CN103232610A - Method for preparing directionally-arranged self-assembled carbon nanotube/thermoplastic resin film - Google Patents
Method for preparing directionally-arranged self-assembled carbon nanotube/thermoplastic resin film Download PDFInfo
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- CN103232610A CN103232610A CN2013101777304A CN201310177730A CN103232610A CN 103232610 A CN103232610 A CN 103232610A CN 2013101777304 A CN2013101777304 A CN 2013101777304A CN 201310177730 A CN201310177730 A CN 201310177730A CN 103232610 A CN103232610 A CN 103232610A
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- thermoplastic resin
- carbon nanotube
- resin membrane
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- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 64
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 64
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 229920005992 thermoplastic resin Polymers 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 claims abstract description 26
- 239000011521 glass Substances 0.000 claims abstract description 25
- 238000001704 evaporation Methods 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 230000008020 evaporation Effects 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 241000252506 Characiformes Species 0.000 claims abstract description 9
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 8
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract 2
- 239000012528 membrane Substances 0.000 claims description 38
- 238000001338 self-assembly Methods 0.000 claims description 21
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 6
- 238000002203 pretreatment Methods 0.000 claims description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 238000001879 gelation Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 11
- 229920005989 resin Polymers 0.000 abstract description 8
- 239000011347 resin Substances 0.000 abstract description 8
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 239000006185 dispersion Substances 0.000 abstract 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 238000007906 compression Methods 0.000 abstract 1
- 239000002904 solvent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000013543 active substance Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003519 biomedical and dental material Substances 0.000 description 1
- -1 carbon nano tube compound Chemical class 0.000 description 1
- 239000002238 carbon nanotube film Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
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Abstract
The invention discloses a method for preparing a directionally-arranged self-assembled carbon nanotube/thermoplastic resin film, relating to a preparation method of a carbon nanotube/thermoplastic resin film. The method is used for solving the problems of existing carbon nanotube/resin films that the forming temperature is high, the dispersion of carbon nanotubes is poor, the orientation is difficult to control, the material properties are unstable and the cost is too high. The method comprises the steps of: dissolving thermoplastic resin particles into N-methyl pyrrolidone so as to obtain a solution A; preparing a piranha solution; pre-treating a glass slide; coating the solution A on the glass slide, and forming a thermoplastic resin film after evaporation; putting carbon nanotubes into anhydrous ethanol, and adding polyvinyl pyrrolidone so as to obtain turbid liquid; preparing the thermoplastic resin film with directionally-arranged carbon nanotubes; and separating the film from the glass slide and drying. According to the method, the high-temperature thermo-compression formation is not required during preparation, and the cost is low; the distribution of the carbon nanotubes in the film has directionality, and the material properties have orientation; and the dispersion of the carbon nanotubes can be always good, and the material properties are stable.
Description
Technical field
The present invention relates to a kind of carbon nanotube/thermoplastic resin membrane's preparation method.
Background technology
The matrix material of carbon nanotube/resin has become the focus of World Science research since reports such as AJAYAN.Compound mutual supplement with each other's advantages and the reinforcement that can realize group element material of carbon nanotube and resin, the most economical special performance that effectively utilizes carbon nanotube is the effective way of carbon nanotube stabilization.Resin/carbon nano tube compound material has wide application prospect at aspects such as information material, bio-medical material, stealth material, catalyzer, high performance structures material, multifunctional materials.
Traditional carbon nanotube/resin film generally adopts blending method or coagulates the wadding method, but these methods all can't realize carbon nanotube align the formation ordered structure.And utilize the method for vapour deposition, though can realize carbon nanotube to align synthetic cost too high and can't widespread use.So seeking the preparation method that easy method prepares orientational alignment carbon nano-tube/resin film is the direction that people study.
Summary of the invention
The present invention seeks to solve existing carbon nanotube/resin film mold temperature height, the carbon nanotube bad dispersibility, be orientated wayward, the material property instability, and adopt the vapour deposition process preparation to have the too high problem of cost, and a kind of preparation method who aligns self-assembly carbon nanotube/thermoplastic resin membrane is provided.
The preparation method who aligns self-assembly carbon nanotube/thermoplastic resin membrane realizes according to the following steps:
One, 5～10g thermoplastic resin particle is dissolved in 50～100g n-methlpyrrolidone, the speed magnetic agitation dissolving extremely fully with 200～500r/min obtains solution A;
Two, be 95%～98% sulfuric acid with 30ml concentration with 10ml concentration be that 30% superoxol mixes, obtain Piranha solution;
Three, glass slide is put into the Piranha solution that step 2 obtains and soaked 5～20min, put into dehydrated alcohol and deionized water for ultrasonic then successively and handle 5min, the pre-treatment of slide glass is finished in oven dry;
Four, solution A is coated on the pretreated slide glass, puts into vacuum drying oven, be heated to 60 ℃, evaporation 4～6h forms the thermoplastic resin membrane in slide surface;
Five, 50～200mg carbon nanotube is dropped in the dehydrated alcohol, add the polyvinylpyrrolidone of 40～150mg then, supersound process 30min obtains the suspension liquid that concentration is 1mg/ml again;
Six, the slide glass that the surface is formed the thermoplastic resin membrane vertically inserts in the suspension liquid, at 60 ℃ of following evaporation at constant temperature 12h, obtains the thermoplastic resin membrane of carbon nano-tube oriented arrangement;
Seven, the thermoplastic resin membrane of carbon nano-tube oriented arrangement is immersed 30min in the deionized water, make film separate with slide glass by gelation, dry 2～5h down at 80 ℃, namely finish the preparation that aligns self-assembly carbon nanotube/thermoplastic resin membrane.
The present invention utilizes thermoplastic resin as the matrix phase, dehydrated alcohol is as the solvent of carbon nanotube, a kind of preparation method who aligns self-assembly carbon nanotube/thermoplastic resin membrane is provided, carbon nanotube aligns the formation linear pattern in capillary effect lower edge liquid level direction, and the pattern width of carbon nano-tube oriented arrangement is 10～15um.The resistivity of film is about 3.3M Ω/cm after tested.
Advantage of the present invention:
One, a kind of preparation method who aligns self-assembly carbon nanotube/thermoplastic resin membrane provided by the invention, carbon nanotube distributes and has directivity in the carbon nano-tube film that obtains, prepare the carbon nanotube resin film than traditional blending method, material property has orientation;
Two, a kind of preparation method who aligns self-assembly carbon nanotube/thermoplastic resin membrane provided by the invention, adopting evaporating solvent method realization carbon nanotube to reach by self-assembly aligns, with respect to additive methods such as Langmuir-Blodgett, equipment and environmental requirement are low, and be with low cost;
Three, a kind of preparation method who aligns self-assembly carbon nanotube/thermoplastic resin membrane provided by the invention, it is molded that preparation process need not elevated temperature heat, easy to operate;
Four, the present invention adopts dehydrated alcohol as solvent, and the water system velocity of evaporation that velocity of evaporation is more traditional is faster, and under Action of Surfactant, carbon nanotube all the time can good distribution, and material property is stable.
Description of drawings
Fig. 1 aligns self-assembly carbon nanotube/thermoplastic resin membrane's opticmicroscope figure for preparation gained among the embodiment.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the preparation method that present embodiment aligns self-assembly carbon nanotube/thermoplastic resin membrane realizes according to the following steps:
One, 5～10g thermoplastic resin particle is dissolved in 50～100g n-methlpyrrolidone, the speed magnetic agitation dissolving extremely fully with 200～500r/min obtains solution A;
Two, be 95%～98% sulfuric acid with 30ml concentration with 10ml concentration be that 30% superoxol mixes, obtain Piranha solution;
Three, glass slide is put into the Piranha solution that step 2 obtains and soaked 5～20min, put into dehydrated alcohol and deionized water for ultrasonic then successively and handle 5min, the pre-treatment of slide glass is finished in oven dry;
Four, solution A is coated on the pretreated slide glass, puts into vacuum drying oven, be heated to 60 ℃, evaporation 4～6h forms the thermoplastic resin membrane in slide surface;
Five, 50～200mg carbon nanotube is dropped in the dehydrated alcohol, add the polyvinylpyrrolidone of 40～150mg then, supersound process 30min obtains the suspension liquid that concentration is 1mg/ml again;
Six, the slide glass that the surface is formed the thermoplastic resin membrane vertically inserts in the suspension liquid, at 60 ℃ of following evaporation at constant temperature 12h, obtains the thermoplastic resin membrane of carbon nano-tube oriented arrangement;
Seven, the thermoplastic resin membrane of carbon nano-tube oriented arrangement is immersed 30min in the deionized water, make film separate with slide glass by gelation, dry 2～5h down at 80 ℃, namely finish the preparation that aligns self-assembly carbon nanotube/thermoplastic resin membrane.
Solution A is light yellow transparent solution in the present embodiment step 1.
In the present embodiment step 3 after the slide glass pre-treatment, its no organic substance residues in surface and smooth cleaning.
Form the thermoplastic resin membrane in slide surface in the present embodiment step 4, require film evenly smooth.
Polyvinylpyrrolidone uses as tensio-active agent in the present embodiment step 5.
Embodiment two: what present embodiment and embodiment one were different is in the step 1 8g thermoplastic resin particle to be dissolved in the 60g n-methlpyrrolidone, with the speed magnetic agitation of 300r/min to dissolving fully.Other step and parameter are identical with embodiment one.
Embodiment three: what present embodiment was different with embodiment one or two is to be heated to 60 ℃ in the step 4, evaporation 5h.Other step and parameter are identical with embodiment one or two.
Embodiment four: what present embodiment was different with one of embodiment one to three is in the step 5 100g carbon nanotube to be dropped in the dehydrated alcohol, adds the polyvinylpyrrolidone of 80mg then.Other step and parameter are identical with one of embodiment one to three.
Embodiment five: what present embodiment was different with one of embodiment one to four is to dry 3h down at 80 ℃ in the step 7.Other step and parameter are identical with one of embodiment one to four.
Embodiment:
The preparation method who aligns self-assembly carbon nanotube/thermoplastic resin membrane realizes according to the following steps:
One, the 10g thermoplastic resin particle is dissolved in the 50g n-methlpyrrolidone, the speed magnetic agitation dissolving extremely fully with 200r/min obtains solution A;
Two, be 98% sulfuric acid with 30ml concentration with 10ml concentration be that 30% superoxol mixes, obtain Piranha solution;
Three, glass slide is put into the Piranha solution that step 2 obtains and soaked 5min, put into dehydrated alcohol and deionized water for ultrasonic then successively and handle 5min, the pre-treatment of slide glass is finished in oven dry; Slide glass;
Four, solution A is coated on the pretreated slide glass, puts into vacuum drying oven, be heated to 60 ℃, evaporation 4h forms the thermoplastic resin membrane in slide surface;
Five, the 50mg carbon nanotube is dropped in the dehydrated alcohol, add the polyvinylpyrrolidone of 40mg then, supersound process 30min obtains the suspension liquid that concentration is 1mg/ml again;
Six, the slide glass that the surface is formed the thermoplastic resin membrane vertically inserts in the suspension liquid, at 60 ℃ of following evaporation at constant temperature 12h, obtains the thermoplastic resin membrane of carbon nano-tube oriented arrangement;
Seven, the thermoplastic resin membrane of carbon nano-tube oriented arrangement is immersed 30min in the deionized water, make film separate with slide glass by gelation, dry 2h down at 80 ℃, namely finish the preparation that aligns self-assembly carbon nanotube/thermoplastic resin membrane.
The preparation gained aligns self-assembly carbon nanotube/thermoplastic resin membrane in the present embodiment, as can be seen from Fig. 1, carbon nanotube aligns the formation linear pattern in capillary effect lower edge liquid level direction, and the pattern width of carbon nano-tube oriented arrangement is 10～15um.The resistivity of film is about 3.3M Ω/cm after tested.
Claims (5)
1. preparation method who aligns self-assembly carbon nanotube/thermoplastic resin membrane is characterized in that it realizes according to the following steps:
One, 5～10g thermoplastic resin particle is dissolved in 50～100g n-methlpyrrolidone, the speed magnetic agitation dissolving extremely fully with 200～500r/min obtains solution A;
Two, be 95%～98% sulfuric acid with 30ml concentration with 10ml concentration be that 30% superoxol mixes, obtain Piranha solution;
Three, glass slide is put into the Piranha solution that step 2 obtains and soaked 5～20min, put into dehydrated alcohol and deionized water for ultrasonic then successively and handle 5min, the pre-treatment of slide glass is finished in oven dry;
Four, solution A is coated on the pretreated slide glass, puts into vacuum drying oven, be heated to 60 ℃, evaporation 4～6h forms the thermoplastic resin membrane in slide surface;
Five, 50～200mg carbon nanotube is dropped in the dehydrated alcohol, add the polyvinylpyrrolidone of 40～150mg then, supersound process 30min obtains the suspension liquid that concentration is 1mg/ml again;
Six, the slide glass that the surface is formed the thermoplastic resin membrane vertically inserts in the suspension liquid, at 60 ℃ of following evaporation at constant temperature 12h, obtains the thermoplastic resin membrane of carbon nano-tube oriented arrangement;
Seven, the thermoplastic resin membrane of carbon nano-tube oriented arrangement is immersed 30min in the deionized water, make film separate with slide glass by gelation, dry 2～5h down at 80 ℃, namely finish the preparation that aligns self-assembly carbon nanotube/thermoplastic resin membrane.
2. a kind of preparation method who aligns self-assembly carbon nanotube/thermoplastic resin membrane according to claim 1, it is characterized in that in the step 1 8g thermoplastic resin particle being dissolved in the 60g n-methlpyrrolidone, with the speed magnetic agitation dissolving extremely fully of 300r/min.
3. a kind of preparation method who aligns self-assembly carbon nanotube/thermoplastic resin membrane according to claim 1 and 2 is characterized in that being heated in the step 4 60 ℃, evaporation 5h.
4. a kind of preparation method who aligns self-assembly carbon nanotube/thermoplastic resin membrane according to claim 3 is characterized in that in the step 5 100g carbon nanotube being dropped in the dehydrated alcohol, adds the polyvinylpyrrolidone of 80mg then.
5. a kind of preparation method who aligns self-assembly carbon nanotube/thermoplastic resin membrane according to claim 4 is characterized in that drying 3h down at 80 ℃ in the step 7.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108385371A (en) * | 2018-03-16 | 2018-08-10 | 哈尔滨工业大学 | A kind of preparation method of plant fiber cloth/resin composite materials of surface grafting carbon nanotube |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004167667A (en) * | 2002-11-01 | 2004-06-17 | Mitsubishi Rayon Co Ltd | Composition containing carbon nanotubes and method of adjusting the same, and composite matter formed of the composition and method of manufacturing the same |
| CN101289568A (en) * | 2008-06-16 | 2008-10-22 | 南昌大学 | Method for preparing cobalt-plating carbon nano-tube/epoxide resin wave- absorbing and camouflage composite material |
| WO2012119526A1 (en) * | 2011-03-04 | 2012-09-13 | 中国石油化工股份有限公司 | Electrically conductive, fully vulcanized, thermoplastic elastomer and preparation method thereof |
| CN102993603A (en) * | 2012-11-29 | 2013-03-27 | 宁波先锋新材料股份有限公司 | Polyvinyl chloride composite material with microwave absorption property and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004167667A (en) * | 2002-11-01 | 2004-06-17 | Mitsubishi Rayon Co Ltd | Composition containing carbon nanotubes and method of adjusting the same, and composite matter formed of the composition and method of manufacturing the same |
| CN101289568A (en) * | 2008-06-16 | 2008-10-22 | 南昌大学 | Method for preparing cobalt-plating carbon nano-tube/epoxide resin wave- absorbing and camouflage composite material |
| WO2012119526A1 (en) * | 2011-03-04 | 2012-09-13 | 中国石油化工股份有限公司 | Electrically conductive, fully vulcanized, thermoplastic elastomer and preparation method thereof |
| CN102993603A (en) * | 2012-11-29 | 2013-03-27 | 宁波先锋新材料股份有限公司 | Polyvinyl chloride composite material with microwave absorption property and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108385371A (en) * | 2018-03-16 | 2018-08-10 | 哈尔滨工业大学 | A kind of preparation method of plant fiber cloth/resin composite materials of surface grafting carbon nanotube |
| CN108385371B (en) * | 2018-03-16 | 2021-04-02 | 哈尔滨工业大学 | Preparation method of plant fiber cloth/resin composite material with surface grafted with carbon nano tubes |
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