CN114334226A - 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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- CN114334226A CN114334226A CN202210036768.9A CN202210036768A CN114334226A CN 114334226 A CN114334226 A CN 114334226A CN 202210036768 A CN202210036768 A CN 202210036768A CN 114334226 A CN114334226 A CN 114334226A
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- polylactic acid
- graphene oxide
- graphene
- bendable
- transparent conductive
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- 229920000747 poly(lactic acid) Polymers 0.000 title claims abstract description 61
- 239000004626 polylactic acid Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 63
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 61
- 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 17
- 238000000034 method Methods 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 claims description 12
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 10
- 238000004528 spin coating Methods 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 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
- 238000004090 dissolution Methods 0.000 claims description 4
- 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
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 21
- 238000012360 testing method Methods 0.000 description 3
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 238000001514 detection method Methods 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
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 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
- 229920006381 polylactic acid film Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
- Non-Insulated Conductors (AREA)
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 invention 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 large-scale 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 receiving attention because of its excellent mechanical properties and its hydrolysis products being harmless to the human body and the environment. Due to the performance problems of polylactic acid, many research groups have made extensive efforts to improve the mechanical properties and electrical conductivity of polylactic acid composites by adding various carbon nanotubes, such as carbon nanotubes and graphene.
Graphene is a two-dimensional nanomaterial composed of a layer of carbon atoms, and has good application prospects in various application fields such as sensors, semiconductors and medical monitors due to the characteristics of excellent electrical properties, high light transmittance, high specific surface area and the like. However, the graphene is not uniformly dispersed in the polymer, and thus, mechanical properties, electrical properties, and the like are degraded or unstable. Therefore, many researchers have studied on the surface treatment and dispersion methods of nanoparticles.
Therefore, there is a need for a method for preparing a flexible transparent conductive film of polylactic acid, which solves the above-mentioned problems.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a bendable polylactic acid transparent conductive film, which is characterized in that graphene oxide is uniformly dispersed in a polylactic acid solution by utilizing the characteristic of hydrophilicity of the graphene oxide, and the graphene oxide is reduced into graphene in a heating mode to prepare the bendable polylactic acid/graphene conductive transparent film.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a 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 to obtain a polylactic acid solution;
step 2, dispersing a certain amount of graphene oxide aqueous solution in tetrahydrofuran or chloroform solvent, and uniformly dispersing the graphene oxide aqueous solution to obtain a graphene oxide dispersion solution;
step 3, adding the graphene oxide dispersion solution obtained in the step 2 into the polylactic acid solution obtained in the step 1, uniformly dispersing graphene oxide in 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 to completely volatilize the solvent.
Preferably, in the step (1), the molecular weight of the polylactic acid is Mw212921, 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 the graphene oxide in the graphene oxide aqueous solution is 6.2g/L, and the size of the graphene oxide aqueous solution is 0.5-5 μm.
Preferably, the mass dispersion of the graphene oxide in the step (3) and the step (2) is 0.1-3.5 wt%, and the mass fraction of the polylactic acid in the step (1) is 0.1-3.5 wt%; and (4) in the step (3), the stirring temperature and the graphene reduction temperature are 40-70 ℃.
Preferably, in the step (4), the spin coating is performed at a rotation speed of 100 to 250 rpm.
Preferably, in the step (5), the drying temperature is 25-60 ℃.
The invention has the beneficial effects that:
1. according to the invention, a hydrophilic graphene oxide aqueous solution is utilized, graphene oxide is uniformly dispersed in a polylactic acid solution, and a polylactic acid/graphene film is prepared by a spin coating method, wherein the polylactic acid/graphene film not only has high conductivity, but also has a flexible transparent property.
2. According to the invention, the transparency, conductivity and flexibility of the film can be regulated and controlled according to the concentration of the graphene oxide, the concentration of 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 large-scale production.
Detailed Description
The technical solutions of the present invention are further illustrated and described below by specific embodiments, but the embodiments of the present invention are not limited thereto.
Example 1:
molecular weight MwAdding 212921-polylactic acid into a chloroform solvent at a concentration of 0.05-0.5 g/ml, and dissolving for 24 hours at 25 ℃; adding the graphene oxide aqueous solution into a tetrahydrofuran or chloroform solvent, and uniformly dispersing at 25 ℃. And pouring the graphene oxide solution into a polylactic acid solution to enable the mass fraction of polylactic acid to be 0.5 wt%, uniformly stirring at 50-70 ℃ and reducing graphene. Polylactic acid/graphene films with different thicknesses are prepared by a spin coating method and dried in a vacuum box for 24 hours.
Example 2:
molecular weight MwAdding 212921-polylactic acid into a chloroform solvent at a concentration of 0.05-0.5 g/ml, and dissolving for 24 hours at 25 ℃; adding the graphene oxide aqueous solution into a tetrahydrofuran or chloroform solvent, and uniformly dispersing at 25 ℃. And pouring the graphene oxide solution into a polylactic acid solution to enable the mass fraction of polylactic acid to be 1.5 wt%, uniformly stirring at 50-70 ℃ and reducing graphene. Polylactic acid/graphene films with different thicknesses are prepared by a spin coating method and dried in a vacuum box for 24 hours.
Example 3:
molecular weight MwAdding 212921-polylactic acid into a chloroform solvent at a concentration of 0.05-0.5 g/ml, and dissolving for 24 hours at 25 ℃; adding the graphene oxide aqueous solution into a tetrahydrofuran or chloroform solvent, and uniformly dispersing at 25 ℃. And pouring the graphene oxide solution into a polylactic acid solution to ensure that the mass fraction of the polylactic acid is 3.5 wt%, uniformly stirring at 50-70 ℃ and reducing the graphene. Polylactic acid/graphene films with different thicknesses are prepared by a spin coating method and dried in a vacuum box for 24 hours.
Comparative example 1:
molecular weight MwAdding 212921-polylactic acid into chloroform solvent at the concentration of 0.05-0.5 g/ml, dissolving for 24 hours at 25 ℃, and then continuing to stir evenly at 50-70 ℃. 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. detecting the dispersion degree: detecting the dispersion degree of the polylactic acid/graphene film prepared by the embodiment by using a Raman spectrometer;
2. and (3) detecting the crystallinity: carrying out crystallinity detection on the polylactic acid/graphene film prepared in the embodiment by using an X-ray diffractometer and a differential scanning calorimeter;
3. and (3) testing the conductivity: the polylactic acid/graphene thin film prepared in this example was prepared into 10cm by 10cm samples according to the ASTM D257 standard, and the conductivity test was performed at 100 v.
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 dispersity and the transparency are reduced along with the increase of the concentration of the graphene.
The application field is as follows: 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 properties of the film. Therefore, the method has good application value.
It is to be noted that the present invention is not described in detail, and is well known to those skilled in the art.
The above examples are only intended to further illustrate the embodiments of the present invention, but the present invention is not limited to the above examples, and all equivalent changes and modifications made to the above examples are included in the scope of the present invention according to the technical spirit of the present invention.
Claims (6)
1. A preparation method of a bendable polylactic acid transparent conductive film is characterized by comprising the following steps:
step 1, adding a certain amount of polylactic acid into a chloroform solvent to completely dissolve a high polymer material to obtain a polylactic acid solution;
step 2, dispersing a certain amount of graphene oxide aqueous solution in tetrahydrofuran or chloroform solvent, and uniformly dispersing the graphene oxide aqueous solution to obtain a graphene oxide dispersion solution;
step 3, adding the graphene oxide dispersion solution obtained in the step 2 into the polylactic acid solution obtained in the step 1, uniformly dispersing graphene oxide in 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 to completely volatilize the solvent.
2. The method for preparing a bendable polylactic acid transparent conductive film according to claim 1, wherein in the step (1), the molecular weight of polylactic acid is Mw212921, 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.
3. The method for preparing a bendable polylactic acid transparent conductive film according to claim 1, wherein in the step (2), the concentration of graphene oxide in the graphene oxide aqueous solution is 6.2g/L, and the size of the graphene oxide aqueous solution is 0.5-5 μm.
4. The preparation method of the bendable polylactic acid transparent conductive film according to claim 1, wherein the graphene oxide in the steps (3) and (2) is dispersed by mass in an amount of 0.1 to 3.5 wt%, and the polylactic acid in the step (1) is present in an amount of 0.1 to 3.5 wt%; and (4) in the step (3), the stirring temperature and the graphene reduction temperature are 40-70 ℃.
5. The method for preparing a bendable polylactic acid transparent conductive film according to claim 1, wherein in the step (4), the spin coating speed is 100-250 rpm.
6. The method for preparing a bendable polylactic acid transparent conductive film according to claim 1, wherein in the step (5), the drying temperature is 25-60 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210036768.9A CN114334226B (en) | 2022-01-11 | 2022-01-11 | Preparation method of bendable polylactic acid transparent conductive film |
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| CN202210036768.9A CN114334226B (en) | 2022-01-11 | 2022-01-11 | Preparation method of bendable polylactic acid transparent conductive film |
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| CN114334226A true CN114334226A (en) | 2022-04-12 |
| CN114334226B CN114334226B (en) | 2024-01-09 |
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Citations (6)
| 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 |
| US20130133925A1 (en) * | 2011-10-24 | 2013-05-30 | Samsung Electro-Mechanics Co., Ltd. | Graphene transparent electrode and method for manufacturing the same |
| 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 |
| US20140323596A1 (en) * | 2011-11-30 | 2014-10-30 | Korea Electrotechnology Research Institute | Graphene oxide reduced material dispersed at high concentration by cation-ii interaction and method for manufacturing same |
| 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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2022
- 2022-01-11 CN CN202210036768.9A patent/CN114334226B/en active Active
Patent Citations (6)
| 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 |
| US20130133925A1 (en) * | 2011-10-24 | 2013-05-30 | Samsung Electro-Mechanics Co., Ltd. | Graphene transparent electrode and method for manufacturing the same |
| US20140323596A1 (en) * | 2011-11-30 | 2014-10-30 | Korea Electrotechnology Research Institute | Graphene oxide reduced material dispersed at high concentration by cation-ii interaction and method for manufacturing same |
| 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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