CN108767109B - Method for preparing inorganic-organic flexible composite material with magnetoelectric coupling performance - Google Patents

Method for preparing inorganic-organic flexible composite material with magnetoelectric coupling performance Download PDF

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CN108767109B
CN108767109B CN201810565512.0A CN201810565512A CN108767109B CN 108767109 B CN108767109 B CN 108767109B CN 201810565512 A CN201810565512 A CN 201810565512A CN 108767109 B CN108767109 B CN 108767109B
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CN108767109A (en
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张易军
唐卓华
张洁
刘明
任巍
叶作光
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Xian Jiaotong University
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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    • C23C14/205—Metallic material, boron or silicon on organic substrates by cathodic sputtering
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    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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Abstract

The invention provides a method for preparing an inorganic-organic flexible composite material with magnetoelectric coupling performance, which comprises the following steps: step one, dispersing PVDF-TrFE powder in dimethylformamide according to the mass ratio of 1:10 to obtain a PVDF solution; step two, filtering the PVDF solution prepared in the step one to obtain a filtered PVDF solution, and adding Fe3O4Dispersing the nano particles in the filtered PVDF solution to obtain a mixed solution; step three, uniformly dripping the mixed solution obtained in the step two on a glass slide, drying for 1.5 hours at 135 ℃, then heating to 142-145 ℃, taking out and cooling to 0 ℃ to obtain a flexible multiferroic material film; and step four, regulating the magnetism of the flexible multiferroic material film obtained in the step three through an external voltage to obtain the flexible multiferroic composite material. The method is simple to operate and easy to realize, and the prepared material has better pressure resistance than an inorganic multiferroic material and flexibility which is not possessed by the inorganic material.

Description

Method for preparing inorganic-organic flexible composite material with magnetoelectric coupling performance
Technical Field
The invention belongs to the technical field of semiconductors, and particularly relates to a method for preparing an inorganic-organic flexible composite material with magnetoelectric coupling performance.
Background
With the rapid development of microelectronics and semiconductor technologies, three-dimensionality, miniaturization, adjustability and multi-functionalization have become new trends in the design and development of current electronic components. The exploration and development of novel intelligent multi-scale materials related to the material, in particular to a multiferroic material integrating ferroelectricity and ferromagnetism and permeating into various fields of modern technology, has become a research hotspot in the last decade. The multiferroic material not only has two or three single ferrosexes (such as ferroelectricity, ferromagnetism and ferroelasticity) at the same time, but also can generate some new functions through the coupling synergistic action between the ferrosexes, for example, the magnetoelectric coupling effect exists between the ferroelectricity and the ferromagnetism, so that the electric control of magnetism or magnetic control electricity becomes possible. In addition, the multiferroic material can also realize the regulation and control effect of a magnetic field on dielectric constant or capacitance. Although many single-phase multiferroic materials have been discovered by researchers so far, compared with the weak magnetoelectric coupling effect of the single-phase multiferroic material at room temperature, the artificially constructed composite multiferroic material not only has better selectivity and flexibility in material combination and structural design, but also can realize stronger magnetoelectric coupling effect and generate novel physical phenomena and regulation mechanisms, particularly complex interaction exists among electron spin, charge, orbit and crystal lattice at an interface, so that a plurality of new magnetoelectric physical phenomena can be caused, and a new-generation multifunctional device integrating magnetoelectric in one body is expected to be realized, so that the composite multiferroic material has important application prospects in the fields of a new-generation memory, a sensor, a microwave device and the like. Meanwhile, by utilizing competition and coexistence of multiple quantum sequence parameters in the multiferroic material, the multi-physical-field behavior of the quantum regulating material can be realized, which is a brand new method different from the traditional semiconductor microelectronics and is one of the main directions of the development of the electronic technology in the post-Mole times.
At present, the most studied in the field of multiferroics is inorganic multiferroic materials, but the work for studying inorganic-organic composite flexible multiferroic materials is very little, which is not favorable for the application of multiferroic materials in the field of flexible devices. Therefore, we designed a process for making a flexible multiferroic thin film material and confirmed its magnetoelectric coupling properties.
Disclosure of Invention
The invention aims to provide a method for preparing an inorganic-organic flexible composite material with magnetoelectric coupling performance, which solves the problems of the prior art
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a method for preparing an inorganic-organic flexible composite material with magnetoelectric coupling performance, which comprises the following steps:
step one, dispersing PVDF-TrFE powder into dimethylformamide according to the mass ratio of 1:10, and stirring until the PVDF-TrFE powder is completely dissolved in the dimethylformamide to obtain a PVDF solution;
step two, filtering the PVDF solution prepared in the step one to obtain a filtered PVDF solution, and adding Fe3O4Dispersing the nano particles in the filtered PVDF solution to obtain a mixed solution, and then carrying out ultrasonic oscillation on the mixed solution until Fe3O4The nanoparticles are uniformly dispersed in the filtered PVDF solution, wherein Fe3O4The mass ratio of the nano particles to the PVDF-TrFE powder added in the step one is (1-10): 100;
step three, uniformly dripping the mixed solution obtained in the step two on a glass slide, and drying to obtain a flexible multiferroic material film;
and step four, adding an external voltage to the flexible multiferroic material film obtained in the step three to obtain the inorganic-organic flexible composite material.
Preferably, the PVDF-TrFE powder used in the first step is a polycrystalline beta-phase PVDF-TrFE powder.
Preferably, in the second step, after the mixed solution is subjected to ultrasonic oscillation, the mixed solution is placed in a vacuum pump to be vacuumized until air in the solution is removed.
Preferably, in the third step, the glass slide is obtained by ultrasonic cleaning sequentially through acetone, absolute ethyl alcohol and deionized water; the drying process parameters are as follows: drying at 135 deg.C for 1.5h, heating to 142-145 deg.C, taking out, and rapidly cooling to 0 deg.C with water.
Preferably, in the third step, the glass slide on which the mixed solution is dripped is cooled and then placed in a magnetron sputtering apparatus, the magnetron sputtering apparatus is vacuumized to 1Pa, and then gold is sprayed on both sides of the flexible multiferroic material film until both sides of the flexible multiferroic material film are plated with gold electrodes.
Preferably, the inorganic-organic flexible composite material is prepared by the preparation method according to any one of claims 1 to 5.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a method for preparing an inorganic-organic flexible composite material with magnetoelectric coupling performance, which takes PVDF-TrFE powder as a substrate and thenAddition of Fe to PVDF-TrFE powder3O4The nano particles further realize the magnetoelectric coupling performance of the flexible multiferroic material film, and simultaneously, the PVDF matrix is deformed by external voltage, so that stress is transferred to Fe dispersed in the PVDF matrix3O4Nano particles, and then electric control magnetism is realized. Meanwhile, the method is simple to operate and easy to realize, and the prepared material has better pressure resistance than an inorganic multiferroic material and flexibility which is not possessed by the inorganic material.
Drawings
FIG. 1 shows 1% Fe prepared in example 1 of the present invention3O4Magnetoelectric regulation and control results of the flexible multiferroic composite material with the content;
FIG. 2 shows 10% Fe prepared in example 2 of the present invention3O4And (3) a magnetoelectric regulation result of the flexible multiferroic composite material.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
The invention provides a method for preparing an inorganic-organic flexible composite material with magnetoelectric coupling performance, which comprises the following steps:
1) cleaning the glass slide and drying the glass slide by using nitrogen for later use;
2) and dispersing PVDF-TrFE powder into dimethylformamide according to the mass ratio of 1:10, and after magnetically stirring for 8 hours, completely dissolving the PVDF-TrFE powder into the dimethylformamide to obtain a PVDF solution, wherein the used PVDF-TrFE powder is polycrystalline beta-phase PVDF-TrFE powder.
3) Filtering the PVDF solution obtained in the step 2) to obtain a filtered PVDF solution;
4) mixing Fe3O4Dispersing the nano particles in the filtered PVDF solution to obtain a mixed solution, and then ultrasonically oscillating the mixed solution for 4 hours to enable Fe3O4Uniformly dispersing the nano particles in the filtered PVDF solution, and then placing the mixed solution in a vacuum pump for vacuumizing for 5 minutes, wherein the vacuumizing is used for removing air in the solution; wherein, Fe3O4The mass ratio of the nano particles to the PVDF-TrFE powder is (1-10): 100;
5) uniformly dripping the mixed solution obtained in the step 4) on a glass slide, drying the glass slide for 1.5 hours at 135 ℃, then heating the glass slide to 142-145 ℃, taking out the glass slide, putting the glass slide in an ice-water mixture, and rapidly cooling the glass slide to 0 ℃ to obtain a flexible multiferroic material film;
6) and (3) peeling off the flexible multiferroic coating film from the glass slide to obtain the self-supporting flexible multiferroic composite material, wherein the flexible multiferroic composite material is of a sheet-like structure with the thickness of 20-200 microns.
7) The magnetism of the obtained flaky flexible multiferroic material can be regulated and controlled by external voltage, so that the inorganic-organic flexible composite material is obtained.
Specifically, in the step 1), the clean glass slide is obtained by sequentially carrying out ultrasonic cleaning on the glass slide by using acetone, absolute ethyl alcohol and deionized water.
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
Example 1
A method for preparing an inorganic-organic composite flexible multiferroic material comprises the following steps:
a. slide preparation:
the slides required for the experiment were washed as follows: ultrasonic cleaning with acetone for 10 min, pouring off acetone, cleaning with anhydrous ethanol for 10 min, pouring off anhydrous ethanol, and repeatedly ultrasonic cleaning with deionized water for 3 times, each for 5 min. And finally, blowing the mixture by using nitrogen for standby.
b. PVDF-TrFE powder is dispersed in dimethylformamide according to the mass ratio of 1:10, and the PVDF solution is filtered after being magnetically stirred for 8 hours. Fe with the mass of 1 percent of that of PVDF-TrFE powder3O4After the nanoparticles are dispersed in the PVDF solution, ultrasonic oscillation is continued for 4 hours, and the solution is placed in a vacuum pump to be vacuumized for 5 minutes.
c. Uniformly dripping the solution uniformly dispersed by ultrasonic oscillation on a glass slide, taking down the glass slide, drying the glass slide in a dryer at 135 ℃ for 1.5 hours, heating to 145 ℃, taking out the glass slide, putting the glass slide in an ice-water mixture, and rapidly cooling to 0 ℃.
d. The glass slide is placed in a small magnetron sputtering instrument, the glass slide is firstly vacuumized to reach about 1Pa, and then gold is sprayed for 25 minutes. And (3) removing the film with one surface plated with gold from the glass slide, and repeating the vacuumizing gold plating process on the reverse surface to plate gold electrodes on the two surfaces. The thickness of the prepared film measured by using a step profiler is 25-40 microns, the corners of the film are cut off to prevent the two sides of the film from being conducted due to the fact that gold is also sputtered on the side surfaces in the sputtering and gold plating process, and an electric field cannot be loaded to carry out magnetoelectric coupling performance test.
e. And the film is placed in an electron paramagnetic resonance spectrometer (ESR), and an electrometer with the maximum output voltage of 1000V is used for testing the in-situ electromagnetic regulation and control performance.
As can be seen from FIG. 1, when the applied electric field reaches 320kV/cm, the maximum control amount can reach 176 Oe.
Example 2
A method for preparing an inorganic-organic composite flexible multiferroic material comprises the following steps:
a. slide preparation:
the slides required for the experiment were washed as follows: ultrasonic cleaning with acetone for 10 min, pouring off acetone, cleaning with anhydrous ethanol for 10 min, pouring off anhydrous ethanol, and repeatedly ultrasonic cleaning with deionized water for 3 times, each for 5 min. And finally, blowing the mixture by using nitrogen for standby.
b. PVDF-TrFE powder is dispersed in dimethylformamide according to the mass ratio of 1:10, and the PVDF solution is filtered after being magnetically stirred for 8 hours. Fe with the mass of 10 percent of PVDF3O4After the nanoparticles are dispersed in the PVDF solution, ultrasonic oscillation is continued for 4 hours, and the solution is placed in a vacuum pump to be vacuumized for 5 minutes.
c. Uniformly dripping the solution uniformly dispersed by ultrasonic oscillation on a glass slide, taking down the glass slide, drying the glass slide in a dryer at 135 ℃ for 1.5 hours, heating to 145 ℃, taking out the glass slide, putting the glass slide in an ice-water mixture, and rapidly cooling to 0 ℃.
d. The glass slide is placed in a small magnetron sputtering instrument, the glass slide is firstly vacuumized to reach about 1Pa, and then gold is sprayed for 25 minutes. And (3) removing the film with one surface plated with gold from the glass slide, and repeating the vacuumizing gold plating process on the reverse surface to plate gold electrodes on the two surfaces. The thickness of the prepared film measured by using a step profiler is 25-40 microns, the corners of the film are cut off to prevent the two sides of the film from being conducted due to the fact that gold is also sputtered on the side surfaces in the sputtering and gold plating process, and an electric field cannot be loaded to carry out magnetoelectric coupling performance test. e. And the film is placed in an electron paramagnetic resonance spectrometer (ESR), and an electrometer with the maximum output voltage of 1000V is used for testing the in-situ electromagnetic regulation and control performance.
As can be seen from FIG. 2, when the applied electric field reaches 320kV/cm, the maximum control amount can reach 150Oe, which is accompanied by Fe3O4The content is increased, and the magnetic control quantity is reduced.

Claims (5)

1. A method for preparing an inorganic-organic flexible composite material with magnetoelectric coupling performance is characterized by comprising the following steps:
step one, dispersing PVDF-TrFE powder into dimethylformamide according to the mass ratio of 1:10, and stirring until the PVDF-TrFE powder is completely dissolved in the dimethylformamide to obtain a PVDF solution;
step two, filtering the PVDF solution prepared in the step one to obtain a filtered PVDF solution, and adding Fe3O4Dispersing the nano particles in the filtered PVDF solution to obtain a mixed solution, and then carrying out ultrasonic oscillation on the mixed solution until Fe3O4The nanoparticles are uniformly dispersed in the filtered PVDF solution, wherein Fe3O4The mass ratio of the nanoparticles to the PVDF-TrFE powder added in the step one is 10: 100;
step three, uniformly dripping the mixed solution obtained in the step two on a glass slide, and drying to obtain a flexible multiferroic material film;
step four, adding an external voltage to the flexible multiferroic material film obtained in the step three to obtain an inorganic-organic flexible composite material;
in the third step, the drying process parameters are as follows: drying at 135 deg.C for 1.5h, heating to 142-145 deg.C, taking out, and rapidly cooling to 0 deg.C with water;
and in the second step, after the mixed solution is subjected to ultrasonic oscillation, putting the mixed solution into a vacuum pump for vacuumizing until air in the solution is removed.
2. The method for preparing the inorganic-organic flexible composite material with magnetoelectric coupling performance according to claim 1, characterized in that the PVDF-TrFE powder used in the first step is a polycrystalline beta-phase PVDF-TrFE powder.
3. The method for preparing the inorganic-organic flexible composite material with magnetoelectric coupling performance according to claim 1, characterized in that in step three, the glass slide is obtained by sequentially carrying out ultrasonic cleaning on acetone, absolute ethyl alcohol and deionized water.
4. The method for preparing the inorganic-organic flexible composite material with magnetoelectric coupling performance according to claim 1, characterized in that in the third step, the glass slide on which the mixed solution is dripped is cooled and placed in a magnetron sputtering apparatus, the magnetron sputtering apparatus is vacuumized to 1Pa, and then gold is sprayed on both sides of the flexible multiferroic material film until both sides of the flexible multiferroic material film are plated with gold electrodes.
5. An inorganic-organic flexible composite material with magnetoelectric coupling performance, characterized in that the inorganic-organic flexible composite material is prepared according to the preparation method of any one of claims 1 to 4.
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