CN115232337A - Preparation method of light-operated multifunctional P (VDF-TrFE) composite film - Google Patents
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Abstract
The invention discloses a preparation method of a light-operated multifunctional P (VDF-TrFE) composite film. The method comprises the steps of uniformly dissolving P (VDF-TrFE) powder in N, N-dimethylformamide, and adding prepared MAPbI 3 And uniformly stirring the precursor solution, taking a proper amount of the solution, spin-coating the solution on a substrate, and annealing to obtain the light-controlled multifunctional P (VDF-TrFE) composite film. The composite film obtained by the invention has obviously enhanced light absorption under the illumination condition and the composite productThe film coercive field is reduced along with the increase of light intensity through the stress effect by the photo-induced stretching effect, and the ferroelectric polarization strength is kept unchanged, so that the film has the multifunctionality of force, electricity and optical coupling. The composite film has important application prospect in the fields of optical sensing devices, electronic functional devices and the like.
Description
Technical Field
The invention relates to the field of organic ferroelectric sensing materials, in particular to a preparation method of a light-operated multifunctional P (VDF-TrFE) composite film.
Background
In the research of the fields of intelligent perception sensors, robot control systems, biomedical tissue imaging, field effect transistors, nano generators and the like, the flexible organic ferroelectric polymer material occupies a great position. At present, in the preparation process of electronic devices, diversified and multifunctional applications are more and more emphasized, so that the requirements on the multifunctional research and development of the organic ferroelectric sensing material are provided. Vinylidene fluoride-trifluoroethylene copolymer (P (VDF-TrFE)) is one of the organic materials with the best ferroelectric piezoelectric performance, and has the advantages of good flexibility, corrosion resistance, low density, low acoustic impedance and the like, and is receiving more and more attention. However, in the current research, P (VDF-TrFE) only shows the response in the infrared band, and cannot realize the optical response in the visible band, and meanwhile, the research on the multifunctional effect of force, electricity and optical coupling is lacked, so that the application of P (VDF-TrFE) in electronic, optical and acoustic sensing devices is greatly restricted.
Disclosure of Invention
The invention aims to provide a light-operated multifunctional P (VDF-TrFE) composite film and a preparation method thereof aiming at the defects of the prior art.
The purpose of the invention is realized by the following technical scheme: a preparation method of a light-operated multifunctional P (VDF-TrFE) composite film comprises the following steps:
(1) Dissolving 1.05-4.74g of P (VDF-TrFE) powder in 10-20ml of N, N-dimethylformamide, and stirring to obtain a uniform solution;
(2) Taking PbI with a molar ratio of 1 2 Dissolving MAI in N, N-dimethylformamide, heating in 55-65 deg.C water bath, and stirring to obtain uniform MAPbI 3 Precursor solution;
(3) Taking a proper amount of MAPbI obtained in the step (2) 3 Adding the precursor solution into the uniform solution obtained in the step (1), and fully stirring and mixing to obtain MAPBI 3 a/P (VDF-TrFE) precursor solution; the MAPbi 3 The mass ratio of the precursor solute to the P (VDF-TrFE) powder is 1-20;
(4) Taking the MAPBI obtained in the step (3) 3 Dripping a VDF-TrFE precursor solution on a substrate, spin-coating on a spin coater at the speed of 500-1000rpm for 3-10s, and spin-coating at the speed of 1500-3000rpm for 30-60s to obtain a spin-coated sample;
(5) And annealing the spin-coated sample to obtain the light-controlled multifunctional P (VDF-TrFE) composite film.
Further, the optimal temperature for heating the water bath in the step (2) is 60 ℃.
Further, the substrate used in the step (4) is a transparent glass substrate.
Specifically, the temperature of the annealing treatment in the step (5) is controlled to be 100-120 ℃, and the time of the annealing treatment is 1-2 hours.
The invention has the following beneficial effects:
the preparation method has simple preparation process and easy control of the process, and MAPbI is contained in the prepared composite film 3 The crystals are uniformly dispersed in the P (VDF-TrFE) film matrix. The absorption edge test results of the composite film samples confirm that the P (VDF-TrFE) film produces a stronger light absorption capacity after compounding. When the material is subjected to a ferroelectric property test under illumination, the result shows that the material is subjected to MAPbI 3 The coercive field of the film under illumination becomes smaller when the content is increased, and MAPbI is added 3 When the mass of (2) is 15% of the mass of the P (VDF-TrFE) powder, the coercive field of the composite film under laser irradiation at 532nm increases with the laser intensityThe saturation ferroelectric polarization intensity and the ferroelectric residual polarization intensity of the film are unchanged, and the photoelectric response process is verified to be reversible through a cycle experiment. Further, the addition of MAPbI was found by in situ X-ray diffraction (XRD) experiments under light 3 Sample (5%) by mass of the P (VDF-TrFE) powder was irradiated with a laser beam at 532nm (637 mW/cm) 2 ) Environment of (3), MAPbI 3 The diffraction peak corresponding to the (310) crystal face of the crystal generates 0.02 DEG peak position left shift, namely 0.171pm lattice expansion, and the photo-induced stretching effect is generated. A large number of expansion experiments show that the stress generated by the photoinduced stretching causes the phenomenon that the coercive field of the composite film changes under illumination, thereby realizing the coupling effect of the force, electricity and light of the composite film.
Drawings
FIG. 1 is MAPbI 3 A micro-topography of a/P (VDF-TrFE) composite film, wherein a is an SEM image of the surface of the composite film, and b is an SEM image of the cross section of the composite film;
FIG. 2 is MAPbI 3 Graph comparing absorption edge of the/P (VDF-TrFE) composite film with that of the pure P (VDF-TrFE);
FIG. 3 is MAPbI 3 A ferroelectric hysteresis loop comparison graph of the/P (VDF-TrFE) composite film before and after laser irradiation;
FIG. 4 is MAPbI 3 A graph showing the change of the/P (VDF-TrFE) composite film and the pure P (VDF-TrFE) film before and after the laser irradiation;
FIG. 5 is a XRD peak position variation curve of crystal plane of the complex (310) before and after irradiation and after returning to dark room.
Detailed Description
The technical scheme of the invention is further illustrated by the following examples.
The experimental procedures described in the following examples are conventional unless otherwise specified, and the reagents and materials, unless otherwise specified, are commercially available.
Example 1
A preparation method of a light-operated multifunctional P (VDF-TrFE) composite film comprises the following steps:
(1) 1.67g of P (VDF-TrFE) powder was dissolved in 10ml of N, N-dimethylformamide and magnetically stirred to form a uniform solution;
(2) Taking PbI with a molar ratio of 1 2 Dissolving MAI in N, N-dimethylformamide, heating in 55-65 deg.C water bath, and stirring to obtain uniform MAPbI 3 Precursor solution;
(3) Taking 110 mu L of MAPbI obtained in the step (2) 3 Adding the precursor solution into the uniform solution obtained in the step (1), and fully stirring and mixing to obtain MAPBI 3 a/P (VDF-TrFE) precursor solution; the MAPbi 3 The mass ratio of the precursor solute to the P (VDF-TrFE) powder is 1-20;
4) Taking the MAPBI obtained in the step (3) 3 Dripping a VDF-TrFE precursor solution on a substrate, spin-coating on a spin coater at the speed of 500-1000rpm for 3-10s, and spin-coating at the speed of 1500-3000rpm for 30-60s to obtain a spin-coated sample;
5) And annealing the spin-coated sample to obtain the light-controlled multifunctional P (VDF-TrFE) composite film with different mass ratios.
The different mass ratios, MAPbI taken in step (3) 3 The ratio of the mass of solute in the precursor solution to the mass of the whole composite film.
Further, the optimal temperature for heating the water bath in the step (2) is 60 ℃.
Further, the substrate used in the step (4) is a transparent glass base.
Specifically, the temperature of the annealing treatment in the step (5) is controlled to be 100-120 ℃, and the time of the annealing treatment is 1-2 hours.
The light-operated multifunctional P (VDF-TrFE) composite film prepared by the method has MAPbI shown in figure 1 3 A micro-topography of a/P (VDF-TrFE) composite film, wherein a is a Scanning Electron Microscope (SEM) image of the surface of the composite film, and b is a scanning electron microscope image of the cross section of the film;
from the graph a in FIG. 1, it can be seen that the platelet structure of P (VDF-TrFE) is not due to MAPbI 3 The complex is destroyed by addition, and MAPbI can be seen in panel b of FIG. 1 3 Crystals are preferably allThe uniform dispersion is coated in the interior of P (VDF-TrFE) platelet, no agglomeration phenomenon is generated, and the size is about 55 nm. MAPbI prepared as in FIG. 2 3 The absorption edge comparison graph of the/P (VDF-TrFE) composite film and the pure P (VDF-TrFE) film shows that the composite film prepared in this example generates stronger light absorption compared with the pure P (VDF-TrFE) film, and combined with the subsequent examples, with MAPbI 3 The light absorption capacity of the composite film is gradually enhanced by increasing the adding proportion.
For MAPbI prepared in this example 3 Subjecting the/P (VDF-TrFE) composite film to 532nm laser (637 mW/cm) 2 ) As shown in FIG. 3, the coercive field of the composite film before laser irradiation is 39.05 MV/m (mean value of positive and negative coercive fields), and after irradiation, the coercive field is 36.41MV/m (mean value of positive and negative coercive fields), the coercive field is reduced by about 6.8%, and the residual polarization intensity before and after irradiation is 8.97 μ C/cm 2 And 8.95. Mu.C/cm 2 Basically, it can be considered that the light is kept unchanged before and after the illumination. The experiment of a control group shows that the coercive field and the ferroelectric remanent polarization of a pure P (VDF-TrFE) film are kept unchanged before and after illumination. Further, as shown in fig. 4, MAPbI in the present embodiment 3 The coercive field of the/P (VDF-TrFE) composite film is continuously reduced along with the continuous increase of the illumination intensity. In combination with the sample performance characterization in examples 2,3, it was found that MAPbI was associated with the complex 3 The coercive field of the composite film is reduced more obviously when the addition amount is increased, and when the composite MAPbI is adopted 3 637mW/cm when the addition is 15wt% 2 Under the irradiation of light intensity, the coercive field is reduced by about 10.7%, and a large number of development experiments also show that the change of the photoinduced coercive field is reversible. Thus, MAPbI 3 the/P (VDF-TrFE) composite film realizes photoresponse, and the coercive field is reduced under the condition that the ferroelectric property is kept unchanged.
As shown in FIG. 5, for the MAPbI in the present embodiment 3 Subjecting the/P (VDF-TrFE) composite film to 532nm laser (with maximum intensity of 637 mW/cm) 2 ) XRD characterization under irradiation showed MAPbI at 31.87 ° 3 (310) The diffraction peak corresponding to the crystal face generates a left shift of 0.02 DEG under the illumination condition, and is arranged after the illumination is finishedThe original peak position is shifted to the right again, and the MAPbI is proved 3 The crystal generates lattice expansion under illumination, and the reversible magnetostriction effect enables the composite film to generate reversible photoresponse strain of a coercive field through stress conduction, so that the coupling effect of force, electricity and light is realized.
Example 2
A preparation method of a light-operated multifunctional P (VDF-TrFE) composite film comprises the following steps:
1) Dissolving 1.67g of P (VDF-TrFE) powder in 10ml of N, N-dimethylformamide, and magnetically stirring to obtain a uniform solution;
2) 0.578g of PbI was taken 2 And 0.2g MAI in 1ml N, N-dimethylformamide, heating in a water bath at 60 deg.C and stirring to obtain uniform MAPbI 3 Precursor solution;
3) Adding 380 mu L of the solution obtained in the step 2) into the solution obtained in the step 1), and fully stirring and mixing to obtain a uniform solution;
4) Dripping the solution obtained in the step 3) on a substrate, spin-coating at the speed of 500rpm for 3s, and then spin-coating at the speed of 1500rpm for 30s;
5) And (3) annealing the sample subjected to spin coating at 120 ℃ for 2h to obtain the 15wt% light-controlled multifunctional P (VDF-TrFE) composite film.
Example 3
A preparation method of a light-operated multifunctional P (VDF-TrFE) composite film comprises the following steps:
1) 1.67g of P (VDF-TrFE) powder was dissolved in 10ml of N, N-dimethylformamide and magnetically stirred to form a uniform solution;
2) 0.578g of PbI was taken 2 And 0.2g MAI in 1ml N, N-dimethylformamide, heating in a water bath at 60 deg.C and stirring to obtain uniform MAPbI 3 Precursor solution;
3) Adding 240 mu L of the solution obtained in the step 2) into the solution obtained in the step 1), and fully stirring and mixing to obtain a uniform solution;
4) Dripping the solution obtained in the step 3) on a substrate, spin-coating at the speed of 500rpm for 3s, and then spin-coating at the speed of 1500rpm for 30s;
5) And (3) annealing the spin-coated sample at 120 ℃ for 2 hours to obtain a 10wt% light-operated multifunctional P (VDF-TrFE) composite film.
Example 4
A preparation method of a light-operated multifunctional P (VDF-TrFE) composite film comprises the following steps:
1) 1.67g of P (VDF-TrFE) powder was dissolved in 10ml of N, N-dimethylformamide and magnetically stirred to form a uniform solution;
2) 0.578g of PbI was taken 2 And 0.2g MAI in 1ml N, N-dimethylformamide, heating in a water bath at 60 deg.C and stirring to obtain uniform MAPbI 3 Precursor solution;
3) Adding 20 mu L of the solution obtained in the step 2) into the solution obtained in the step 1), and fully stirring and mixing to obtain a uniform solution;
4) Dripping the solution obtained in the step 3) on a substrate, spin-coating at the speed of 500rpm for 3s, and then spin-coating at the speed of 1500rpm for 30s;
5) And (3) annealing the spin-coated sample at 120 ℃ for 2 hours to obtain the 1wt% optically-controlled multifunctional P (VDF-TrFE) composite film.
Example 5
A preparation method of a light-operated multifunctional P (VDF-TrFE) composite film comprises the following steps:
1) 4.74g of P (VDF-TrFE) powder was dissolved in 10ml of N, N-dimethylformamide and magnetically stirred to form a homogeneous solution;
2) 0.578g of PbI is taken 2 And 0.2g MAI in 1ml N, N-dimethylformamide, heating in a water bath at 60 deg.C and stirring to obtain uniform MAPbI 3 Precursor solution;
3) Adding 320 mu L of the solution obtained in the step 2) into the solution obtained in the step 1), and fully stirring and mixing to obtain a uniform solution;
4) Dripping the solution obtained in the step 3) on a substrate, spin-coating at the speed of 1000rpm for 3s, and then spin-coating at the speed of 3000rpm for 30s;
5) And (3) annealing the sample subjected to spin coating at 120 ℃ for 2h to obtain the 5wt% light-controlled multifunctional P (VDF-TrFE) composite film.
Example 6
A preparation method of a light-operated multifunctional P (VDF-TrFE) composite film comprises the following steps:
1) Dissolving 1.05g of P (VDF-TrFE) powder in 20ml of N, N-dimethylformamide, and magnetically stirring to form a uniform solution;
2) 0.578g of PbI was taken 2 And 0.2g MAI in 1ml N, N-dimethylformamide, heating in a water bath at 60 deg.C and stirring to obtain uniform MAPbI 3 Precursor solution;
3) Adding 70 mu L of the solution obtained in the step 2) into the solution obtained in the step 1), and fully stirring and mixing to obtain a uniform solution;
4) Dripping the solution obtained in the step 3) on a substrate, spin-coating at the speed of 1000rpm for 3s, and then spin-coating at the speed of 3000rpm for 30s;
5) And (3) annealing the spin-coated sample at 120 ℃ for 2 hours to obtain the 5wt% light-operated multifunctional P (VDF-TrFE) composite film.
Example 7
A preparation method of a light-operated multifunctional P (VDF-TrFE) composite film comprises the following steps:
1) Dissolving 1.67g of P (VDF-TrFE) powder in 10ml of N, N-dimethylformamide, and magnetically stirring to obtain a uniform solution;
2) 0.578g of PbI was taken 2 And 0.2g MAI in 1ml N, N-dimethylformamide, heating in a water bath at 60 deg.C and stirring to obtain uniform MAPbI 3 Precursor solution;
3) Adding 110 mu L of the solution obtained in the step 2) into the solution obtained in the step 1), and fully stirring and mixing to obtain a uniform solution;
4) Dripping the solution obtained in the step 3) on a substrate, spin-coating at the speed of 1000rpm for 3s, and then spin-coating at the speed of 3000rpm for 30s;
5) And (3) annealing the sample subjected to spin coating at 100 ℃ for 1h to obtain the 5wt% light-controlled multifunctional P (VDF-TrFE) composite film.
Examples 2 to 7 all prepared light-operated multifunctional P (VDF-TrFE) composite films.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
The above embodiments are only used for illustrating the design idea and features of the present invention, and the purpose of the present invention is to enable those skilled in the art to understand the content of the present invention and implement the present invention accordingly, and the protection scope of the present invention is not limited to the above embodiments. Therefore, all equivalent changes or modifications based on the principles and design concepts disclosed herein are intended to be included within the scope of the present invention.
Claims (5)
1. A preparation method of a light-operated multifunctional P (VDF-TrFE) composite film is characterized by comprising the following steps:
(1) Dissolving 1.05-4.74g of P (VDF-TrFE) powder in 10-20ml of N, N-dimethylformamide, and stirring to obtain a uniform solution;
(2) Taking PbI with a molar ratio of 1 2 Dissolving MAI in N, N-dimethylformamide, heating in 55-65 deg.C water bath, and stirring to obtain uniform MAPbI 3 Precursor solution;
(3) Taking a proper amount of MAPbI obtained in the step (2) 3 Adding the precursor solution into the uniform solution obtained in the step (1), and fully stirring and mixing to obtain MAPBI 3 a/P (VDF-TrFE) precursor solution; the MAPbi 3 The mass ratio of the precursor solute to the P (VDF-TrFE) powder is 1-20;
(4) Taking the MAPBI obtained in the step (3) 3 Dripping a VDF-TrFE precursor solution on a substrate, spin-coating on a spin coater at the speed of 500-1000rpm for 3-10s, and spin-coating at the speed of 1500-3000rpm for 30-60s to obtain a spin-coated sample;
(5) And annealing the spin-coated sample to obtain the light-operated multifunctional P (VDF-TrFE) composite film.
2. The method for preparing a light-operated multifunctional P (VDF-TrFE) composite film according to claim 1, wherein the optimal temperature for heating the water bath in the step (2) is 60 ℃.
3. The method for preparing a light-operated multifunctional P (VDF-TrFE) composite film according to claim 1, wherein the substrate used in the step (4) is a transparent glass substrate.
4. The method for preparing a light-operated multifunctional P (VDF-TrFE) composite film according to claim 1, wherein the annealing temperature in the step (5) is controlled to be 100 to 120 ℃ and the annealing time is 1 to 2 hours.
5. A light-operated multifunctional P (VDF-TrFE) composite film, wherein the light-operated multifunctional P (VDF-TrFE) composite film is prepared by the method of any one of claims 1 to 5.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103848644A (en) * | 2014-01-17 | 2014-06-11 | 中国科学院上海技术物理研究所 | Preparation method for silver nanoparticle-doped P(VDF-TrFE) (polyvinylidene fluoride-trifluoroethylene) composite thin film |
| CN109560197A (en) * | 2018-11-21 | 2019-04-02 | 苏州大学 | Ferroelectric perovskite solar cell based on polarization and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103848644A (en) * | 2014-01-17 | 2014-06-11 | 中国科学院上海技术物理研究所 | Preparation method for silver nanoparticle-doped P(VDF-TrFE) (polyvinylidene fluoride-trifluoroethylene) composite thin film |
| CN109560197A (en) * | 2018-11-21 | 2019-04-02 | 苏州大学 | Ferroelectric perovskite solar cell based on polarization and preparation method thereof |
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