CN111763276B - Liquid metal/high polymer composite dielectric material and preparation method thereof - Google Patents
Liquid metal/high polymer composite dielectric material and preparation method thereof Download PDFInfo
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- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
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Abstract
The invention belongs to the technical field of composite materials, and particularly relates to a liquid metal/polymer composite dielectric material and a preparation method thereof. Uniformly blending the polymerization monomer solution, the liquid metal and the cross-linking agent to obtain a precursor solution; and standing the precursor solution to obtain the high-molecular dielectric material. The preparation method is simple and convenient, and the prepared composite material has excellent dielectric property and better tensile property than the traditional dielectric material, and has wide application prospect in the fields of wearable electronic equipment, soft robots and the like.
Description
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a liquid metal/polymer composite dielectric material and a preparation method thereof.
Background
Dielectric materials have an important strategic position in modern electronic and power systems. The method has wide application prospect in the aspects of future power generation, bionics, biomedicine, optics, microsystems, aerospace and the like. The traditional inorganic ceramic material has high dielectric constant and high thermoelectric stability, but the processing temperature is higher and the brittleness is large, so that the requirement of the modern electronic industry is difficult to meet.
The rapid development in the field of wearable electronic products and soft robots puts higher demands on dielectric materials, and the dielectric materials have excellent dielectric properties and good mechanical properties and processability. The introduction of inorganic micro/nano particles or other inorganic substances into polymer composite dielectric materials using polymers as matrix has become the mainstream of research. Increasing the loading of these inorganic materials can increase the dielectric properties of the materials, but at the same time results in a significant decrease in the mechanical properties of the materials. Therefore, although the electrochemical performance and mechanical properties of the polymer composite dielectric material blended with the rigid inorganic material are improved to a certain extent, the polymer composite dielectric material still cannot meet the increasingly high performance requirements of the rapidly developed electronic industry on the electronic material, and therefore, the deep research and development of the polymer composite dielectric material with better performance is still very important.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a liquid metal/polymer composite dielectric material and a preparation method thereof aiming at the defects in the prior art.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for preparing a liquid metal/polymer composite dielectric material comprises the following steps:
(1) uniformly blending the polymerization monomer solution, the liquid metal and the cross-linking agent to obtain a precursor solution;
(2) and standing the precursor solution to obtain the high-molecular dielectric material.
Further, the following steps are carried out:
(1) adding liquid metal into a polymerization monomer solution at normal temperature, and uniformly blending in a blending mode to realize micron-scale or nano-scale dispersion of the liquid metal in the polymer monomer solution to obtain a precursor dispersion liquid;
(2) and (2) oscillating and polymerizing the precursor dispersion liquid in the step (1) into glue, transferring the glue into a mould, and standing for 1-14 days to obtain the liquid metal/polymer composite dielectric material.
The blending mode in the step (1) comprises magnetic stirring or low-temperature ultrasound, the ultrasound power is 100-400W, the ultrasound time is 10-20 minutes, a cell disruption instrument is used in the ultrasound, and the ultrasound process is carried out in an ice bath to prevent implosion;
the liquid metal is dispersed into the polymer monomer solution to ensure that the particle size of the liquid metal reaches 50 nm-20 mu m to form a micron or nanometer grade.
And (2) oscillating the precursor dispersion liquid in the step (1) for 20-60 minutes to synthesize the glue.
The liquid metal accounts for 0.5-5% of the mass of the polymerization monomer solution.
The polymerization monomer solution is formed by dissolving a monomer in a solvent; wherein the monomer accounts for 10-30% of the total mass of the polymerized monomer solution.
The monomer is one or more of acrylic acid, acrylamide, acrylonitrile, methyl acrylate and methyl methacrylate; the solvent is deionized water or ethanol.
When the monomers are acrylamide, acrylonitrile, methyl acrylate and methyl methacrylate, a cross-linking agent can be added when a precursor dispersion liquid is prepared, so that cross-linking among macromolecules can be further promoted, the network structure of a system is enhanced, and the addition amount is 0-0.2 mol% of the monomers; the cross-linking agent is N, N-methylene bisacrylamide.
The liquid metal is a liquid solution of gallium and/or gallium-containing alloy with a low melting point at normal temperature.
The gallium-containing alloy is a binary alloy of gallium and/or a ternary alloy of gallium.
The liquid metal is a binary alloy of gallium; wherein, the gallium content in the gallium-indium alloy is 50-90% by mass, and the balance is indium; the liquid metal is gallium indium tin ternary alloy; wherein, the gallium content in the gallium indium tin ternary alloy is 60 to 80 mass percent, the indium content is 10 to 30 mass percent, and the balance is tin.
The liquid metal/polymer composite dielectric material with the dielectric constant of 7.5-20.0 is prepared according to the method.
Compared with the prior art, the invention has the following advantages and technical effects:
the polymerization monomers used in the preparation process do not need to be purified to remove the polymerization inhibitor, and oxygen and nitrogen discharging protection is not needed in the polymerization process, so that the traditional polymerization process is simplified, the production efficiency is improved, and the production cost is reduced;
when the acrylic acid is used as a polymerization monomer or a copolymerization unit in the polymerization monomer solution, the acrylic acid can corrode liquid metal and gradually release gallium ions capable of complexing polyacrylic acid, so that physical crosslinking of polymer chains is realized, and the crosslinking among polymers can be realized without adding other crosslinking agents. When acrylamide, acrylonitrile, methyl acrylate and methyl methacrylate are used as monomers and dispersed with liquid metal, a cross-linking agent is added to form a stable network structure through physical cross-linking and chemical cross-linking, gallium ions in the dispersion liquid in each cross-linking form are slowly released, and the system shows excellent plasticity at the initial stage of reaction, can be shaped at will and is convenient to process and form; and the preparation process is carried out at normal temperature and normal pressure, so that the requirement on equipment is low.
The material prepared by the invention improves the mechanical property of the traditional dielectric material, and due to the addition of the liquid metal which is a flexible material, the material has more excellent flexibility and elasticity, the elongation at break can reach 1600 percent to the maximum extent, and the material can better meet the development requirements of wearable equipment and electronic industry.
Drawings
FIG. 1 is an optical micrograph of a composite material provided in example 1 of the present invention;
FIG. 2 is a photograph showing plasticity of the composite material provided in example 1 of the present invention;
fig. 3 is a stress-strain curve of the composite material provided in example 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to test examples and specific embodiments. It should be understood that the scope of the above-described subject matter is not limited to the following examples, and any techniques implemented based on the disclosure of the present invention are within the scope of the present invention.
The composite material of the invention is formed by blending liquid metal and macromolecules. Adding liquid metal into a polymerization monomer solution, and performing low-temperature ultrasonic dispersion to obtain a liquid metal micro/nano-scale dispersed precursor dispersion liquid; and transferring the gel into a mold for standing after the gel is formed, thereby obtaining the liquid metal/polymer composite dielectric material. The liquid metal is one or more of gallium, binary alloy of gallium and ternary alloy of gallium, and the polymerization monomer comprises one or more of acrylic acid, acrylamide, acrylonitrile, methyl acrylate and methyl methacrylate. The preparation method is simple and convenient, and the prepared composite material has excellent dielectric property and better tensile property than the traditional dielectric material, and has wide application prospect in the fields of wearable electronic equipment, soft robots and the like.
The composite material is flexible, and the liquid metal with high thermal conductivity is added into the polymer substrate, so that the mechanical property of the traditional dielectric material is improved, the composite material has more excellent flexibility and elasticity, the elongation at break can reach 1600 percent at most, and the requirements of development of wearable equipment and the electronic industry can be met.
Example 1
The preparation method of the liquid metal/polymer composite dielectric material comprises the following specific steps:
(1) weighing 3g of acrylic acid in a small sample bottle at room temperature, adding 12g of deionized water, uniformly mixing, and adding 0.17g of gallium-indium alloy; wherein, the mass ratio of gallium to indium in the gallium-indium alloy is 3: 1 g/g.
(2) Placing the sample in the step (1) in a cell disruptor for ultrasonic dispersion and ice bath treatment, wherein the ultrasonic time is 10 minutes and the power is 300W (see figure 1);
(3) and (3) shaking the dispersion liquid in the step (2) for 20 minutes in a shaking table, transferring the dispersion liquid to a plastic culture dish with the diameter of 6mm, sealing, flatly placing and storing for 7 days to obtain the liquid metal/polymer composite dielectric material.
The dielectric properties of the composite material obtained in the example were tested by using an E4980A Agilent instrument and a 609B ferroelectrics instrument after the material exhibited good plasticity during the preparation process (see FIG. 2), the dielectric constant was 8.0(25 ℃,10kHz), and the elongation at break of the prepared liquid metal/polymer composite dielectric material was about 900% as measured by using an electronic universal tester (see FIG. 3).
As can be seen from fig. 1, the nano-dispersed liquid metal droplets can be observed by a transmission electron microscope, and the surface is coated with polyacrylic acid, which represents the complexation and crosslinking of gallium ions and macromolecules. As can be seen from FIG. 2, the obtained material can realize various deformations in the preparation process; and from fig. 3 it can be seen that the stress-strain curve of the resulting material, the elongation at break is close to 900%.
Example 2
A method for preparing a liquid metal/polymer composite dielectric material comprises the following specific steps:
(1) weighing 4g of acrylic acid in a small sample bottle at room temperature, adding 12g of deionized water, uniformly mixing, and adding 0.2g of metal gallium into the mixture;
(2) placing the sample in the step (1) in a cell disruptor for ultrasonic dispersion, carrying out ice bath treatment, and carrying out ultrasonic treatment for 15 minutes at a power of 200W;
(3) and (3) shaking the dispersion liquid in the step (2) for 30 minutes in a shaking table, transferring the dispersion liquid to a plastic culture dish with the diameter of 6mm, sealing, flatly placing and storing for 14 days to obtain the liquid metal/polymer composite dielectric material.
The composites obtained in the examples were tested for their properties: the liquid metal/polymer composite dielectric material has elongation at break of about 680 percent and toughness of 3.54MJ/m3The dielectric constant is 8.5(25 ℃,10kHz), and the prepared composite material shows excellent plasticity.
Example 3
A liquid metal/polymer composite dielectric material comprises the following specific steps:
(1) weighing 2.4g of acrylamide in a small sample bottle at room temperature, adding deionized water until the total mass is 16g, adding 52mg of N, N-methylene bisacrylamide after the acrylamide is fully dissolved, and adding 0.14g of gallium-indium alloy after the acrylamide is uniformly dissolved; wherein the mass ratio of gallium to indium in the gallium-indium alloy is 3: 2;
(2) placing the sample in the step (1) in a cell disruptor for ultrasonic dispersion, carrying out ice bath treatment, and carrying out ultrasonic treatment for 20 minutes at a power of 300W;
(3) and (3) shaking the dispersion liquid in the step (2) for 30 minutes in a shaking table, transferring the dispersion liquid to a plastic culture dish with the diameter of 6mm, sealing, flatly placing and storing for 7 days to obtain the liquid metal/polymer composite dielectric material.
The composites obtained in the examples were tested for their properties: the liquid metal/polymer composite dielectric material has an elongation at break of about 750% and a dielectric constant of 8.0(25 ℃,10 kHz).
Example 4
A liquid metal/polymer composite dielectric material comprises the following specific steps:
(1) weighing 1.33g of acrylamide and 0.67g of acrylic acid in a small sample bottle at room temperature, adding deionized water until the total mass is 16g, completely dissolving and uniformly mixing, adding 8mg of N, N-methylene bisacrylamide, dissolving and uniformly mixing, and then adding 0.14g of gallium-indium alloy; wherein the mass ratio of gallium to indium in the gallium-indium alloy is 3: 2;
(2) placing the sample in the step (1) in a cell disruptor for ultrasonic dispersion, carrying out ice bath treatment, and carrying out ultrasonic treatment for 20 minutes at a power of 300W;
(3) and (3) shaking the dispersion liquid in the step (2) for 30 minutes in a shaking table, transferring the dispersion liquid to a plastic culture dish with the diameter of 6mm, sealing, flatly placing and storing for 1 day to obtain the liquid metal/polymer composite dielectric material. The composites obtained in the examples were tested for their properties: the liquid metal/polymer composite dielectric material has an elongation at break of about 2000% and a dielectric constant of 7.8(25 ℃,10 kHz).
Example 5
A liquid metal/polymer composite dielectric material comprises the following specific steps:
(1) weighing 2.33g of acrylonitrile and 0.67g of methyl acrylate in a small sample bottle at room temperature, adding 0.7g of sodium bisulfite dissolved in 2ml of deionized water, uniformly mixing, and then adding 0.17g of gallium-indium-tin alloy and 10ml of water; wherein, the mass ratio of gallium to indium and tin in the gallium-indium-tin alloy is 3: 1: 1.
(2) placing the sample in the step (1) in a cell disruptor for ultrasonic dispersion, carrying out ice bath treatment, and carrying out ultrasonic treatment for 10 minutes at a power of 300W;
(3) and (3) shaking the dispersion liquid obtained in the step (2) for 20 minutes in a shaking table, filtering and washing, transferring to a plastic culture dish with the diameter of 6mm, sealing, flatly placing and storing for 2 days to obtain the liquid metal/polymer composite dielectric material.
The performance test of the composite material obtained in the embodiment is carried out: the liquid metal/polymer composite dielectric material has an elongation at break of about 100% and a dielectric constant of 16.0(25 ℃,10 kHz).
Example 6
A liquid metal/polymer composite dielectric material comprises the following specific steps:
(1) weighing 2g of methyl methacrylate and 0.15g of alkyl vinyl sulfonate in a small sample bottle at room temperature, and then adding 15g of water and 0.2g of gallium-indium alloy; wherein, the mass ratio of gallium to indium in the gallium-indium alloy is 9: 1.
(2) placing the sample in the step (1) in a cell disruptor for ultrasonic dispersion, carrying out ice bath treatment, and carrying out ultrasonic treatment for 20 minutes at a power of 400W;
(3) and (3) placing the dispersion liquid in the step (2) into a shaking table to shake for 30 minutes, filtering and washing, transferring to a plastic culture dish with the diameter of 6mm, sealing, flatly placing and storing for 1 day to obtain the liquid metal/polymer composite dielectric material.
The composite material obtained in the examples was subjected to a performance test: the liquid metal/polymer composite dielectric material has an elongation at break of about 110% and a dielectric constant of 20(25 ℃,10 kHz).
Furthermore, it can be seen from the above embodiments that the composite material obtained by blending and polymerizing the liquid metal and the polymerized monomer not only exhibits higher dielectric properties, but also has plasticity and better flexibility which are not possessed by general composite materials, and in addition, the steps necessary for conventional polymerization reactions such as oxygen removal and nitrogen protection are not required in the preparation process, so that the production efficiency can be improved.
Claims (5)
1. A method for preparing a liquid metal/polymer composite dielectric material is characterized by comprising the following steps:
(1) weighing 3g of acrylic acid in a small sample bottle, adding 12g of deionized water, uniformly mixing, and adding 0.17g of gallium-indium alloy; wherein, the mass ratio of gallium to indium in the gallium-indium alloy is 3: 1 g/g;
(2) placing the sample in the step (1) in a cell disruptor for ultrasonic dispersion, carrying out ice bath treatment, and carrying out ultrasonic treatment for 10 minutes at a power of 300W;
(3) and (3) shaking the dispersion liquid in the step (2) for 20 minutes in a shaking table, transferring the dispersion liquid to a plastic culture dish with the diameter of 6mm, sealing, flatly placing and storing for 7 days to obtain the liquid metal/polymer composite dielectric material.
2. A method for preparing a liquid metal/polymer composite dielectric material is characterized by comprising the following steps:
(1) weighing 4g of acrylic acid in a small sample bottle, adding 12g of deionized water, uniformly mixing, and adding 0.2g of metal gallium into the mixture;
(2) placing the sample in the step (1) in a cell disruptor for ultrasonic dispersion, carrying out ice bath treatment, and carrying out ultrasonic treatment for 15 minutes at a power of 200W;
(3) and (3) shaking the dispersion liquid in the step (2) for 30 minutes in a shaking table, transferring the dispersion liquid to a plastic culture dish with the diameter of 6mm, sealing, flatly placing and storing for 14 days to obtain the liquid metal/polymer composite dielectric material.
3. A method for preparing a liquid metal/polymer composite dielectric material is characterized by comprising the following steps:
(1) weighing 2.4g of acrylamide in a small sample bottle, adding deionized water until the total mass is 16g, adding 52mg of N, N-methylene bisacrylamide after the acrylamide is fully dissolved, and adding 0.14g of gallium-indium alloy after the acrylamide is uniformly dissolved; wherein the mass ratio of gallium to indium in the gallium-indium alloy is 3: 2;
(2) placing the sample in the step (1) in a cell disruptor for ultrasonic dispersion, carrying out ice bath treatment, and carrying out ultrasonic treatment for 20 minutes at a power of 300W;
(3) and (3) shaking the dispersion liquid in the step (2) for 30 minutes in a shaking table, transferring the dispersion liquid to a plastic culture dish with the diameter of 6mm, sealing, flatly placing and storing for 7 days to obtain the liquid metal/polymer composite dielectric material.
4. A method for preparing a liquid metal/polymer composite dielectric material is characterized by comprising the following steps:
(1) weighing 1.33g of acrylamide and 0.67g of acrylic acid in a small sample bottle, adding deionized water until the total mass is 16g, completely dissolving and uniformly mixing, adding 8mg of N, N-methylene bisacrylamide, dissolving and uniformly mixing, and then adding 0.14g of gallium-indium alloy; wherein the mass ratio of gallium to indium in the gallium-indium alloy is 3: 2;
(2) placing the sample in the step (1) in a cell disruptor for ultrasonic dispersion, carrying out ice bath treatment, and carrying out ultrasonic treatment for 20 minutes at a power of 300W;
(3) and (3) shaking the dispersion liquid in the step (2) for 30 minutes in a shaking table, transferring the dispersion liquid to a plastic culture dish with the diameter of 6mm, sealing, flatly placing and storing for 1 day to obtain the liquid metal/polymer composite dielectric material.
5. A liquid metal/polymer composite dielectric material obtained by the method according to any one of claims 1 to 4.
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| EP2431413A1 (en) * | 2009-05-12 | 2012-03-21 | Wuxi Now Materials Corp. | Composite nanogranules from polymer/inorganic nanoparticles, preparation method thereof and use of the same |
| CN109467931A (en) * | 2017-09-07 | 2019-03-15 | 北京化工大学 | A kind of flexible dielectric elastic composite and preparation method thereof based on nanometer liquid metal |
| CN108384039A (en) * | 2018-03-02 | 2018-08-10 | 华南理工大学 | A kind of design method of liquid metal and flexible substrate Interface Adhesion structure |
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