CN104559175B - Preparation method of carbon nano tube-Kevlar nanofiber composite film - Google Patents
Preparation method of carbon nano tube-Kevlar nanofiber composite film Download PDFInfo
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Abstract
The invention discloses a preparation method of a carbon nano tube-Kevlar nanofiber composite film. The preparation method comprises the following steps: a carbon nano tube and Kevlar nanofiber, which are treated with acid, are used as raw materials, the two materials with excellent mechanical properties are compounded effectively for the first time, and a thought of vacuum filtration assisted layer-by-layer assembly is put forward to prepare the carbon nano tube-Kevlar nanofiber composite film. The carbon nano tube and the Kevlar nanofiber are effectively compounded for the first time to prepare the carbon nano tube enhanced Kevlar nanofiber composite film; the carbon nano tube enhanced Kevlar nanofiber composite film inherits the advantages of the carbon nano tube and a Kevlar fiber monomer in the aspects of heat, electricity and mechanics and the like. A layer-by-layer self-assembly method is adopted, so that the problem that the carbon nano tube has poor dispersibility in a polymer is reduced. The vacuum filtration assisted self-assembly method is presented, and has the characteristics of being simple and feasible, low in cost, and high in preparation speed on the basis of keeping the advantages of layer-by-layer assembly.
Description
Technical field
The invention belongs to field of material technology, it is related to a kind of CNT-Kev and draws the superpower laminated film of nanofiber
Preparation method.
Background technology
CNT heat, electrically and mechanically excellent performance, its low density, big draw ratio, high mechanical property make its
Strengthen phase aspect as polymer matrix and present huge potentiality.But the problem of CNT bad dispersibility in the polymer, resistance
Hinder its embodiment in macroscopic body for many excellent properties.At this stage with CNT for strengthening the polymer matrix composite of phase
Mechanical property lifting is limited mostly, or even some polymer produce " repulsion " reaction to CNT.Kafra fiber is as one
Kind of new aramid fiber, due to its prominent mechanical property, good heat stability and be extensively applied to chemical industry, machinery, the energy, army
The directions such as work.But the fiber of this excellent performance limits it in composite side because being difficult to find that suitable process for dispersing
To application and development.It is even more from being not directed to preparing multifunctional composite field.The uniqueness of CNT can be projected
Electricity, mechanical characteristic, can highlight Kev again and draw the composite of excellent mechanics, calorifics feature certainly will have a wide range of applications
Prospect.Based on this, how Kafra fiber to be disperseed, select appropriate method to prepare CNT-Kev and draw composite, overcome
CNT in the polymer bad dispersibility the problems such as, become the practical problem of urgent need to resolve.Do not find at this stage by
Both are mixed with the correlational study of composite, also do not find the Suitable preparation methods solving problem above.
Content of the invention
For problem above, the invention provides a kind of preparation side of CNT-Kev Rana rice fiber composite thin film
Method.The method achieves, using the method for deprotonation, the dispersion that Kev draws nanofiber in common solvents；Using layer by layer certainly
The method of assembling is realized controlling the growth of multilayer film on nanoscale, and realizes the control of material structure and component, reduces nanometer
Storeroom is mutually reunited, and lifts dispersibility in Kev draws for the CNT；Propose the method that sucking filtration assists layer assembly, overcome
Common layer assembly method haves such problems as that operation is numerous and diverse, time length, a large amount of duplication of labour；Finally prepare and had
The laminated film of excellent mechanical, electrically and thermally performance.
The purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of CNT-Kev Rana rice fiber composite thin film, with acid-treated CNT and
It is raw material that Kev draws nanofiber, first the material of both excellent in mechanical performance effectively combines, and proposes vacuum filtration
The thinking of auxiliary layer assembly, prepares CNT and strengthens Kev Rana rice fiber composite thin film.Concrete preparation process is as follows:
First, Kev draws the preparation of nanofiber: weighs Kafra fiber 1-5g, 12-24 is dried little in vacuum drying oven
When take out standby.Take Lithium hydrate 1-3g, with magnetic force in the dimethyl sulfoxide that dried Kafra fiber puts into 500-800ml
Stirring 3-7 days, you can obtain wine-colored Kev Rana rice fiber solution.
2nd, the preparation of carbon nano tube dispersion liquid: weigh 20-30mg multi-walled carbon nano-tubes, add concentrated sulphuric acid to mix with nitric acid
Liquid 120-180ml, stirs 2-4 hour, subsequent ultrasonic vibration in the environment of 60 DEG C.Resulting solution deionized water is diluted,
Filtering with microporous membrane, the solid on flushing membrane to filtrate ph=7, gained black precipitate is vacuum dried, that is, obtains carboxylated carbon and receive
Mitron.Weigh the CNT 5-10mg of carboxylated process, mix with 500-1000ml dimethyl sulphoxide solution, after ultrasonic vibration
Centrifugation, takes supernatant, that is, obtain carbon nano tube dispersion liquid.
In this step, described concentrated sulphuric acid is 3:1 with the volume ratio of nitric acid.
In this step, described vacuum drying temperature is 60-80 DEG C, and the time is 12-24 hour.
In this step, described ultrasonic power is 80-100w.
In this step, described centrifugation rotating speed is 4000r/min.
3rd, Kev draws the outfit of solution: Kev Rana rice fiber solution that step one is obtained, dimethyl sulfoxide and go from
Sub- water mixes in turbine mixer according to the volume ratio of 3:30:4-8, obtains Kev and draws solution.
In this step, described incorporation time is 1-3 hour.
4th, vacuum filtration method householder methods prepare thin film: draw solution, one layer of carbon nano tube dispersion liquid according to one layer of Kev
Order successively Deca on filter paper, with the carrying out of sucking filtration, you can deposits last layer thin film in filter paper, and that is, Kev draws-carbon nanometer
Manage thin composite membrane.
In this step, described filter paper selects diameter 50mm, organic nylon leaching film in 0.1-0.15 μm of aperture.
In this step, next layer of solution will be gradually dropped after last layer solution is drained only by each sucking filtration again.
In this step, described Kev draws-and the number of plies of the thin composite membrane of CNT is 10-30 layer.
In this step, Kev draws-the thin composite membrane of CNT in the content of CNT be 1-10wt.%
5th, the acquisition of thin film: the thin film having filtered is soaked 12-24 hour in deionized water, removes impurity on thin film.
Thin film is dried in normal temperature air and tears, you can obtain Kev and draw-carbon nano-tube coextruded film.
The method have the advantages that
1st, first CNT and Kev are drawn nanofiber effectively compound, prepared CNT enhancing Kev and drawn
Nanofiber laminated film；This laminated film inherits CNT with Kafra fiber monomer in heat, electricity and terms of mechanics
Many advantages.
2nd, the method adopting LBL self-assembly, decreases the problem that CNT increases bad dispersibility in the polymer.Propose
The method of vacuum filtration assisted self assembling, the method have keep layer assembly advantage on the basis of, have simple,
The features such as low cost, preparation speed are fast.
Brief description
Fig. 1 prepares carbon compound film front and the section electricity of carbon nanotube mass fraction 2.5% for embodiment 1 methods described
Mirror figure；
The stress-strain that Fig. 2 prepares the carbon compound film of carbon nanotube mass fraction 3% for embodiment 2 methods described is bent
Line；
Fig. 3 prepares the thermal strain curve of the carbon compound film of carbon nanotube mass fraction 5% for embodiment 3 methods described；
Fig. 4 is the THIN COMPOSITE conduction linearity curve under different content of carbon nanotubes.
Specific embodiment
Below in conjunction with the accompanying drawings technical scheme is further described, but is not limited thereto, every to this
Inventive technique scheme is modified or equivalent, without deviating from the spirit and scope of technical solution of the present invention, all should cover
In protection scope of the present invention.
Embodiment 1:
Present embodiments provide a kind of preparation method of the laminated film of carbon nanotube mass fraction 2.5%, concrete preparation step
Suddenly as follows:
First, Kev draws the preparation of nanofiber: weigh Kafra fiber (dupont, k69) 1g, dry in vacuum drying oven
Take out within dry 24 hours standby.Take Lithium hydrate 1.5g, with magnetic in the dimethyl sulfoxide that dried Kafra fiber puts into 500ml
Power stirs 1 week, you can obtain wine-colored Kev Rana rice fiber solution.
2nd, the preparation of carbon nano tube dispersion liquid: weigh 20mg multi-walled carbon nano-tubes, add the concentrated sulphuric acid that volume ratio is 3:1
With concentrated nitric acid mixed liquor 120ml, stir 4 hours in the environment of 60 DEG C, subsequent ultrasonic vibration 2 hours.Resulting solution is spent
Ionized water dilutes, filtering with microporous membrane, and gained black precipitate is done by the solid on flushing membrane to filtrate ph=7 in 80 DEG C of vacuum
It is dried in dry case 24 hours, that is, obtain carboxylic carbon nano-tube.Weigh the CNT 10mg of carboxylated process, with 1000ml bis-
Methyl sulfoxide solution mixes, and in the ultrasonic vibration 1 hour of 100w, centrifugation under the speed of 4000r/min took supernatant after 20 minutes
Liquid, that is, obtain carbon nano tube dispersion liquid.
3rd, Kev draws the outfit of solution: the Kev Rana rice fiber solution of acquisition, dimethyl sulfoxide and deionized water are pressed
Volume ratio according to 3:30:4 mixes 2 hours in turbine mixer, obtains Kev and draws solution.
4th, vacuum filtration method householder methods prepare thin film: filter paper selects diameter 50mm, organic nylon filter in 0.1 μm of aperture
Film.Taking prepare 20 layers of self-assembled film as a example, respectively the Kev of 37ml is drawn the carbon nano tube dispersion liquid of solution and 15.3ml
10 parts of decile, draws the order successively sucking filtration of solution, one layer of carbon nano tube dispersion liquid according to one layer of Kev.Sucking filtration will wait until every time
Next layer of solution is gradually dropped after draining only by last layer solution again.Increasing it can be observed that filter paper deposits with the number of plies
Thin film, that is, Kev draw the-thin composite membrane of CNT.
5th, the acquisition of thin film: the thin film having filtered is soaked 1 hour in deionized water, removes impurity on thin film.Will be thin
Film is dried in normal temperature air and tears, you can obtains Kev and draws-carbon nano-tube coextruded film (Fig. 1).
Embodiment 2:
Present embodiments provide a kind of preparation method of the laminated film of carbon nanotube mass fraction 3%, concrete preparation process
As follows:
First, Kev draws the preparation of nanofiber: weighs Kafra fiber (dupont, k69) 1.5g, in vacuum drying oven
24 hour taking-up is dried standby.Take Lithium hydrate 2g, with magnetic in the dimethyl sulfoxide that dried Kafra fiber puts into 750ml
Power stirs 1 week, you can obtain wine-colored Kev Rana rice fiber solution.
2nd, the preparation of carbon nano tube dispersion liquid: weigh 30mg multi-walled carbon nano-tubes, add the concentrated sulphuric acid that volume ratio is 3:1
With concentrated nitric acid mixed liquor 150ml, stir 4 hours in the environment of 60 DEG C, subsequent ultrasonic vibration 2 hours.Resulting solution is spent
Ionized water dilutes, filtering with microporous membrane, and gained black precipitate is done by the solid on flushing membrane to filtrate ph=7 in 60 DEG C of vacuum
It is dried in dry case 24 hours, that is, obtain carboxylic carbon nano-tube.Weigh the CNT 10mg of carboxylated process, 1000ml diformazan
Base sulfoxide solution mixes, and in the ultrasonic vibration 1 hour of 100w, centrifugation under the speed of 4000r/min took supernatant after 20 minutes,
Obtain carbon nano tube dispersion liquid.
3rd, Kev draws the outfit of solution: the Kev Rana rice fiber solution of acquisition, dimethyl sulfoxide and deionized water are pressed
Volume ratio according to 3:30:4 mixes 1.5 hours in turbine mixer, obtains Kev and draws solution.
4th, vacuum filtration method householder methods prepare thin film: filter paper selects diameter 50mm, organic nylon filter in 0.1 μm of aperture
Film.Taking prepare 20 layers of self-assembled film as a example, respectively the Kev of 37ml is drawn the carbon nano tube dispersion liquid decile with 18.5ml
10 parts, draw the order successively sucking filtration of solution, one layer of carbon nano tube dispersion liquid according to one layer of Kev.Sucking filtration will wait until upper one every time
Next layer of solution is gradually dropped after draining only by layer solution again.Increasing it can be observed that filter paper deposits last layer with the number of plies
Thin film, that is, Kev draw the-thin composite membrane of CNT.
5th, the acquisition of thin film: the thin film having filtered is soaked 1.5 hours in deionized water, removes impurity on thin film.Will
Thin film is dried in normal temperature air and tears, you can obtains Kev and draws-carbon nano-tube coextruded film.
As shown in Figure 2, with the increase of strain, the stress of laminated film is gradually increased.Laminated film maximum intensity
318mpa, modulus 29.9gpa.Thin film mechanicalness compared with strengthening laminated film with other CNTs, prepared by the present embodiment
Similar thin film can be far above.
Embodiment 3:
Present embodiments provide a kind of preparation method of the laminated film of carbon nanotube mass fraction 5%, concrete preparation process
As follows:
First, Kev draws the preparation of nanofiber: weigh Kafra fiber (dupont, k69) 2g, dry in vacuum drying oven
Take out within dry 12 hours standby.Take Lithium hydrate 2g, with magnetic in the dimethyl sulfoxide that dried Kafra fiber puts into 1000ml
Power stirs 1 week, you can obtain wine-colored Kev Rana rice fiber solution.
2nd, the preparation of carbon nano tube dispersion liquid: weigh 30mg multi-walled carbon nano-tubes, add the concentrated sulphuric acid that volume ratio is 3:1
With concentrated nitric acid mixed liquor 180ml, stir 4 hours in the environment of 60 DEG C, subsequent ultrasonic vibration 2 hours.Resulting solution is spent
Ionized water dilutes, filtering with microporous membrane, and gained black precipitate is done by the solid on flushing membrane to filtrate ph=7 in 80 DEG C of vacuum
It is dried in dry case 24 hours, that is, obtain carboxylic carbon nano-tube.Weigh the CNT 5mg of carboxylated process, with 500ml diformazan
Base sulfoxide solution mixes, and in the ultrasonic vibration 1 hour of 100w, centrifugation under the speed of 4000r/min took supernatant after 20 minutes,
Obtain carbon nano tube dispersion liquid.
3rd, Kev draws the outfit of solution: the Kev Rana rice fiber solution of acquisition, dimethyl sulfoxide and deionized water are pressed
Volume ratio according to 3:30:6 mixes 2 hours in turbine mixer, obtains Kev and draws solution.
4th, vacuum filtration method householder methods prepare thin film: filter paper selects diameter 50mm, organic nylon filter in 0.1 μm of aperture
Film.Taking prepare 30 layers of self-assembled film as a example, respectively the Kev of 78ml is drawn carbon nano tube dispersion liquid with 63ml etc. point 15
Part, the order successively sucking filtration of solution, one layer of carbon nano tube dispersion liquid is drawn according to one layer of Kev.Sucking filtration will wait until last layer every time
Next layer of solution is gradually dropped after draining only by solution again.Increasing it can be observed that filter paper deposition last layer is thin with the number of plies
Film, that is, Kev draw the-thin composite membrane of CNT.
5th, the acquisition of thin film: the thin film having filtered is soaked 2 hours in deionized water, removes impurity on thin film.Will be thin
Film is dried in normal temperature air and tears, you can obtains Kev and draws-carbon nano-tube coextruded film.
It is to raise with temperature from Fig. 3, laminated film presents positive thermal coefficient of expansion.Prepared by the present embodiment
Thin film before 200 DEG C thin film remain to keep good heat stability.Laminated film size in thermal environment keeps not substantially
Become thermal coefficient of expansion and be less than 5 ppm/k.
Introducing due to CNT be can be seen that by the curve in Fig. 4, laminated film there occurs non-conductor conductor 801
Change.With the increase of content of carbon nanotubes, the surface resistance value of laminated film is gradually reduced.In carbon nanotube mass fraction 10%
When, the surface resistance value of laminated film reaches 10-2The order of magnitude, the good conduction property of laminated film tool.
Claims (9)
1. a kind of preparation method of CNT-Kev Rana rice fiber composite thin film is it is characterised in that described preparation method walks
Suddenly as follows:
First, Kev draws the preparation of nanofiber: weighs Kafra fiber 1-5g, 12-24 hour is dried takes in vacuum drying oven
Go out standby；Take Lithium hydrate 1-3g, with magnetic agitation in the dimethyl sulfoxide that dried Kafra fiber puts into 500-800ml
3-7 days, that is, obtain wine-colored Kev Rana rice fiber solution；
2nd, the preparation of carbon nano tube dispersion liquid: weigh 20-30mg multi-walled carbon nano-tubes, add concentrated sulphuric acid and nitric acid mixed liquor
120-180ml, stirs 2-4 hour, subsequent ultrasonic vibration in the environment of 60 DEG C；Resulting solution deionized water is diluted, micro-
Hole membrane filtration, the solid on flushing membrane to filtrate ph=7, gained black precipitate is vacuum dried, that is, obtains carboxylated carbon nanometer
Pipe；Weigh the CNT 5-10mg of carboxylated process, mix with 500-1000ml dimethyl sulphoxide solution, after ultrasonic vibration from
The heart separates, and takes supernatant, that is, obtain carbon nano tube dispersion liquid；
3rd, Kev draws the outfit of solution: by Kev Rana rice fiber solution, dimethyl sulfoxide and deionized water according to 3:30:4-8
Volume ratio mix in turbine mixer, obtain Kev and draw solution；
4th, vacuum filtration method householder methods prepare thin film: draw the order of solution, one layer of carbon nano tube dispersion liquid according to one layer of Kev
Successively Deca on filter paper, with the carrying out of sucking filtration, you can deposits last layer thin film in filter paper, that is, Kev draw-CNT is multiple
Close thin film；
5th, the acquisition of thin film: the thin film having filtered is soaked 12-24 hour in deionized water, removes impurity on thin film, will be thin
Film is dried in normal temperature air and tears, that is, obtain Kev and draw-carbon nano-tube coextruded film.
2. CNT according to claim 1-Kev Rana rice fiber composite thin film preparation method it is characterised in that
In described step 2, concentrated sulphuric acid is 3:1 with the volume ratio of nitric acid.
3. CNT according to claim 1-Kev Rana rice fiber composite thin film preparation method it is characterised in that
In described step 2, vacuum drying temperature is 60-80 DEG C, and the time is 12-24 hour.
4. CNT according to claim 1-Kev Rana rice fiber composite thin film preparation method it is characterised in that
In described step 2, the CNT of carboxylated process mix with dimethyl sulphoxide solution after in ultrasonic power for 80-100w's
Under the conditions of ultrasonic vibration.
5. CNT according to claim 1-Kev Rana rice fiber composite thin film preparation method it is characterised in that
In described step 2, centrifugation rotating speed is 4000r/min.
6. CNT according to claim 1-Kev Rana rice fiber composite thin film preparation method it is characterised in that
In described step 3, incorporation time is 1-3 hour.
7. CNT according to claim 1-Kev Rana rice fiber composite thin film preparation method it is characterised in that
In described step 4, described filter paper selects diameter 50mm, organic nylon leaching film in 0.1-0.15 μm of aperture.
8. CNT according to claim 1-Kev Rana rice fiber composite thin film preparation method it is characterised in that
In described step 4, next layer of solution will be gradually dropped after last layer solution is drained only by each sucking filtration again.
9. CNT according to claim 1-Kev Rana rice fiber composite thin film preparation method it is characterised in that
In described step 4, Kev draws-and the number of plies of carbon nano-tube coextruded film is 10-30 layer.
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| CN105648614B (en) * | 2015-12-29 | 2017-06-13 | 哈尔滨工业大学 | A kind of porous heat-insulating strong film functionalization lunar exploration high of gradient distribution takes the preparation method of earth coring soft bag |
| CN108084468B (en) * | 2017-12-29 | 2020-12-01 | 陕西科技大学 | Preparation method of nano aramid fiber film based on vacuum-assisted layer-by-layer self-assembly |
| CN108559188B (en) * | 2018-05-10 | 2020-08-07 | 南通市第一人民医院 | Substrate for blood sugar test paper for gestational diabetes |
| CN110526198B (en) * | 2018-05-24 | 2024-05-28 | 深圳先进技术研究院 | Flexible pressure sensor based on hemispherical microstructure and manufacturing method thereof |
| CN109881540B (en) * | 2019-03-20 | 2020-11-06 | 湖北大学 | Preparation method of novel Kevlar fiber reinforced multipurpose paper based on ultra-long hydroxyapatite nanowires |
| CN110556559B (en) * | 2019-09-16 | 2022-06-14 | 东北大学 | Method for preparing low-temperature proton exchange membrane with layered structure based on vacuum-assisted flocculation technology |
| CN111040237B (en) * | 2019-12-25 | 2022-07-26 | 陕西科技大学 | Conductive aramid nanofiber composite aerogel and preparation method thereof |
| CN114573983B (en) * | 2022-03-16 | 2022-11-04 | 哈尔滨工业大学 | Preparation method of nano-diamond/aramid nanofiber multifunctional composite heat-conducting film |
| CN115364682B (en) * | 2022-08-19 | 2024-06-11 | 浙江工业大学 | Preparation method of nano heterostructure composite membrane and application of nano heterostructure composite membrane in dye desalination |
| CN116876253A (en) * | 2023-06-14 | 2023-10-13 | 哈尔滨工程大学 | Controllable preparation method of multifunctional aramid nanofiber wave-absorbing composite membrane |
| CN116751388B (en) * | 2023-07-02 | 2024-05-24 | 南昌大学附属口腔医院(江西省口腔医院) | High-strength conductive cellulose nanocrystalline/carbon nanotube/aramid nanofiber composite membrane and preparation method thereof |
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