannic oxide/graphene nano piece is regularly assembled into three
Tie up structure.
4) Fourier turn infrared is carried out to prepared graphene fiber and oxidation of precursor graphene.Such as
Shown in Fig. 4.Graphene oxide is respectively in 1050cm-1、1390cm-1、1630cm-1、1730cm-1Place have epoxy group stretching vibration peak,
Edge hydroxyl stretching vibration peak, C=C double bond peak, edge carboxyl stretching vibration peak；In contrast, the hydroxyl of graphene fiber, carboxylic
Peak position intensity where base and epoxy group weakens, and C=C key peak intensity then improves.It can be seen that it is subjected to thermal response of restricting water supply, forerunner
The oxygen-containing functional group of body graphene oxide has obtained part and has removed.
5) prepared graphene fiber is made into the electrode of 1cm long, using the linear voltammetric scan method of electrochemical workstation
Test its VA characteristic curve.The conductivity for calculating graphene fiber is 443.41S/m.
Claims (6)
1. a kind of graphene fiber, which is characterized in that in conjunction with atomic force microscope, Fourier Transform Infrared Spectroscopy test, scanning
Electron microscope observation and the linear voltammetric scan method test of electrochemical workstation, graphene fiber diameter size distribution is uniform, table
Parallel orientation gender gap gully structure is presented in face, and gully size and conductivity range can be by changing precursor graphene oxide layer ruler
Very little regulation, stannic oxide/graphene nano piece with a thickness of 1nm within, the big minor control field of lamella be 2.12~9.22 μm, gully ruler
Very little 0.81~1.73 μm, conductivity range is 345.58~443.41S/m.
2. a kind of preparation method of graphene fiber, which is characterized in that the invention includes the following steps:
1) improved Hummers method is used, graphite oxide colloid is prepared；
2) the graphite oxide colloid of 5-12mg/ml, ultrasonic disperse are configured using ultrapure water, time 20-100min is mixed
Uniform graphene oxide colloid；
3) graphene oxide colloid is injected to diameter with syringe is to close capillary in the capillary of 0.2-1.2mm, is carried out
Hydro-thermal reaction, temperature are 150-300 DEG C, and then drying at room temperature obtains graphene fiber.
3. a kind of preparation method of graphene fiber as claimed in claim 2, which is characterized in that step 1) selection prepares oxygen
The crystalline flake graphite of graphite alkene colloid, granularity 20-350 mesh.
4. a kind of preparation method of graphene fiber as claimed in claim 2, which is characterized in that step 2) ultrasonic power is
50-500w。
5. a kind of preparation method of graphene fiber as claimed in claim 2, which is characterized in that the hydro-thermal in step 3) is anti-
It is 30-480min between seasonable.
6. a kind of preparation method of graphene fiber as claimed in claim 2, which is characterized in that graphene is fine in step 3)
Dimension drying is completed in a glass tube.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115074865A (en) * | 2022-07-29 | 2022-09-20 | 青岛理工大学 | Graphene fiber preparation method, graphene fiber temperature sensor and application |
| CN116377616A (en) * | 2023-04-20 | 2023-07-04 | 吉林大学 | Graphene micro-nano structural fiber with antibacterial activity and preparation method thereof |
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| CN102583334A (en) * | 2012-01-19 | 2012-07-18 | 北京理工大学 | Preparation method for graphene fiber |
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| CN103966699A (en) * | 2014-01-14 | 2014-08-06 | 中国科学院上海应用物理研究所 | Preparation method of graphene fibers |
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2019
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| EP2837716A1 (en) * | 2013-04-10 | 2015-02-18 | Huawei Technologies Co., Ltd. | Graphene fiber and preparation method therefor |
| US20150111449A1 (en) * | 2013-10-21 | 2015-04-23 | The Penn State Research Foundation | Method for preparing graphene oxide films and fibers |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115074865A (en) * | 2022-07-29 | 2022-09-20 | 青岛理工大学 | Graphene fiber preparation method, graphene fiber temperature sensor and application |
| CN116377616A (en) * | 2023-04-20 | 2023-07-04 | 吉林大学 | Graphene micro-nano structural fiber with antibacterial activity and preparation method thereof |
| CN116377616B (en) * | 2023-04-20 | 2024-08-09 | 吉林大学 | Graphene micro-nano structural fiber with antibacterial activity and preparation method thereof |
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