CN109355799A - A kind of graphene fiber non-woven fabrics of N doping and preparation method thereof - Google Patents
A kind of graphene fiber non-woven fabrics of N doping and preparation method thereof Download PDFInfo
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- CN109355799A CN109355799A CN201811109168.0A CN201811109168A CN109355799A CN 109355799 A CN109355799 A CN 109355799A CN 201811109168 A CN201811109168 A CN 201811109168A CN 109355799 A CN109355799 A CN 109355799A
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- graphene
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- woven fabrics
- graphene fiber
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Classifications
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4209—Inorganic fibres
- D04H1/4242—Carbon fibres
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Nonwoven Fabrics (AREA)
- Artificial Filaments (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses graphene fiber non-woven fabrics of a kind of N doping and preparation method thereof, the graphene sheet layer for constituting graphene fiber contains a certain number of nitrogen heteroatom doping, and the graphene fiber non-woven fabrics of N doping can be obtained from fusion by graphene fiber, be conducive to improve hydrophily, electric conductivity and the electro-chemical activity of graphene fiber and its nonwoven fabric construct, therefore can be used for the high performance electrode material of aqueous electrolysis plastidome energy storage device.
Description
Technical field
The present invention relates to the graphene fiber non-woven fabrics of graphene fiber and fabric more particularly to a kind of nitrogen atom doping and
Preparation method.
Background technique
Graphene fiber non-woven fabrics be it is a kind of mutually merged by graphene fiber in fiber overlapped joints it is novel carbon-based
Fabric (Nature Communications, 2016,13684), the graphene fiber due to constituting non-woven fabrics are fused mutually
Effect is stronger, and significantly reduces interfibrous contact resistance, therefore this nonwoven cloth material has preferable stable structure
Property, the flexible and excellent performances such as conductive, thermally conductive are a kind of potential high performance electrode materials, can be used for super electricity
The energy storage devices such as container and battery field, especially shows biggish application prospect in flexible electronic device.
However, when graphene fiber non-woven fabrics is used as electrode material, in order to guarantee that higher electric conductivity and mechanics are stablized
Property, the structure of component units graphene fiber is comparatively dense, and the functional group of graphene sheet layer is less, and work is lacked in fiber skeleton
Property site, thus it is poor with the affinity of aqueous electrolyte, and the electro-chemical activity of non-woven fabrics electrode also receives a degree of
Limitation, constrains using graphene fiber non-woven fabrics as the raising of the electrochemical device performance of electrode.Nitrogen-atoms is carried out to carbon material
Doping be to improve a kind of common method of its hydrophily and electro-chemical activity, the graphene oxide fiber non-woven of N doping at present
The preparation of cloth is not seen in report.Technology path proposed by the present invention based on composite spinning and heat treatment can effectively be realized to stone
The N doping of black alkene fabric nonwoven cloth is conducive to improve its electro-chemical activity.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of graphene fiber nonwoven of nitrogen atom doping
Cloth and preparation method thereof.
The invention is realized by the following technical scheme: a kind of graphene fiber non-woven fabrics of N doping, by the graphite of 1-7mm
Alkene fiber passes through mutually to be formed by overlapping from fusion, and the graphene fiber is accumulated by the graphene film of nitrogen atom doping, nitrogen
Atom is connected in the form of covalent bond with the carbon atom of graphene；The doping of nitrogen-atoms is passed through by nitrogenous compound and graphene
Heat treatment is realized.
A kind of preparation method of the graphene fiber non-woven fabrics of N doping, comprising the following steps:
(1) continuous wet spinning is carried out by spinning solution of the graphene oxide dispersion containing nitrogenous compound.
(2) obtained graphene oxide/nitrogenous compound composite fibre is being placed at room temperature for 12h or more, then not high
3h is dried in vacuo at a temperature of 100 DEG C.
(3) dry composite fibre is dispersed in ethanol solution, and is blended growth using high shear homomixer
Degree is the staple fiber of 1-7mm, obtains the dispersion liquid of composite short fiber.
(4) deposited oxide graphene/nitrogenous compound composite short fiber on strainer, and be filtered by vacuum to drying, it obtains
Composite fibre nonwoven cloth.
(3) 600-1000 DEG C of heat treatment is carried out to composite fibre nonwoven cloth obtained, obtains the graphene fiber of N doping
Non-woven fabrics.
Further, the nitrogenous compound being added in spinning solution is polyvinylpyrrolidone, polyaniline, melamine, urine
Element etc. is water-soluble or the nitrogenous compound of n,N-Dimethylformamide solvent, and the mass fraction of nitrogenous compound is 10%-
50%.
Further, spinning solution is the aqueous solution or n,N-Dimethylformamide solution of graphene oxide.It is corresponding, it spins
The coagulating bath that silk process uses is calcium chloride/water/alcohol mixeding liquid or ethyl acetate.
Compared with the prior art, the present invention has the following beneficial effects:
(1) present invention constitutes non-woven fabrics, the graphene fiber as structural unit using the graphene staple fiber of N doping
Non-woven fabrics can be made to obtain better hydrophily, electric conductivity and more active sites after nitrogen atom doping, be conducive to it
Application in textile electrode.
(2) removing of nitrogenous compound can introduce micro- knots such as a large amount of micropores and fold for graphene fiber in composite fibre
Structure.Compared to conventional nitrogen-doped graphene film, non-woven fabrics has a porous reticular structure, and network skeleton itself have it is more
Micro-structure, the micro-structure of this specific surface area being obviously improved and multistage scale can greatly improve the electrochemistry of electrode material
Performance.
(3) mechanics that its network structure is maintained while graphene fiber non-woven fabrics electro-chemical activity is substantially improved is stablized
Property with it is flexible, be with a wide range of applications in flexible wearable energy storage device field.
(4) preparation method is simple, 600-1000 DEG C of high-temperature heat treatment process can a step realize graphene oxide layer
Reduction is to improve electric conductivity；Pass through the doping for reacting realization nitrogen-atoms of graphene sheet layer and polymer simultaneously.
Detailed description of the invention
Fig. 1 a is the graphene fiber nonwoven surface pattern of obtained N doping, and b is the scanning electron microscope of single fiber
Figure；
Fig. 2 is the x-ray photoelectron spectroscopy (XPS) of the graphene fiber non-woven fabrics of N doping.
Specific embodiment
The solution system that the present invention uses graphene oxide to be blended with polymer with nitrogen first prepares composite fibre, in spinning
Graphene oxide sheet and the evenly dispersed of polymer are the necessary conditions for guaranteeing fiberizing in liquid.Due to the composite fibre of preparation
Still there is stronger hydrophily, can be swollen in alcohol solvent, therefore assembling system can be merged by means of the wet process of fiber
Standby graphene oxide/polymer composite fibrous non-woven fabrics.Why need to obtain composite fibre nonwoven cloth first, purpose is then
The nitrogen-atoms for being used to adulterate is introduced by polymer and is stored in non-woven fabrics.And then hot place is carried out to composite fibre nonwoven cloth
Reason is to obtain the committed step of nitrogen-doped graphene fabric nonwoven cloth.During high-temperature heat treatment, one side graphite oxide
Alkene lamella is restored, and electric conductivity is provided with；On the other hand, polymer with nitrogen occurs with graphene sheet layer anti-at high temperature
It answers, nitrogen-atoms is connected in the form of covalent bond with the carbon atom of graphene, realizes doping of the nitrogen-atoms to graphene sheet layer, according to
According to the difference of itself and peripheral carbon atoms combination, the mode of N doping can be generally divided into pyridine nitrogen, pyrroles's nitrogen and graphite nitrogen.
Its electric conductivity can not only be promoted by carrying out N doping to graphene fiber non-woven fabrics, more can increase the hydrophilic of its surface
Property, improve the contact of graphene fiber non-woven fabrics electrode and water system electrolyte, reduces the internal resistance of electrochemical system, while nitrogen-atoms
The active site that can be used as electrode surface provides additional fake capacitance, further increases the chemical property of the electrode material.Separately
On the one hand, the nitrogenous compound of composite graphite alkene fiber decomposes removing at high temperature, can draw inside graphene fiber with surface
Enter the micro-structures such as a large amount of micropores and fold (as shown in Figure 1 b), dramatically increases the active surface area of the structure.Therefore, the present invention mentions
The method for preparing nitrogen-doped graphene fabric nonwoven cloth out is that one kind simply and efficiently obtains the effective of high performance electrode material
Approach.And N doping process can't significantly change the mechanical property of graphene fiber non-woven fabrics, to inherit this material
Good flexible characteristic makes it have biggish potential value in flexible energy storage device field.
The present invention is specifically described below by embodiment, the present embodiment is served only for doing further the present invention
It is bright, it should not be understood as limiting the scope of the invention, those skilled in the art makes one according to the content of foregoing invention
A little nonessential changes and adjustment, all belong to the scope of protection of the present invention.
Embodiment 1:
(1) using concentration for 5mg/mL graphene oxide/aqueous solution as spinning solution, wherein the poly- of mass fraction 10% is added
Vinylpyrrolidone, calcium chloride/water/alcohol mixeding liquid (mass ratio 20:300:100) are that coagulating bath carries out continuous wet spinning.
(2) obtained graphene oxide fiber is being placed at room temperature for 12h, then 100 DEG C at a temperature of be dried in vacuo 3h.
(3) dry composite fibre is dispersed in ethanol solution, and is blended using high shear homomixer, obtained
The dispersion liquid of staple fiber.
(4) it in filter deposited thereon composite short fiber, and is filtered by vacuum to drying, obtains graphene oxide/polyvinyl pyrrole
Alkanone composite fibre nonwoven cloth.
(5) 1000 DEG C of heat treatments are carried out to composite fibre nonwoven cloth obtained, obtains the graphene fiber nonwoven of N doping
Cloth.
Fig. 1 a is the graphene fiber nonwoven surface pattern of obtained N doping, and b is the scanning electron microscope of single fiber
Figure is mutually formed by overlapping it can be seen from the figure that being passed through by graphene fiber from fusion, and the graphene fiber is mixed by nitrogen-atoms
Miscellaneous graphene film is accumulated.Wherein nitrogen-atoms is connected in the form of covalent bond with the carbon atom of graphene, and nitrogen content is about
3%, as shown in the XPS spectrum figure of Fig. 2, the C1s spectrogram of non-woven fabrics contains the peak position that apparent C-N key generates, positioned at the position of 285eV
It sets；The 162F/g (0.1A/g) that the capacitance of the graphene fiber non-woven fabrics electrode never carries out N doping is promoted to 181F/g,
Improve about 11.7%.
Embodiment 2:
(1) using concentration for 5mg/mL graphene oxide/n,N-Dimethylformamide solution as spinning solution, wherein matter is added
The urea of score 10% is measured, ethyl acetate is that coagulating bath carries out continuous wet spinning.
(2) obtained graphene oxide fiber is placed at room temperature for 14h, is dried in vacuo 3h at a temperature of 100 DEG C.
(3) dry composite fibre is dispersed in ethanol solution, and is blended using high shear homomixer, obtained
The dispersion liquid of staple fiber.
(4) it in filter deposited thereon composite short fiber, and is filtered by vacuum to drying, obtains the compound fibre of graphene oxide/urea
Tie up non-woven fabrics.
(5) 800 DEG C of heat treatments are carried out to composite fibre nonwoven cloth obtained, obtains the graphene fiber nonwoven of N doping
Cloth.
By above step, obtained graphene fiber non-woven fabrics nitrogen content is about 6%, graphene fiber non-woven fabrics electrode
Capacitance be promoted to 210F/g from 153F/g (0.1A/g), improve about 37.2%.
Embodiment 3:
For step 1-5 with embodiment 2, the polymer being added in spinning solution is the melamine of mass fraction 5%, at final heat
Managing temperature is 1000 DEG C.Gained graphene fiber non-woven fabrics nitrogen content is about 3%.
The capacitance of the graphene fiber non-woven fabrics electrode is 184F/g (0.1A/g).
Embodiment 4:
For step 1-5 with embodiment 1, the polymer being added in spinning solution is the polyaniline of mass fraction 20%, at final heat
Managing temperature is 700 DEG C.Gained graphene fiber non-woven fabrics nitrogen content is about 4%.
The capacitance of the graphene fiber non-woven fabrics electrode is 192F/g (0.1A/g).
Claims (5)
1. a kind of graphene fiber non-woven fabrics of N doping, which is characterized in that passed through by the graphene fiber of 1-7mm from fusion phase
It is mutually formed by overlapping, the graphene fiber is accumulated by the graphene film of nitrogen atom doping, and nitrogen-atoms is in the form of covalent bond
It is connect with the carbon atom of graphene；The doping of nitrogen-atoms is realized by nitrogenous compound and graphene by heat treatment.
2. a kind of preparation method of the graphene fiber non-woven fabrics of N doping, which comprises the following steps:
(1) continuous wet spinning is carried out by spinning solution of the graphene oxide dispersion containing nitrogenous compound.
(2) obtained graphene oxide/nitrogenous compound composite fibre is placed at room temperature for 12h or more, is then not higher than 100
3h is dried in vacuo at a temperature of DEG C.
(3) dry composite fibre is dispersed in ethanol solution, and is blended into length using high shear homomixer and is
The staple fiber of 1-7mm obtains the dispersion liquid of composite short fiber.
(4) deposited oxide graphene/nitrogenous compound composite short fiber on strainer, and be filtered by vacuum to drying, it obtains compound
Fabric nonwoven cloth.
(3) 600-1000 DEG C of heat treatment is carried out to composite fibre nonwoven cloth obtained, obtains the graphene fiber nonwoven of N doping
Cloth.
3. according to the method described in claim 2, it is characterized in that, the polymer being added in spinning solution is polyvinylpyrrolidine
Ketone, polyaniline, melamine, urea etc. is water-soluble or the nitrogenous compound of n,N-Dimethylformamide solvent, nitrogenous chemical combination
The mass fraction of object is 10%-50%.
4. according to the method described in claim 2, it is characterized in that, spinning solution is the aqueous solution or N of graphene oxide, N- diformazan
Base formamide solution.
5. according to the method described in claim 2, it is characterized in that, the coagulating bath that uses of spinning process is calcium chloride/water/ethyl alcohol
Mixed liquor or ethyl acetate.
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| KR20200112082A (en) * | 2019-03-20 | 2020-10-05 | 한국전력공사 | Graphene fiber and method for preparing the same |
| CN112726193A (en) * | 2020-12-21 | 2021-04-30 | 华中科技大学 | Cobalt-nitrogen co-doped carbon nanotube modified graphene fiber, and preparation and application thereof |
| CN113215857A (en) * | 2021-04-13 | 2021-08-06 | 中国科学院电工研究所 | Heteroatom-doped graphene nanofiber non-woven fabric and preparation method thereof |
| CN116575144A (en) * | 2023-07-13 | 2023-08-11 | 烯源科技无锡有限公司 | Preparation method for preparing antibacterial graphene fibers through electrostatic spinning |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113215857A (en) * | 2021-04-13 | 2021-08-06 | 中国科学院电工研究所 | Heteroatom-doped graphene nanofiber non-woven fabric and preparation method thereof |
| CN116575144A (en) * | 2023-07-13 | 2023-08-11 | 烯源科技无锡有限公司 | Preparation method for preparing antibacterial graphene fibers through electrostatic spinning |
| CN116575144B (en) * | 2023-07-13 | 2023-09-26 | 烯源科技无锡有限公司 | Preparation method for preparing antibacterial graphene fibers through electrostatic spinning |
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