CN103232610B - 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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- CN103232610B CN103232610B CN201310177730.4A CN201310177730A CN103232610B CN 103232610 B CN103232610 B CN 103232610B CN 201310177730 A CN201310177730 A CN 201310177730A CN 103232610 B CN103232610 B CN 103232610B
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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 21
- 239000011521 glass Substances 0.000 claims abstract description 25
- 238000002360 preparation method Methods 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001704 evaporation Methods 0.000 claims abstract description 13
- 230000008020 evaporation Effects 0.000 claims abstract description 12
- 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
- 238000001338 self-assembly Methods 0.000 claims description 21
- 239000012528 membrane Substances 0.000 claims description 17
- 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
- -1 by gelation Substances 0.000 claims description 5
- 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
- 238000007654 immersion Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 10
- 229920005989 resin Polymers 0.000 abstract description 8
- 239000011347 resin Substances 0.000 abstract description 8
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 238000007906 compression Methods 0.000 abstract description 2
- 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
- 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
- 239000002238 carbon nanotube film Substances 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
- 239000000126 substance Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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 preparation method of carbon nanotube/thermoplastic resin film.
Background technology
The matrix material of carbon nanotube/resin has become the focus of World Science research since the reports such as AJAYAN.The compound of carbon nanotube and resin can realize mutual supplement with each other's advantages and the reinforcement of group element material, and the most economical special performance effectively utilizing carbon nanotube is the effective way of carbon nanotubes.Resin/carbon nano tube compound material has broad application prospects in information material, bio-medical material, stealth material, catalyzer, high performance structures material, multifunctional material etc.
Traditional carbon nanotube/resin film, general adopts blending method or solidifying wadding method, but these methods all cannot realize aligning of carbon nanotube is formed with sequence structure.And utilize the method for vapour deposition, although can realize carbon nanotube align synthesis high cost and cannot widespread use.So finding 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 high, carbon nanotube dispersed is poor, orientation is wayward, material property is unstable, and adopt vapour deposition process preparation to there is the problem of high cost, and a kind of preparation method aligning self-assembly carbon nanotube/thermoplastic resin film is provided.
The preparation method aligning self-assembly carbon nanotube/thermoplastic resin film realizes according to the following steps:
One, 5 ~ 10g thermoplastic resin particle being dissolved in 50 ~ 100g n-methlpyrrolidone, with the speed magnetic agitation of 200 ~ 500r/min to dissolving completely, obtaining solution A;
Two, by 30ml concentration be 95% ~ 98% sulfuric acid and 10ml concentration be 30% superoxol mixes, obtain Piranha solution;
Three, glass slide is put into Piranha solution immersion 5 ~ 20min that step 2 obtains, then put into dehydrated alcohol and deionized water for ultrasonic process 5min successively, dry, complete the pre-treatment of slide glass;
Four, solution A be coated on pretreated slide glass, put into vacuum drying oven, be heated to 60 DEG C, evaporation 4 ~ 6h, forms thermoplastic resin membrane in slide surface;
Five, 50 ~ 200mg carbon nanotube is dropped in dehydrated alcohol, then add the polyvinylpyrrolidone of 40 ~ 150mg, then supersound process 30min, obtain the suspension liquid that concentration is 1mg/ml;
Six, slide glass surface being formed thermoplastic resin membrane vertically inserts in suspension liquid, and evaporation at constant temperature 12h at 60 DEG C, 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 deionized water, by gelation, film is separated with slide glass, at 80 DEG C, dry 2 ~ 5h, namely complete the preparation aligning self-assembly carbon nanotube/thermoplastic resin film.
The present invention utilizes thermoplastic resin as matrix phase, dehydrated alcohol is as the solvent of carbon nanotube, provide a kind of preparation method aligning self-assembly carbon nanotube/thermoplastic resin film, carbon nanotube aligns formation linear pattern along liquid level direction under capillary effect, 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 aligning self-assembly carbon nanotube/thermoplastic resin film provided by the invention, in the carbon nano-tube film obtained, carbon nanotube distribution has directivity, prepare carbon nanotube resin film compared to traditional blending method, material property has orientation;
Two, a kind of preparation method aligning self-assembly carbon nanotube/thermoplastic resin film provided by the invention, adopt evaporating solvent method to realize carbon nanotube to be reached by self-assembly and align, relative to additive methods such as Langmuir-Blodgett, equipment and environmental requirement low, with low cost;
Three, a kind of preparation method aligning self-assembly carbon nanotube/thermoplastic resin film provided by the invention, preparation process is without the need to high-temperature thermo-compression formation, easy to operate;
Four, the present invention adopts dehydrated alcohol as solvent, and the more traditional water system velocity of evaporation of velocity of evaporation is faster, and under Action of Surfactant, carbon nanotube all the time can good distribution, strong mechanical property.
Accompanying drawing explanation
Fig. 1 prepares the opticmicroscope figure that gained aligns self-assembly carbon nanotube/thermoplastic resin film in 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 film realizes according to the following steps:
One, 5 ~ 10g thermoplastic resin particle being dissolved in 50 ~ 100g n-methlpyrrolidone, with the speed magnetic agitation of 200 ~ 500r/min to dissolving completely, obtaining solution A;
Two, by 30ml concentration be 95% ~ 98% sulfuric acid and 10ml concentration be 30% superoxol mixes, obtain Piranha solution;
Three, glass slide is put into Piranha solution immersion 5 ~ 20min that step 2 obtains, then put into dehydrated alcohol and deionized water for ultrasonic process 5min successively, dry, complete the pre-treatment of slide glass;
Four, solution A be coated on pretreated slide glass, put into vacuum drying oven, be heated to 60 DEG C, evaporation 4 ~ 6h, forms thermoplastic resin membrane in slide surface;
Five, 50 ~ 200mg carbon nanotube is dropped in dehydrated alcohol, then add the polyvinylpyrrolidone of 40 ~ 150mg, then supersound process 30min, obtain the suspension liquid that concentration is 1mg/ml;
Six, slide glass surface being formed thermoplastic resin membrane vertically inserts in suspension liquid, and evaporation at constant temperature 12h at 60 DEG C, 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 deionized water, by gelation, film is separated with slide glass, at 80 DEG C, dry 2 ~ 5h, namely complete the preparation aligning self-assembly carbon nanotube/thermoplastic resin film.
In present embodiment step one, solution A is light yellow transparent solution.
In present embodiment step 3 after slide glass pre-treatment, its surface is without organic substance residues and smooth pieces.
Form thermoplastic resin membrane in slide surface in present embodiment step 4, require film uniform ground.
In present embodiment step 5, polyvinylpyrrolidone uses as tensio-active agent.
Embodiment two: 8g thermoplastic resin particle is dissolved in 60g n-methlpyrrolidone unlike in step one by present embodiment and embodiment one, with the speed magnetic agitation of 300r/min to dissolving completely.Other step and parameter identical with embodiment one.
Embodiment three: present embodiment and embodiment one or two, unlike being heated to 60 DEG C in step 4, evaporate 5h.Other step and parameter identical with embodiment one or two.
Embodiment four: 100g carbon nanotube drops in dehydrated alcohol unlike in step 5 by one of present embodiment and embodiment one to three, then adds the polyvinylpyrrolidone of 80mg.Other step and parameter identical with one of embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four dry 3h unlike in step 7 at 80 DEG C.Other step and parameter identical with one of embodiment one to four.
Embodiment:
The preparation method aligning self-assembly carbon nanotube/thermoplastic resin film realizes according to the following steps:
One, 10g thermoplastic resin particle being dissolved in 50g n-methlpyrrolidone, with the speed magnetic agitation of 200r/min to dissolving completely, obtaining solution A;
Two, by 30ml concentration be 98% sulfuric acid and 10ml concentration be 30% superoxol mixes, obtain Piranha solution;
Three, glass slide is put into the Piranha solution that step 2 obtains and soak 5min, then put into dehydrated alcohol and deionized water for ultrasonic process 5min successively, dry, complete the pre-treatment of slide glass; Slide glass;
Four, solution A be coated on pretreated slide glass, put into vacuum drying oven, be heated to 60 DEG C, evaporation 4h, forms thermoplastic resin membrane in slide surface;
Five, 50mg carbon nanotube is dropped in dehydrated alcohol, then add the polyvinylpyrrolidone of 40mg, then supersound process 30min, obtain the suspension liquid that concentration is 1mg/ml;
Six, slide glass surface being formed thermoplastic resin membrane vertically inserts in suspension liquid, and evaporation at constant temperature 12h at 60 DEG C, 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 deionized water, by gelation, film is separated with slide glass, at 80 DEG C, dry 2h, namely complete the preparation aligning self-assembly carbon nanotube/thermoplastic resin film.
Prepare gained in the present embodiment and align self-assembly carbon nanotube/thermoplastic resin film, as can be seen from Fig. 1, carbon nanotube aligns formation linear pattern along liquid level direction under capillary effect, 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. align a preparation method for self-assembly carbon nanotube/thermoplastic resin film, it is characterized in that it realizes according to the following steps:
One, 5 ~ 10g thermoplastic resin particle being dissolved in 50 ~ 100g n-methlpyrrolidone, with the speed magnetic agitation of 200 ~ 500r/min to dissolving completely, obtaining solution A;
Two, by 30ml concentration be 95% ~ 98% sulfuric acid and 10ml concentration be 30% superoxol mixes, obtain Piranha solution;
Three, glass slide is put into Piranha solution immersion 5 ~ 20min that step 2 obtains, then put into dehydrated alcohol and deionized water for ultrasonic process 5min successively, dry, complete the pre-treatment of slide glass;
Four, solution A be coated on pretreated slide glass, put into vacuum drying oven, be heated to 60 DEG C, evaporation 4 ~ 6h, forms thermoplastic resin membrane in slide surface;
Five, 50 ~ 200mg carbon nanotube is dropped in dehydrated alcohol, then add the polyvinylpyrrolidone of 40 ~ 150mg, then supersound process 30min, obtain the suspension liquid that concentration is 1mg/ml;
Six, slide glass surface being formed thermoplastic resin membrane vertically inserts in suspension liquid, and evaporation at constant temperature 12h at 60 DEG C, 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 deionized water, by gelation, film is separated with slide glass, at 80 DEG C, dry 2 ~ 5h, namely complete the preparation aligning self-assembly carbon nanotube/thermoplastic resin film.
2. a kind of preparation method aligning self-assembly carbon nanotube/thermoplastic resin film according to claim 1, it is characterized in that in step one, 8g thermoplastic resin particle being dissolved in 60g n-methlpyrrolidone, with the speed magnetic agitation of 300r/min to dissolving completely.
3. a kind of preparation method aligning self-assembly carbon nanotube/thermoplastic resin film according to claim 1 and 2, is characterized in that being heated to 60 DEG C in step 4, evaporation 5h.
4. a kind of preparation method aligning self-assembly carbon nanotube/thermoplastic resin film according to claim 3, is characterized in that being dropped in dehydrated alcohol by 100g carbon nanotube in step 5, then adds the polyvinylpyrrolidone of 80mg.
5. a kind of preparation method aligning self-assembly carbon nanotube/thermoplastic resin film according to claim 4, is characterized in that at 80 DEG C, drying 3h in step 7.
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