CN114334226B - Preparation method of bendable polylactic acid transparent conductive film - Google Patents
Preparation method of bendable polylactic acid transparent conductive film Download PDFInfo
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- CN114334226B CN114334226B CN202210036768.9A CN202210036768A CN114334226B CN 114334226 B CN114334226 B CN 114334226B CN 202210036768 A CN202210036768 A CN 202210036768A CN 114334226 B CN114334226 B CN 114334226B
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- 229920000747 poly(lactic acid) Polymers 0.000 title claims abstract description 55
- 239000004626 polylactic acid Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 62
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 59
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000002861 polymer material Substances 0.000 claims abstract description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 16
- 239000002904 solvent Substances 0.000 claims description 13
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 238000004528 spin coating Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 7
- 238000004090 dissolution Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 230000001276 controlling effect Effects 0.000 claims description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920006381 polylactic acid film Polymers 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 229920002988 biodegradable polymer Polymers 0.000 description 1
- 239000004621 biodegradable polymer Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Abstract
The invention relates to the technical field of high polymer materials, in particular to a preparation method of a bendable polylactic acid transparent conductive film. The transparent polylactic acid/graphene film prepared by the method has excellent conductivity and bendability. In addition, the preparation method disclosed by the invention is simple and flexible, can effectively control the thickness of the film, and is beneficial to mass production.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a preparation method of a bendable polylactic acid transparent conductive film.
Background
Polylactic acid is an environmentally friendly biodegradable polymer, and is attracting attention due to its excellent mechanical properties and its hydrolysate being harmless to human body and environment. Because of the performance problems of polylactic acid, many research groups have made a great deal of effort to improve the mechanical properties and electrical conductivity of polylactic acid composite materials by adding various carbon nanotubes, such as carbon nanotubes and graphene.
Graphene is a two-dimensional nanomaterial consisting of a layer of carbon atom thickness, and has good application prospects in various application fields such as sensors, semiconductors, medical monitors and the like due to the characteristics of excellent electrical properties, high light transmittance, high specific surface area and the like. However, the graphene is unevenly dispersed in the polymer, which may cause degradation or instability of mechanical properties, electrical properties, and the like. Therefore, many scholars have studied about the surface treatment and dispersion method of nanoparticles.
Accordingly, there is a need for a method for preparing a flexible transparent conductive polylactic acid film, which solves the above-mentioned related technical problems.
Disclosure of Invention
According to the preparation method of the bendable polylactic acid transparent conductive film, the characteristics of hydrophilicity of graphene oxide are utilized, after graphene oxide is uniformly dispersed into a polylactic acid solution, the graphene oxide is reduced into graphene in a heating mode, and the bendable polylactic acid/graphene transparent conductive film is prepared and is applied to the fields of sensors, intelligent wearable electronics and the like, and has good application value.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the preparation method of the bendable polylactic acid transparent conductive film specifically comprises the following steps:
step 1, adding a certain amount of polylactic acid into a chloroform solvent to completely dissolve a high polymer material, so as to obtain a polylactic acid solution;
step 2, dispersing a certain amount of graphene oxide aqueous solution in tetrahydrofuran or chloroform solvent to uniformly disperse the graphene oxide aqueous solution, so as to obtain graphene oxide dispersion solution;
step 3, adding the graphene oxide dispersion solution in the step 2 into the polylactic acid solution in the step 1, uniformly dispersing graphene oxide in the polylactic acid at a certain temperature, and regulating and controlling the stirring temperature to effectively reduce the graphene oxide into graphene;
step 4, preparing polylactic acid/graphene films with different thicknesses by using a spin coating method;
and 5, drying the polylactic acid/graphene film obtained in the step 4, and completely volatilizing the solvent.
Preferably, in the step (1), the polylactic acid has a molecular weight of M w = 212921, the concentration of polylactic acid is 0.05-0.5 g/ml, the dissolution temperature of polylactic acid is 25 ℃, and the dissolution time is 24 hours.
Preferably, in the step (2), the concentration of graphene oxide in the graphene oxide aqueous solution is 6.2g/L, and the size is 0.5-5 μm.
Preferably, the mass dispersion of the graphene oxide in the step (3) and the step (2) is 0.1 to 3.5wt%, and the mass fraction of the polylactic acid in the step (1) is 0.1 to 3.5wt%; and (3) stirring the graphene at 40-70 ℃.
Preferably, in the step (4), the spin coating method has a spin speed of 100 to 250rpm.
Preferably, in the step (5), the drying temperature is 25 to 60 ℃.
The invention has the beneficial effects that:
1. according to the invention, the hydrophilic graphene oxide aqueous solution is utilized to uniformly disperse the graphene oxide in the polylactic acid solution, and the polylactic acid/graphene film is prepared by a spin coating method, so that the polylactic acid/graphene film has high conductivity and flexible transparent performance.
2. According to the invention, the transparency, the conductivity and the flexibility of the film can be regulated and controlled according to the concentration of the graphene oxide, the concentration of the polylactic acid, the rotation speed, the reduction temperature and time of the graphene oxide and the drying temperature and time.
3. The preparation method of the bendable polylactic acid transparent conductive film disclosed by the invention is simple and flexible, can effectively control the thickness of the film, and is beneficial to mass production.
Detailed Description
The technical scheme of the present invention is further illustrated and described below by means of specific embodiments, but the embodiments of the present invention are not limited thereto.
Example 1:
molecular weight is M w Polylactic acid= 212921 is added into chloroform solvent with the concentration of 0.05-0.5 g/ml, and is dissolved for 24 hours at 25 ℃; the graphene oxide aqueous solution is added to tetrahydrofuran or chloroform solvent to uniformly disperse it at 25 ℃. And pouring the graphene oxide solution into a polylactic acid solution, enabling the mass fraction of the polylactic acid to be 0.5wt%, uniformly stirring at 50-70 ℃ and enabling the graphene to be reduced. Polylactic acid/graphene films of different thicknesses were prepared by spin coating and dried in a vacuum oven for 24 hours.
Example 2:
molecular weight is M w Polylactic acid= 212921 is added into chloroform solvent with the concentration of 0.05-0.5 g/ml, and is dissolved for 24 hours at 25 ℃; the graphene oxide aqueous solution is added to tetrahydrofuran or chloroform solvent to uniformly disperse it at 25 ℃. The graphite oxide is treatedAnd pouring the graphene solution into the polylactic acid solution, enabling the mass fraction of the polylactic acid to be 1.5wt%, uniformly stirring at 50-70 ℃ and enabling the graphene to be reduced. Polylactic acid/graphene films of different thicknesses were prepared by spin coating and dried in a vacuum oven for 24 hours.
Example 3:
molecular weight is M w Polylactic acid= 212921 is added into chloroform solvent with the concentration of 0.05-0.5 g/ml, and is dissolved for 24 hours at 25 ℃; the graphene oxide aqueous solution is added to tetrahydrofuran or chloroform solvent to uniformly disperse it at 25 ℃. And pouring the graphene oxide solution into a polylactic acid solution, enabling the mass fraction of the polylactic acid to be 3.5wt%, uniformly stirring at 50-70 ℃ and enabling the graphene to be reduced. Polylactic acid/graphene films of different thicknesses were prepared by spin coating and dried in a vacuum oven for 24 hours.
Comparative example 1:
molecular weight is M w Polylactic acid= 212921 was added to chloroform solvent at a concentration of 0.05 to 0.5g/ml, and after 24 hours of dissolution at 25 ℃, stirring was continued uniformly at 50 to 70 ℃. Polylactic acid films of different thicknesses were prepared by spin coating and dried in a vacuum oven for 24 hours.
And (3) performance detection:
1. and (3) detecting the dispersity: the dispersity of the polylactic acid/graphene film prepared by the embodiment is detected by a Raman spectrometer;
2. and (3) detecting crystallinity: the crystallinity of the polylactic acid/graphene film prepared in this example was detected using an X-ray diffractometer and a differential scanning calorimeter;
3. conducting performance test: the polylactic acid/graphene film prepared in this example was prepared into a 10cm x 10cm sample according to ASTM D257 standard, and the conductivity performance test was performed at 100 volts.
TABLE 1
The test result shows that the conductivity of the film is improved along with the increase of the concentration of the graphene, and the opposite dispersity and transparency are reduced along with the increase of the concentration of the graphene.
Application field: the polylactic acid/graphene bendable conductive transparent film prepared by the invention is applied to the fields of sensors, intelligent wearable electronics and the like by regulating and controlling the thickness, conductivity, flexibility and other performances of the film. Therefore, the method has good application value.
It should be noted that, not described in detail, the present invention is well known to those skilled in the art.
The above embodiments are only for further illustrating the embodiments of the present invention, but the present invention is not limited to the above embodiments, and all the equivalent changes and modifications made in the above embodiments are included in the scope of the present invention according to the technical spirit of the present invention.
Claims (1)
1. The preparation method of the bendable polylactic acid transparent conductive film is characterized by comprising the following steps of:
step 1, adding a certain amount of polylactic acid into a chloroform solvent to completely dissolve a high polymer material, so as to obtain a polylactic acid solution;
step 2, dispersing a certain amount of graphene oxide aqueous solution in tetrahydrofuran or chloroform solvent to uniformly disperse the graphene oxide aqueous solution, so as to obtain graphene oxide dispersion solution;
step 3, adding the graphene oxide dispersion solution in the step 2 into the polylactic acid solution in the step 1, uniformly dispersing graphene oxide in the polylactic acid at a certain temperature, and regulating and controlling the stirring temperature to effectively reduce the graphene oxide into graphene;
step 4, preparing polylactic acid/graphene films with different thicknesses by using a spin coating method;
step 5, drying the polylactic acid/graphene film obtained in the step 4 to completely volatilize the solvent;
in the step 1, the molecular weight of the polylactic acid is M w = 212921, the concentration of polylactic acid is 0.05-0.5 g/ml, the dissolution temperature of polylactic acid is 25 ℃, and the dissolution time is 24 hours;
in the step 2, the concentration of graphene oxide in the graphene oxide aqueous solution is 6.2g/L, and the size is 0.5-5 mu m;
the mass dispersion of the graphene oxide in the step 3 and the step 2 is 0.1 to 3.5 weight percent, and the mass fraction of the polylactic acid in the step 1 is 0.1 to 3.5 weight percent; the stirring temperature and the graphene reduction temperature in the step 3 are 40-70 ℃;
in the step 4, the rotation speed of the spin coating method is 100-250 rpm;
in the step 5, the drying temperature is 25-60 ℃.
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| CN114334226B true CN114334226B (en) | 2024-01-09 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167894A (en) * | 2011-01-24 | 2011-08-31 | 中国科学院长春应用化学研究所 | Graphene/polylactic acid composite material and preparation method thereof |
| CN103578771A (en) * | 2012-07-18 | 2014-02-12 | 海洋王照明科技股份有限公司 | Graphene thin film and preparation method and application thereof |
| CN103788604A (en) * | 2012-10-29 | 2014-05-14 | 山东科技大学 | Novel polylactic acid microspheres and preparation method thereof |
| CN105732038A (en) * | 2016-01-15 | 2016-07-06 | 东南大学 | Highly conductive flexible self-supported graphene film and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101388695B1 (en) * | 2011-10-24 | 2014-04-28 | 삼성전기주식회사 | Graphene transparent electrode and method for manufacturing the same |
| KR101297423B1 (en) * | 2011-11-30 | 2013-08-14 | 한국전기연구원 | High concentration and stable dispersion of reduced graphene oxide by cation-pi interaction and the manufacturing method thereby |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167894A (en) * | 2011-01-24 | 2011-08-31 | 中国科学院长春应用化学研究所 | Graphene/polylactic acid composite material and preparation method thereof |
| CN103578771A (en) * | 2012-07-18 | 2014-02-12 | 海洋王照明科技股份有限公司 | Graphene thin film and preparation method and application thereof |
| CN103788604A (en) * | 2012-10-29 | 2014-05-14 | 山东科技大学 | Novel polylactic acid microspheres and preparation method thereof |
| CN105732038A (en) * | 2016-01-15 | 2016-07-06 | 东南大学 | Highly conductive flexible self-supported graphene film and preparation method thereof |
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