CN108385450A - A kind of carbon nanotube paper and preparation method thereof - Google Patents
A kind of carbon nanotube paper and preparation method thereof Download PDFInfo
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- CN108385450A CN108385450A CN201810062419.8A CN201810062419A CN108385450A CN 108385450 A CN108385450 A CN 108385450A CN 201810062419 A CN201810062419 A CN 201810062419A CN 108385450 A CN108385450 A CN 108385450A
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- carbon nanotube
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21J—FIBREBOARD; MANUFACTURE OF ARTICLES FROM CELLULOSIC FIBROUS SUSPENSIONS OR FROM PAPIER-MACHE
- D21J7/00—Manufacture of hollow articles from fibre suspensions or papier-mâché by deposition of fibres in or on a wire-net mould
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
- D21H13/02—Synthetic cellulose fibres
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
Abstract
The invention belongs to carbon nanomaterial technical field more particularly to a kind of carbon nanotube paper, the carbon nanotube paper includes carbon nanotube and chemical fibre.The invention further relates to a kind of preparation methods of above-mentioned carbon nanotube paper, and this method comprises the following steps：Carbon nanotube is placed in alcohols solvent and carries out ultrasonic disperse by step 1；Chemical fibre is placed in alcohols solvent and carries out high speed dispersion；Chemical fibre dispersion liquid and carbon nano tube dispersion liquid are mixed to get uniform mixed liquor by step 2；Step 3, uniform mixed liquor is placed in corresponding filter device and is filtered, and carbon nanotube l Water Paper in homogeneous thickness is formed on filter membrane；Carbon nanotube l Water Paper is put into togerther with filter membrane in baking oven and toasts by step 4；Step 5 removes the carbon nanotube paper after drying from filter membrane, and carries out roll-in using roll squeezer.The carbon nanotube paper of the present invention and preparation method thereof is not only at low cost, process is few, purity is high, facilitates transfer, but also is suitble to large-scale production.
Description
Technical field
The invention belongs to carbon nanomaterial technical fields more particularly to a kind of carbon nanotube paper and preparation method thereof.
Background technology
Carbon nanotube also known as Baji-tube are that with special construction, (radial dimension is nanometer scale to one kind, and axial dimension is
Micron dimension, pipe both ends are substantially all sealing) One-dimensional Quantum material, number is mainly constituted by the carbon atom of hexagonal arrangement
Layer arrives tens of layers of coaxial pipe.Carbon nanotube possesses high aspect ratio structures, has good electric conductivity, mechanical property excellent
It is different, large specific surface area.Carbon nanotube can regard that graphene sheet layer crimps as, therefore can divide according to the number of plies of graphene film
For:Single-walled carbon nanotube and multi-walled carbon nanotube.Common preparation method of carbon nano-tube mainly has:Arc discharge method, laser are burnt
Erosion method, chemical vapour deposition technique (hydrocarbon gas pyrolysismethod), solid-phase pyrolysis, electric glow discharge method, gas combustion method and polymerization
Reaction synthesis method etc..
Carbon nanotube paper (Buckie paper) is made of the unordered carbon nanotube of certain length, has the ratio much larger than carbon fiber paper
Intensity, good electrical and thermal conductivity and chemical stability similar in surface area and conductive graphite piece are spread in fuel cell gas
Layer, electric chemical super capacitor, lithium ion battery cathode, the cooling pad of high-power electronic device, high-performance polymer composite wood
There is larger application value in the fields such as material.
Nano-grade size due to carbon nanotube and special long gauge structure, dispersion are very difficult.And traditional carbon
Nanotube paper structure is fluffy, poor mechanical property.According to above deficiency, the production method of many carbon papers is shown one's talent, such as China
Patent publication No. is described in 106396680A, and by carbon pipe and dispersant in solvent, ultrasonic disperse processing adds
Paper pulp, high speed shear dispersion, mixing, is molded using conventional paper-making processes, then carries out high temperature modified processing to carbon paper, then carry out
Carbonization treatment, last roll-forming；For another example China Patent Publication No. 102877367A equally first mixes carbon pipe with dispersant
It closes, is dispersed with stirring processing, staple fiber is then added, high speed shear dispersion is molded thereafter using curtain coating paper technology, most afterwards after
Dispersant is taken out in processing, obtains target product；Process is more in this way, on the one hand increases cost, and another aspect dispersant is easy
The electric conductivity for influencing carbon nanotube, to reduce the performance of carbon nanotube paper.
Invention content
It is an object of the invention to overcome the defect of the prior art, a kind of carbon nanotube paper and preparation method thereof is provided,
It is not only at low cost, process is few, purity is high, facilitates transfer, but also be suitble to large-scale production.
The invention is realized in this way：
The present invention provides a kind of carbon nanotube paper, and the carbon nanotube paper includes carbon nanotube and chemical fibre.
Further, carbon nanotube and the mass ratio of chemical fibre are in the carbon nanotube paper（90-99.9）：
（0.1-10）.
The present invention also provides a kind of preparation methods of above-mentioned carbon nanotube paper, and this method comprises the following steps：
Step 1, dispersion：Carbon nanotube is placed in alcohols solvent and carries out ultrasonic disperse, obtains carbon nano tube dispersion liquid；It will be chemical
Fiber, which is placed in alcohols solvent, carries out high speed dispersion, obtains chemical fibre dispersion liquid；
Step 2, mixing：Chemical fibre dispersion liquid is mixed with carbon nano tube dispersion liquid, by high-speed stirred, is obtained uniform
Mixed liquor；
Step 3, filtering：Mixed liquor obtained in step 2 is placed in corresponding filter device and is filtered, is formed on filter membrane
Carbon nanotube l Water Paper in homogeneous thickness；
Step 4, baking：Carbon nanotube l Water Paper is put into togerther with filter membrane in baking oven and is toasted, solvent is removed；
Step 5, tabletting：Carbon nanotube paper after drying is removed from filter membrane, using roll squeezer to dry carbon nanotube paper
Roll-in is carried out, target product is obtained.
Further, in the step 1 carbon nanotube quality（mg）With the volume of alcohols solvent（mL）The ratio between be
0.01mg/mL-0.5mg/mL；The power of ultrasonic disperse is 30W-600W, and the time of ultrasonic disperse is 0.1h-5h.
Further, in the step 1 chemical fibre quality（mg）With the volume of alcohols solvent（mL）The ratio between be
0.1mg/mL-1mg/mL；The rotating speed of high speed dispersion is 1000-20000rpm, and the time of high speed dispersion is 0.1-10h.
Further, the rotating speed of the step 2 high speed stirring is 500-10000rpm；In the mixed liquor, carbon nanometer
It manages and is with the mass ratio of chemical fibre（90-99.9）：（0.1-10）.
Further, the filter type in the step 3 can be vacuum filtration or press filtration；The vacuum of the vacuum filtration
The speed of exhaust of pump is 0.1L/s-20.0L/s；The pressure of the press filtration is 0.3-3MPa.
Further, the filter membrane in the step 3 is polyethylene filter membrane, polypropylene filter, teflon membrane filter, Buddhist nun
The aperture of any one in imperial filter membrane, filter membrane is 0.05-50 μm.
Further, the baking temperature in the step 4 is 25-150 DEG C, baking time 0.1h-5h, roasting mode
For air blast baking or vacuum bakeout.
Further, the compacted density of the carbon nanotube paper tabletting in the step 5 is 0.5-2g/cm3。
The principle of the present invention is：Carbon nanotube has preferable compatibility in alcohols solvent, by the effect of ultrasonic disperse,
Make to realize whole dispersity in a solvent between carbon nanotube molecule；High-speed stirred in advance, disperse chemical fiber will be chemical
Fiber dispersion is mixed with carbon nano tube dispersion liquid, high speed dispersion, keeps mixed liquor more uniform；Later in filter process, carbon
Self assembly effect is formed between nanotube is intermolecular and chemical fibre, and binding force is mainly shown as molecule Van der Waals force and major diameter point
Crosslinked action between son；In carbon nanotube paper, pass through the crosslinking between Van der Waals force and major diameter molecule between carbon nanotube molecule
Effect is mutually tangled, meanwhile, chemical fibre is interleaved together, and forms tridimensional network, support is provided for carbon nanotube, is improved
The flexibility and flexible energy of carbon nanotube paper.
Compared with prior art, the invention has the advantages that：
（1）Carbon nanotube paper prepared by the present invention, including carbon nanotube and chemical fibre；The chemical fibre is natural fiber
Or protein fibre or natural inorganic object or phasphorus-containing polymer are raw material, the manufactured fibre by chemical treatment and mechanical processing
Dimension, can be divided into staple fibre（Regenerated fiber）, synthetic fibers and inorfil.Chemical fibre mechanical property is strong, stable structure, no
The structure of meeting destroying carbon nanometer tube, while the chemical fibre of suitable diameter, length, molecular weight can be selected according to demand；On a small quantity
Chemical fibre can fetter carbon nanotube, reduce the loss of carbon nanotube, enhance the mechanical performance of carbon nanotube paper；Meanwhile
Since chemical fibre content is less, the electric conductivity of carbon nanotube paper entirety is not interfered with；Therefore, a small amount of chemical fibre ensures
Carbon nanotube paper good electric conductivity, and make it have good bending property；
（2）For carbon nanotube paper provided by the invention in preparation process, process is few, simple for process；In preparation process, do not introduce additional
Functional group, there are very high cleannes, filtered carbon nanotube paper can accomplish that zero loss, solvent can be repeatedly circulated,
To reduce production cost, strong condition is provided for large-scale production；
（3）Pass through the crosslinking between Van der Waals force and major diameter molecule in carbon nanotube paper provided by the invention between carbon nanotube molecule
Effect is mutually tangled；Meanwhile chemical fibre is interleaved together, and forms tridimensional network, support is provided for carbon nanotube, is improved
The flexibility and flexible energy of carbon nanotube paper.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
Other attached drawings are obtained according to these attached drawings.
Fig. 1 is the photo of carbon nanotube paper provided by the invention；
Fig. 2 is the SEM photograph of carbon nanotube paper provided by the invention；
Fig. 3 is the flexible display diagram of carbon nanotube paper provided by the invention.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts all other
Embodiment shall fall within the protection scope of the present invention.
The embodiment of the present invention provides a kind of carbon nanotube paper, and carbon nanotube paper includes carbon nanotube and chemical fibre.Chemistry
Fiber is natural fiber or protein fibre or natural inorganic object or phasphorus-containing polymer is raw material, by chemical treatment and machinery
It processes and manufactured fiber, as Figure 1-Figure 2.
Further, carbon nanotube and the mass ratio of chemical fibre are in carbon nanotube paper（90-99.9）：（0.1-
10）.
Chemical fibre mechanical property is strong in the present embodiment, stable structure, will not destroying carbon nanometer tube structure, a small amount of change
Carbon nanotube can be fettered by learning fiber, reduced the loss of carbon nanotube, enhanced the mechanical performance of carbon nanotube paper；Simultaneously as
Chemical fibre content is less, does not interfere with the electric conductivity of carbon nanotube paper entirety；Therefore, a small amount of chemical fibre ensure that carbon
The good electric conductivity of nanotube paper, and good bending property is made it have, as shown in Figure 3.
The present invention also provides a kind of preparation methods of above-mentioned carbon nanotube paper, and this method comprises the following steps：
Step 1, dispersion：Carbon nanotube is placed in alcohols solvent and carries out ultrasonic disperse, obtains carbon nano tube dispersion liquid；It will be chemical
Fiber, which is placed in alcohols solvent, carries out high speed dispersion, obtains chemical fibre dispersion liquid；
Step 2, mixing：Chemical fibre dispersion liquid is mixed with carbon nano tube dispersion liquid, by high-speed stirred, is obtained uniform
Mixed liquor；
Step 3, filtering：Mixed liquor obtained in step 2 is placed in corresponding filter device and is filtered, is formed on filter membrane
Carbon nanotube l Water Paper in homogeneous thickness；
Step 4, baking：Carbon nanotube l Water Paper is put into togerther with filter membrane in baking oven and is toasted, solvent is removed；
Step 5, tabletting：Carbon nanotube paper after drying is removed from filter membrane, using roll squeezer to dry carbon nanotube paper
Roll-in is carried out, the volume density of carbon nanotube paper is improved, enhances its mechanical property, obtain target product.
For carbon nanotube paper in the present embodiment in preparation process, process is few, simple for process；In preparation process, volume is not introduced
There are very high cleannes, filtered carbon nanotube paper can accomplish zero loss for outer functional group, solvent can iterative cycles make
With, to reduce production cost, for large-scale production provide strong condition；In addition pass through model moral between carbon nanotube molecule
Crosslinked action between Hua Li and major diameter molecule is mutually tangled；Meanwhile chemical fibre is interleaved together, and forms three-dimensional netted knot
Structure provides support for carbon nanotube, improves the flexibility and flexible energy of carbon nanotube paper.
Further, in step 1 carbon nanotube quality（mg）With the volume of alcohols solvent（mL）The ratio between be 0.01mg/
mL-0.5mg/mL；The power of ultrasonic disperse is 30W-600W, and the time of ultrasonic disperse is 0.1h-5h.
Further, in step 1 chemical fibre quality（mg）With the volume of alcohols solvent（mL）The ratio between be 0.1mg/
mL-1mg/mL；The rotating speed of high speed dispersion is 1000-20000rpm, and the time of high speed dispersion is 0.1-10h.
Further, alcohols solvent is at least one of ethyl alcohol, ethylene glycol, isopropanol, n-butanol.
Further, chemical fibre is arbitrary in polyethylene fibre, polypropylene fibre, polymethylmethacrylate fibers
It is a kind of.
Further, the rotating speed of step 2 high speed stirring is 500-10000rpm；In mixed liquor, carbon nanotube and chemistry
The mass ratio of fiber is（90-99.9）：（0.1-10）.
Further, the filter type in step 3 can be vacuum filtration or press filtration；The pumping of the vacuum pump of vacuum filtration
Rate is 0.1L/s-20.0L/s；The pressure of press filtration is 0.3-3MPa.
Further, the filter membrane in step 3 is polyethylene filter membrane, polypropylene filter, teflon membrane filter, nylon filter
The aperture of any one in film, filter membrane is 0.05-50 μm.
Further, the baking temperature in step 4 is 25-150 DEG C, baking time 0.1h-5h, and roasting mode is drum
Wind toasts or vacuum bakeout.
Further, it is 0.5-2g/cm that the compacted density of the carbon nanotube paper tabletting in step 5, which is no more than,3。
Embodiment one
Carbon nanotube is placed in isopropanol solvent, the quality of carbon nanotube（mg）With the volume of isopropanol solvent（mL）The ratio between be
0.01mg/mL, using ultrasound method in the isopropanol solvent dispersing Nano carbon tubes, ultrasonic power 60W, ultrasonic time
0.5h；Polyethylene fibre is dissolved in isopropanol solvent, 5000rpm disperses 1h, the quality of chemical fibre（mg）It is molten with isopropanol
The volume of agent（mL）The ratio between be 0.1mg/mL；The wherein molecular weight 3 × 10 of polyethylene fibre4, 70 nanometers of diameter, length 350 is micro-
Rice；After dispersion, two kinds of dispersion liquids are mixed, 5000rpm high-speed stirred 1h obtain uniform mixed liquor；In mixed liquor, carbon
The mass ratio of nanotube and polyethylene fibre is 98:2；Uniform mixed liquor is transferred to filter device, is filtered by vacuum, vacuum
The speed of exhaust of pump is 1L/s, and filter membrane is polyethylene filter membrane；After the completion of suction filtration, filter membrane and carbon nanotube l Water Paper are put into togerther drum
It is toasted in wind drying box, 100 DEG C of baking temperature, baking time 1h；Finally by dry carbon nanotube paper from polyethylene filter membrane
Transfer, selective carry out tabletting are 0.5g/cm to get the compacted density to target carbon nanotube paper, the carbon nanotube paper3。
Embodiment two
Carbon nanotube is placed in ethyl alcohol and ethylene glycol solvent, the volume ratio of ethyl alcohol and ethylene glycol（mL）It is 1:2, carbon nanotube
Quality（mg）With the volume of alcohol mixed solvent（mL）The ratio between be 0.5mg/mL, using the method for ultrasound in the alcohol in the mixed solvent point
Dissipate carbon nanotube, ultrasonic power 100W, ultrasonic time 0.5h；Polypropylene fibre is dissolved in alcohol solvent, 6000rpm dispersions
1.5h, chemical fibre quality（mg）With the volume of alcohol solvent（mL）Ratio be 1mg/mL, wherein polyethylene fibre, molecular weight
20×104, 50 nanometers of diameter, 300 microns of length；After dispersion, two kinds of dispersion liquids are mixed, 8000rpm high-speed stirreds
0.5h obtains uniform mixed liquor；In mixed liquor, the mass ratio of carbon nanotube and polypropylene fibre is 99.5：0.5；It will be uniform
Mixed liquor be transferred to filter device, carry out press filtration, pressure 2MPa, filter membrane is teflon membrane filter；After the completion of press filtration, it will filter
Film is put into togerther in air dry oven with carbon nanotube l Water Paper and toasts, 80 DEG C of baking temperature, baking time 0.5h；It will finally dry
Carbon nanotube paper shifted from teflon membrane filter, selective carry out tabletting is to get to target carbon nanotube paper, the carbon
The compacted density of nanotube paper is 2g/cm3。
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (10)
1. a kind of carbon nanotube paper, it is characterised in that：The carbon nanotube paper includes carbon nanotube and chemical fibre.
2. a kind of carbon nanotube paper as described in claim 1, it is characterised in that：Carbon nanotube and chemistry in the carbon nanotube paper
The mass ratio of fiber is（90-99.9）：（0.1-10）.
3. a kind of preparation method of carbon nanotube paper as described in claim 1, which is characterized in that this method includes following step
Suddenly：
Step 1, dispersion：Carbon nanotube is placed in alcohols solvent and carries out ultrasonic disperse, obtains carbon nano tube dispersion liquid；It will be chemical
Fiber, which is placed in alcohols solvent, carries out high speed dispersion, obtains chemical fibre dispersion liquid；
Step 2, mixing：Chemical fibre dispersion liquid is mixed with carbon nano tube dispersion liquid, by high-speed stirred, is obtained uniform
Mixed liquor；
Step 3, filtering：Mixed liquor obtained in step 2 is placed in corresponding filter device and is filtered, is formed on filter membrane
Carbon nanotube l Water Paper in homogeneous thickness；
Step 4, baking：Carbon nanotube l Water Paper is put into togerther with filter membrane in baking oven and is toasted, solvent is removed；
Step 5, tabletting：Carbon nanotube paper after drying is removed from filter membrane, using roll squeezer to dry carbon nanotube paper
Roll-in is carried out, target product is obtained.
4. the preparation method of carbon nanotube paper as claimed in claim 3, it is characterised in that：Carbon nanotube in the step 1
Quality（mg）With the volume of alcohols solvent（mL）The ratio between be 0.01mg/mL-0.5mg/mL；The power of ultrasonic disperse is 30W-
The time of 600W, ultrasonic disperse are 0.1h-5h.
5. the preparation method of carbon nanotube paper as claimed in claim 3, it is characterised in that：Chemical fibre in the step 1
Quality（mg）With the volume of alcohols solvent（mL）The ratio between be 0.1mg/mL-1mg/mL；The rotating speed of high speed dispersion is 1000-
The time of 20000rpm, high speed dispersion are 0.1-10h.
6. the preparation method of carbon nanotube paper as claimed in claim 3, it is characterised in that：The step 2 high speed stirring
Rotating speed is 500-10000rpm；In the mixed liquor, the mass ratio of carbon nanotube and chemical fibre is（90-99.9）：（0.1-
10）.
7. the preparation method of carbon nanotube paper as claimed in claim 3, it is characterised in that：Filter type in the step 3
Can be vacuum filtration or press filtration；The speed of exhaust of the vacuum pump of the vacuum filtration is 0.1L/s-20.0L/s；The press filtration
Pressure is 0.3-3MPa.
8. the preparation method of carbon nanotube paper as claimed in claim 3, it is characterised in that：Filter membrane in the step 3 is poly-
The aperture of any one in ethylene filter membrane, polypropylene filter, teflon membrane filter, nylon leaching film, filter membrane is 0.05-50 μ
m。
9. the preparation method of carbon nanotube paper as claimed in claim 3, it is characterised in that：Baking temperature in the step 4
It it is 25-150 DEG C, baking time 0.1h-5h, roasting mode is air blast baking or vacuum bakeout.
10. the preparation method of carbon nanotube paper as claimed in claim 3, it is characterised in that：Carbon nanometer in the step 5
The compacted density of pipe letterweight piece is 0.5-2g/cm3。
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Cited By (7)
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| CN108749194A (en) * | 2018-08-30 | 2018-11-06 | 天津工业大学 | A kind of electromagnetic shielding sandwich laminated film and preparation method thereof |
| CN109167093A (en) * | 2018-09-03 | 2019-01-08 | 江西克莱威纳米碳材料有限公司 | A kind of hydroxylating whisker carbon nanotube paper and preparation method thereof and a kind of lithium-sulfur cell |
| CN109371742A (en) * | 2018-11-02 | 2019-02-22 | 杭州特种纸业有限公司 | A kind of coaster paper and preparation method thereof |
| CN109834960A (en) * | 2019-02-15 | 2019-06-04 | 柔电（武汉）科技有限公司 | A kind of carbon nano-tube film and preparation method thereof |
| CN111778779A (en) * | 2020-07-06 | 2020-10-16 | 上海安崎智能科技有限公司 | Whisker carbon nanotube far infrared paper and preparation method thereof |
| CN112176772A (en) * | 2020-09-25 | 2021-01-05 | 柔电（武汉）科技有限公司 | Preparation method of lithium-philic carbon nanotube paper and preparation method of composite metal lithium cathode |
| CN113073496A (en) * | 2020-09-17 | 2021-07-06 | 江汉大学 | Method for preparing conductive fiber paper with hydrophilic-hydrophobic lithium gradient structure and conductive fiber paper |
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| CN113073496A (en) * | 2020-09-17 | 2021-07-06 | 江汉大学 | Method for preparing conductive fiber paper with hydrophilic-hydrophobic lithium gradient structure and conductive fiber paper |
| CN112176772A (en) * | 2020-09-25 | 2021-01-05 | 柔电（武汉）科技有限公司 | Preparation method of lithium-philic carbon nanotube paper and preparation method of composite metal lithium cathode |
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