CN108102121B - Anisotropic magnetic polymer composite film material and preparation method thereof - Google Patents
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- 229910002546 FeCo Inorganic materials 0.000 claims abstract description 33
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Abstract
The invention discloses an anisotropic magnetic polymer composite film material and a preparation method thereof, belonging to the technical field of magnetic polymer composite materials. The composite thin film material comprises FeCo magnetic nanoparticles and a polymer matrix. The preparation method comprises the following steps of 1) adding nano FeCo cubic magnetic nanoparticles into a high molecular polymer, and uniformly stirring to obtain a mixture; 2) spin-coating the obtained mixture on a glass sheet or a silicon sheet to form a film, placing the prepared film in a magnetic field to perform self-assembly of magnetic particles, and then curing at a certain temperature to prepare the anisotropic magnetic polymer composite film. The invention has simple process, easy control of film thickness, good directionality of the contained anisotropic self-assembled nano rope, high production efficiency and good mechanical property, and has potential application in high and new technical fields of flexible magnetic devices and the like.
Description
Technical Field
The invention relates to the technical field of preparation of a nano material composite film, in particular to an anisotropic magnetic polymer composite film material and a preparation method thereof.
Background
Conventional magnetic nanomaterials include pure metal nanomaterials, metal alloy nanomaterials, and metal oxide nanomaterials, all of which are "hard materials" that are not suitable for use in the field of flexible electronics. Polymeric materials have several unique properties compared to inorganic materials, including flexibility, processability, transparency, and the like. Therefore, the polymer and the magnetic nanometer material are mixed together to obtain a mixture which has the advantages of the polymer material and the properties of the nanometer material, thereby expanding the application range of the material. Magnetic polymer composites have become one of the research hotspots in the emerging field, attracting the interest of many researchers. Magnetic nanoparticle composite films also find many novel applications in the fields of magnetic storage, sensors and electromagnetic shielding.
The nano particles can be directionally arranged in the magnetic field by using an external magnetic field, and the anisotropic magnetic polymer film can be obtained, so that the composite film has different responses to the magnetic field in different directions. At present, for the reported nanowire structure self-assembled under a magnetic field, the defect of poor orientation exists, which seriously influences the magnetic anisotropy performance of the film and limits the application range of the film.
Disclosure of Invention
The invention aims to provide an anisotropic magnetic polymer composite film material and a preparation method thereof, and the prepared composite film material has the advantages of good flexibility, strong magnetic anisotropy, easy film thickness control, good directionality and the like, and can be widely applied to the field of flexible electronics. The preparation method is simple and easy to implement, and the result repeatability is good and easy to control.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for preparing an anisotropic magnetic polymer composite film material comprises the following steps:
(1) adding the ground FeCo magnetic nanoparticles into a high polymer material, and uniformly mixing under an ultrasonic condition to obtain a mixed material; the content of FeCo magnetic nanoparticles in the mixed material is 0.05-10 wt%;
(2) placing the mixed material obtained in the step (1) in a drying box, and placing the mixed material under the conditions of vacuum and room temperature to exhaust bubbles in the mixed material;
(3) pre-coating the mixture material with bubbles removed on a clean glass sheet or a silicon sheet, then spin-coating the mixture material by using spin-coating equipment to form a film, and placing the prepared film in a magnetic field to enable FeCo magnetic nano particles in the film to be self-assembled;
(4) and (4) placing the film treated in the step (3) in a constant-temperature oven for curing to obtain the anisotropic magnetic polymer composite film material.
In the step (1), the polymer material is Polydimethylsiloxane (PDMS), polymethyl methacrylate (PMMA) or epoxy resin, and is preferably Polydimethylsiloxane (PDMS).
In the step (2), the vacuum condition means that the vacuum degree is 40-200Pa, and the time for placing the obtained mixed material in the drying oven is more than 20 minutes.
In the step (3), the rotation speed adopted by the spin coating equipment is 500rpm-8000 rpm; the applied external magnetic field intensity is 30mT-200mT, and the external magnetic field time is 10min-2 h.
In the step (3), the cleaning method of the glass sheet or the silicon wafer comprises the following steps: and sequentially ultrasonically cleaning the substrate with acetone, alcohol and deionized water for 3 times, wherein the ultrasonic time is 10min each time.
In the step (4), in the curing process, the curing temperature is 80-120 ℃, and the heat preservation time is 30min-2 h.
The anisotropic magnetic polymer composite film material prepared by the method is formed by distributing FeCo magnetic nano particles in a polymer matrix, wherein: the FeCo magnetic nanoparticles are arranged in a chain shape along the direction of a magnetic field to form a structure similar to a nano rope, the length of the chain structure can reach 500 mu m, and the width of the chain structure can reach 1 mu m.
In the composite film material, the mass fraction of the FeCo magnetic nanoparticles is 0.05-10%, and the particle size of the FeCo magnetic nanoparticles is 20nm-1 μm (preferably 170 nm); the thickness of the film is in the range of 2 μm to 1 mm.
In the composite film material, the FeCo magnetic nano particles are in a cubic structure, the exposed surface of the cube is {100}, and the easy magnetization direction is <100 >.
The invention has the advantages and beneficial effects that:
1. the invention can obtain films with a series of thicknesses by spin-coating the uniformly mixed FeCo nano-particles and the polymer mixture by a spin coater, and then can ensure that the nano-particles are directionally arranged along the direction of the magnetic induction line by an external magnetic field to form an anisotropic magnetic polymer composite film.
2. Under the condition of an external magnetic field, the magnetic polymer composite film prepared by the invention enables the nano particles to be self-assembled into a 'nano rope' structure, so that the magnetic polymer composite film generates magnetic anisotropy in different directions, the method is simple and easy to implement, the production efficiency is high, the magnetic anisotropy is strong, and the industrial scale production is favorably realized.
3. The invention can obtain magnetic nano-particle polymer composite films with different thicknesses by utilizing different spin coating parameters, and is easy to control.
4. The 'nano rope' structure assembled in the magnetic field has obvious enhancement effect on the mechanical property of the macromolecule, and the application range of the material is expanded.
5. The preparation method is simple and easy to implement, and the result repeatability is good and easy to control. Moreover, for such flexible composite films, the structure of the oriented nanowires also has varying degrees of influence on their mechanical properties. Therefore, the composite film with good nanowire structure orientation, strong magnetic anisotropy and excellent mechanical property is developed on the basis of the existing method, and has obvious application value. These anisotropic magnetic polymer composite films have wide application prospects in the field of flexible electromagnetism in the future.
Drawings
FIG. 1 is a flow chart of the preparation of an anisotropic magnetic polymer composite film;
FIG. 2 is a graph showing the effect of spin-coating speed on film thickness;
FIG. 3 shows the appearance of self-assembled "ropes" under scanning electron microscope with a low power and a high power, and a transmission electron microscope bright field image, when the applied magnetic field is 140mT and the mass fraction of FeCo nanoparticles is 1%; wherein: (a) and (b) low high power morphology, (c) transmission electron microscopy bright field image;
FIG. 4 is a room temperature hysteresis loop of FeCo-PDMS composite film in different directions (parallel to the assembled nanowire (/ /), perpendicular to the assembled nanowire (#)) when the applied magnetic field is 140mT and the mass fraction of FeCo nanoparticles is 1%;
FIG. 5 shows the tensile strength of pure PDMS and FeCo (1.0 wt%) -PDMS composite films.
The specific implementation mode is as follows:
the invention is described in detail below with reference to the figures and examples.
The invention relates to an anisotropic magnetic polymer composite film material and a preparation method thereof, wherein the preparation process is shown in figure 1, and the preparation method specifically comprises the following steps:
1. mixing Part A and Part B of commercial polymer Polydimethylsiloxane (PDMS) Hasuncast RTVS603 according to the mass ratio of 1:1, and uniformly stirring to obtain a mixture;
2. manually grinding the synthesized FeCo cubic magnetic nanoparticles after vacuum drying for 20-40min by using a grinding body, adding the FeCo cubic magnetic nanoparticles into the mixture according to the mass fraction of 0.05-10%, and carrying out ultrasonic treatment for 2-3h after stirring to fully mix the nanoparticles with the high polymer to form a uniform FeCo-PDMS mixture;
3. placing the fully mixed FeCo-PDMS mixture in a vacuum environment for standing for 30min, and exhausting air bubbles in the mixture; taking a cleaned glass sheet or a cleaned silicon wafer as a substrate, and spin-coating the mixture of FeCo-PDMS with bubbles being exhausted into a film with a certain thickness by using spin-coating equipment;
4. placing the prepared film in a magnetic field (30mT-200mT) with certain strength for self-assembly, wherein the time of the external magnetic field is 10min-2 h;
5. and then placing the film after magnetic orientation in a vacuum oven to be cured for 1h at 100 ℃ or cured for 3h at 80 ℃, and peeling the film from the substrate after curing.
The thickness of the prepared anisotropic magnetic polymer film is 2 mu m-1mm, and the filling mass fraction of FeCo magnetic nanoparticles is 0.05% -10%.
The magnetic nano-particles FeCo in the anisotropic magnetic polymer film are arranged along the direction of the magnetic induction line to form a structure similar to a nano-rope, the length of the nano-rope can reach 500 mu m, and the width of the nano-rope can reach 1 mu m.
The strength range of the external magnetic field of the anisotropic magnetic polymer film is 30-200mT, the length and the width of the nano rope assembled in the magnetic field are increased along with the increase of the strength of the external magnetic field, and then the nano rope tends to be stable: in a low magnetic field region (10-40mT), the growth and the growth are basically synchronous, and the external magnetic field is too low to enable one direction to grow rapidly; in the middle magnetic field area (50-150mT), the growth speed of the nano rope is faster than the coarsening speed; in the high magnetic field region (150-. The magnetic polymer composite film has strong anisotropy in the directions parallel and vertical to the assembled nano rope.
Example 1:
in this example, an anisotropic magnetic polymer composite thin film material was prepared, in which the external magnetic field strength was 140mT and the mass fraction of FeCo cubic nanoparticles (170nm) was 1%. The preparation process comprises the following steps:
1. weighing Part A and Part B of commercial high-molecular Polydimethylsiloxane (PDMS) Hasuncast RTVS603, mixing according to the mass ratio of 1:1, and uniformly stirring to obtain a high-molecular polymer;
2. manually grinding the synthesized FeCo magnetic nanoparticles after vacuum drying for 30min by using a grinding body, uniformly adding the FeCo magnetic nanoparticles into a polymer according to the mass fraction of 1%, uniformly stirring, and performing ultrasonic treatment for 3h to fully mix the nanoparticles with a high polymer to form a uniform FeCo-PDMS mixture;
3. placing the fully mixed FeCo-PDMS mixture in a vacuum box for standing for 30min, and exhausting bubbles in the mixture; taking a cleaned glass sheet or a cleaned silicon wafer as a substrate, and spin-coating the mixture of FeCo-PDMS with bubbles being exhausted into a film with a certain thickness by using spin-coating equipment; wherein the spin-coating speed affects the thickness of the formed thin film, as shown in fig. 2.
4. Placing the film prepared in the last step in a magnetic field (140mT) with certain strength for magnetic orientation, wherein the time of the external magnetic field is 1 h;
5. placing the film assembled under the magnetic field in a vacuum oven, curing for 1h at 100 ℃, and stripping the film from the substrate after the curing is finished;
the magnetic nano particles FeCo in the prepared anisotropic magnetic polymer film are arranged along the direction of the magnetic induction line to form a structure similar to a 'nano rope', the appearance of the self-assembled nanowire is shown in figure 3, when the mass fraction of the FeCo nano particles is 1% and the external magnetic field intensity is 140mT, the average length of the self-assembled nano rope is 160 micrometers, the longest length can reach 500 micrometers, and the average width is 1 micrometer;
fig. 4 is a room temperature hysteresis loop of the FeCo-PDMS composite film in different directions (//and ×) respectively indicating the assembled nanowire direction parallel or perpendicular to the stretching direction when the applied magnetic field is 140mT and the mass fraction of the FeCo nanoparticles is 1%. As can be seen from the figure, the composite film containing the assembled "nano-rope" structure has strong magnetic anisotropy;
FIG. 5 shows the tensile strength of pure PDMS and FeCo (1 wt%) -PDMS films. As can be seen from the graph, the tensile strength in the direction of the assembled nanowires (2.20MPa) was increased by 26.2% compared to pure PDMS (1.73MPa), and the tensile strength perpendicular to the direction of the assembled nanowires (3.20MPa) was increased by 85.2% compared to pure PDMS. The improvement of the mechanical property expands the application range of the composite film, and is beneficial to the application of the self-assembled anisotropic nanoparticle film on a flexible device.
Claims (6)
1. A preparation method of an anisotropic magnetic polymer composite film material is characterized by comprising the following steps: the method comprises the following steps:
(1) adding the ground FeCo magnetic nanoparticles into a high polymer material, and uniformly mixing under an ultrasonic condition to obtain a mixed material; the content of FeCo magnetic nanoparticles in the mixed material is 0.05-10 wt%; the FeCo magnetic nanoparticles are of a cubic structure, the exposed surface of the cube is {100}, the easy magnetization direction is <100>, and the particle size of the FeCo magnetic nanoparticles is 20nm-1 mu m;
(2) placing the mixed material obtained in the step (1) in a drying box, and placing the mixed material under the conditions of vacuum and room temperature to exhaust bubbles in the mixed material;
(3) pre-coating the mixture material with bubbles removed on a clean glass sheet or a silicon sheet, then spin-coating the mixture material by using spin-coating equipment to form a film, and placing the prepared film in a magnetic field to enable FeCo magnetic nano particles in the film to be self-assembled; the rotating speed adopted by the spin coating equipment is 500-8000 rpm; the applied external magnetic field intensity is 30mT-200mT, and the external magnetic field time is 10min-2 h;
(4) curing the film treated in the step (3) in a constant-temperature oven at the curing temperature of 80-120 ℃ for 30min-3 h; and curing to obtain the anisotropic magnetic polymer composite film material.
2. The method for preparing the anisotropic magnetic polymer composite thin film material according to claim 1, wherein: in the step (1), the polymer material is Polydimethylsiloxane (PDMS), polymethyl methacrylate (PMMA) or epoxy resin.
3. The method for preparing the anisotropic magnetic polymer composite thin film material according to claim 1, wherein: in the step (2), the vacuum condition refers to that the vacuum degree is 40-200Pa, and the time for placing the obtained mixed material in a drying box is more than 20 minutes.
4. The method for preparing the anisotropic magnetic polymer composite thin film material according to claim 1, wherein: in the step (3), the cleaning method of the glass sheet or the silicon wafer comprises the following steps: and sequentially ultrasonically cleaning the substrate with acetone, alcohol and deionized water for 3 times, wherein the ultrasonic time is 10min each time.
5. An anisotropic magnetic polymer composite film material prepared by the method of any one of claims 1 to 4, characterized in that: the composite film material is formed by distributing FeCo magnetic nano particles in a polymer matrix, wherein: the FeCo magnetic nanoparticles are arranged along the direction of a magnetic field to form a chain structure, the length of the chain structure can reach 500 mu m, and the width of the chain structure can reach 1 mu m.
6. The anisotropic magnetic polymer composite thin film material of claim 5, wherein: in the composite film material, the mass fraction of the FeCo magnetic nano particles is 0.05-10%, and the thickness range of the film is 2 mu m-1 mm.
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| CN110498943B (en) * | 2019-08-26 | 2021-10-19 | 哈尔滨工程大学 | Preparation method of anisotropic surface with controllable laminated structure |
| CN110862689B (en) * | 2019-11-29 | 2022-04-26 | 中国科学院合肥物质科学研究院 | Preparation method of magnetic control flexible surface material with orthotropic wettability |
| CN111234277A (en) * | 2020-03-04 | 2020-06-05 | 北京大学 | Preparation method and application of magnetic multi-size stripe film structure |
| CN112876598B (en) * | 2021-03-04 | 2022-09-27 | 中国科学院合肥物质科学研究院 | Preparation method of multi-response and anisotropic magnetic hydrogel |
| CN113184803B (en) * | 2021-04-22 | 2022-07-12 | 西安交通大学 | Magnetic nanoparticle self-assembly system based on magnetic field driving and processing method |
| CN113583448B (en) * | 2021-08-25 | 2023-03-14 | 中国科学院宁波材料技术与工程研究所 | Deformable-variable-rigidity dual-function magnetic intelligent material and preparation method and application thereof |
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| CN104530455A (en) * | 2014-12-28 | 2015-04-22 | 电子科技大学 | Preparation method and application of PDMS (polydimethylsiloxane)-magnetic nano-particle composite optical film |
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