CN109467931B - Flexible dielectric elastomer composite material based on nano liquid metal and preparation method thereof - Google Patents
Flexible dielectric elastomer composite material based on nano liquid metal and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a flexible dielectric elastomer composite material based on nano liquid metal, which comprises an elastomer and the liquid metal and is prepared by the following steps: preparing mercaptan-coated nano liquid metal emulsion by ultrasonic crushing, dissolving an elastomer in a solvent, mixing with the nano liquid metal emulsion and uniformly stirring to obtain a liquid metal/elastomer/solvent suspension, and forming a film by adopting a hot pressing method or curing at room temperature to obtain the flexible dielectric elastomer composite material. The invention improves the dielectric constant of the composite material, effectively reduces the dielectric loss, and does not remarkably increase the elastic modulus, thereby solving the problems of poor compatibility and flexibility and the like of the traditional inorganic rigid filler modified dielectric elastomer and preparing the liquid metal-based dielectric elastomer composite material which can meet the technical requirements of flexible wearable.
Description
Technical Field
The invention relates to the field of dielectric materials, and further relates to a flexible dielectric elastomer composite material and a preparation method thereof.
Background
In recent years, with the development of wearable technology, flexible robots, and other fields, the development of flexible electronic systems for sensing, driving, and energy conversion has become one of the core tasks. In which the dielectric elastomer material is a polysiloxane, polyurethane or block copolymerThe chemical properties are usually obtained by adding 10-30% volume fraction of inorganic filler, which may be silver (Ag) powder, Ag-coated nickel (Ni) microspheres, structured Carbon Black (CB), exfoliated graphite, Carbon Nanotubes (CNT), barium titanate (BaTiO)3) Titanium dioxide (TiO)2) Other metals, carbon-based or ceramic micro/nanoparticles. While rigid particles are incorporated into the elastomer matrix to increase the composite dielectric constant, the inherent stiffness of the inorganic filler particles does not match the flexibility of the soft, stretchable elastomer matrix, resulting in internal stress concentrations, delamination and friction, increasing system stiffness, decreasing ductility, while limiting the durability of the material in mechanical response.
In the Chinese patent application "high dielectric composite material containing carbon nanotube and method for preparing the same" (patent application No. 03104776.9), the use of carbon nanotube CNT and barium titanate (BaTiO) is proposed3) And an organic polyvinylidene fluoride having a dielectric constant of up to 450. However, in the case of a composite material filled with a conductive filler, the dielectric loss of the material is greatly increased near the percolation threshold due to current leakage and the like. High dielectric loss materials greatly limit the applications of composite materials. In addition, barium titanate BaTiO3The large amount of the filler is difficult to disperse, the viscosity of the material is increased, the processing and forming performance is reduced, the quality of the final material is reduced, the modulus of the material is increased, and the material can deform under a high voltage field, so that the application of the material in the flexible dielectric elastomer is limited.
To prepare a Dielectric elastomer material with both flexibility and Dielectric properties, Carmel et al propose to add Liquid Metal as a filler to an elastomer matrix in Stretchable, High-k Dielectric materials through Liquid-Metal Inclusions, advanced Material,2016,28, 3726-containing 3731, but the size of the Liquid Metal filler is in the micron level, which cannot be well compatible with Elastomers, is prone to mechanical defects, and has a High percolation value of the filler.
Jiang et al, in Nanodroplets for Linear Superconducting Circuits, adv.Funct.Mater, 2016, 8111-.
Disclosure of Invention
The invention provides a flexible dielectric elastomer composite material based on nano liquid metal and a preparation method thereof, which solve the technical problems that: (1) the problem that the flexibility of an elastomer is not matched with the rigidity of an inorganic filler in the dielectric composite material; (2) the liquid metal is distributed in the elastomer in a micron level, and can not play the role of the nano filler; (3) the problem that the high dielectric constant and the low dielectric loss of the dielectric composite material can not be considered simultaneously.
One of the purposes of the invention is to provide a flexible dielectric elastomer composite material based on nano liquid metal, which comprises the following blended components in parts by weight:
100 parts of elastomer;
30-900 parts of liquid metal; preferably 100 to 400 parts.
The liquid metal dosage is too small, and the dielectric property of the obtained composite material is not obviously influenced; too much liquid metal is used, which is not favorable for compounding with the elastic matrix due to its fluidity. The mass fraction of liquid metal is greater because its density is around 6, much higher than the elastomer matrix.
Wherein the liquid metal is a eutectic alloy with a melting point lower than 20 ℃, preferably at least one of gallium (Ga), indium (In), tin (Sn) eutectic alloy or gallium (Ga), indium (In) eutectic alloy.
The liquid metal is dispersed in the elastomer in a dispersed phase, and the average particle diameter of the liquid metal when mixed with the elastomer is 20nm to 200nm, preferably 60nm to 120 nm.
The elastomer is at least one of room temperature vulcanized silicone Rubber (RTV) and thermoplastic elastomer.
The thermoplastic elastomer is preferably any one or more of thermoplastic polyurethane elastomer (TPU), styrenic thermoplastic elastomer (e.g., SBS, SEBS, SIS).
The invention also aims to provide a preparation method of the dielectric elastomer composite material, which comprises the following steps:
and dissolving the elastomer in a solvent, mixing with the nano liquid metal emulsion, uniformly stirring to obtain a liquid metal/elastomer/solvent suspension, and forming a film by adopting a hot pressing method or curing at room temperature to obtain the flexible dielectric elastomer composite material.
The method comprises the following specific steps:
step 1, dispersing the liquid metal and mercaptan in a dispersing agent, and performing ultrasonic crushing to obtain stable mercaptan-coated liquid metal nano-droplet emulsion, wherein the volume ratio of the liquid metal to the dispersing agent is 0.2-2%, and preferably 1-2%; the mass ratio of the mercaptan to the liquid metal is 0.5-10%, preferably 1-5%;
step 2, centrifugally separating the liquid metal emulsion to remove supernatant, adding a dispersing agent again, centrifugally washing for 2-3 times, and adding a solvent to obtain an emulsion a, wherein the volume ratio of the liquid metal to the solvent is 0.2% -2%, and preferably 0.5% -1%;
step 3, dissolving the elastomer in the same solvent as in the step 2 to obtain a completely dissolved solution b, wherein the mass ratio of the elastomer to the solvent is 8-30%, and preferably 10-15%; mixing the emulsion a and the solution b according to the using amounts of the elastomer and the liquid metal, and uniformly stirring to obtain a liquid metal/elastomer/solvent suspension;
and 4, forming a film from the liquid metal/elastomer/solvent suspension by a hot pressing method or curing at room temperature to obtain the flexible dielectric elastomer composite material.
The solvent in step 2 and step 3 is an elastomer good solvent, is an organic solvent with a boiling point of less than 80 ℃ under the standard atmospheric pressure, and preferably at least one of ethyl acetate, tetrahydrofuran and toluene.
The thiol is a thiol commonly used in the prior art, and in the present invention, at least one of an alkyl thiol, a furfuryl thiol, and an organosiloxane having a mercapto functional group is preferable.
The dispersant is an organic dispersant generally used in the prior art, and in the present invention, at least one of tetrahydrofuran, acetone, ethanol, methanol, toluene, and ethyl acetate is preferable.
Preferably, the first and second liquid crystal materials are,
in the step 1, the power of ultrasonic crushing is 1000W-2000W, and the time is 0.5-3 h;
in the step 2, the liquid metal emulsion is subjected to mild centrifugation for 20-40min at the centrifugation speed of 1000-3000r/min, the supernatant is removed, and the liquid metal emulsion is subjected to centrifugal washing again for 2-3 times under the same conditions.
In the step 4, if the elastomer is room temperature vulcanized silicone rubber, adding a crosslinking system into the liquid metal/elastomer/solvent suspension, wherein the mass ratio of the crosslinking system to the elastomer is 3% -10%, preferably 5% -8%, and curing at room temperature to obtain the flexible dielectric elastomer composite material with a smooth surface;
if the elastomer is a thermoplastic elastomer, a crosslinking system is not needed, and the flexible dielectric elastomer composite material is obtained by adopting a hot-pressing method to form a film.
In the step 4, the crosslinking system is a crosslinking system commonly used for silicone rubber, and comprises a crosslinking agent and a catalyst, and the proportion is also a common proportion. Generally, the cross-linking agent is preferably at least one of tetraethoxysilane and oligomer hydrosilicon compound; the catalyst is preferably at least one of an organotin catalyst, a castt catalyst or chloroplatinic acid.
The crosslinking system of the silicone rubber can also be selected from a commercial silicone rubber crosslinking system in which a crosslinking agent and a catalyst are already matched, such as a B component of a prepared crosslinking system DC3481 sold by Dow Corning company, and contains an ethyl orthosilicate crosslinking agent and a dibutyltin dilaurate catalyst.
In the film forming by the hot pressing method, the pressure is 0.5MPa to 1MPa, and the temperature is 20 ℃ to 30 ℃ higher than the melting temperature of the thermoplastic elastomer.
According to the invention, the mercaptan is used for coating the liquid metal nano liquid drops, and the mercaptan forms an organic molecular layer on the surface of the liquid drops through self-assembly, so that the liquid metal can be effectively prevented from being oxidized, the agglomeration among the nano liquid drops is reduced, the dielectric loss can be obviously reduced, and the blending uniformity of the liquid metal and the elastomer is improved, thereby obtaining the elastomer composite material with both flexibility and excellent dielectric property, and meeting the technical requirements in the field of wearable and flexible electronic systems.
When the flexible dielectric elastomer composite material based on the nano liquid metal prepared by the invention takes the silicon rubber as an elastomer matrix, the dielectric constant of the flexible dielectric elastomer composite material can be improved by 825% compared with that of pure silicon rubber, the dielectric loss is kept at a lower level of less than 0.1, meanwhile, the elongation at break of the flexible dielectric elastomer composite material is more than 200%, and the elastic modulus is not increased significantly.
Detailed Description
The invention is further described with reference to the following examples:
description of related Performance tests：
The method for measuring the particle size of the nano liquid metal emulsion is to utilize Dynamic Light Scattering (DLS) to test the average particle size of the nano liquid metal emulsion, and the adopted instrument is a Malvern laser particle size analyzer, which comprises the following steps: and after the ultrasonic treatment is finished, taking 10mL of stable liquid metal nano emulsion, placing the stable liquid metal nano emulsion in a cuvette which is transparent on four sides, and placing the cuvette in a laser particle size analyzer for testing to obtain the average particle size of the metal nano emulsion.
In the comparative example, the size of the liquid droplet of the liquid metal emulsion is specifically observed by a scanning electron microscope during simple mechanical blending, and the specific steps are as follows: preparing a sample of the ground liquid metal, observing the surface appearance by using a scanning electron microscope (S-4800), and carrying out particle size statistics by combining NanoMeasurer software to obtain the average particle size of the liquid metal.
The dielectric property determination method of the flexible dielectric elastomer composite material comprises the following steps: diluting the conductive silver adhesive with acetone, and brushing the upper surface and the lower surface of the prepared flexible dielectric elastomer composite circular electrode plate with the thickness of 0.5mm and the upper and lower surface areas of 10mm x 10mm uniformly by using a fine brush; then drying the conductive silver adhesive in a blast oven at 60 ℃ to solidify the conductive silver adhesive to prepare an electrode; a Novocontrol broadband dielectric impedance spectrometer is adopted, and the test 10 is performed according to the reference standard GB/T1693-2007 of the dielectric constant and the dielectric loss tangent of vulcanized rubber at room temperature-1-107Dielectric constant and dielectric loss in the frequency range of Hz.
Tensile testing was performed on the composite bars at a tensile rate of 50mm/min using a tensile machine (CMT4104) from Shenzhen SANs at room temperature to measure the modulus of elasticity and elongation at break. The composite material membrane is cut into rectangular sample strips with the specification of 8cm by 1cm in length and width, the membrane thickness is about 0.5mm, and strain data corresponding to 5% of strain before linear fitting is carried out to obtain the elastic modulus. The modulus and elongation at break of the rubber composite are tested with reference to the GB/T528-2009 standard. The relevant test data are shown in table 1.
Example 1: M/R33: 100
The nanometer liquid metal/elastomer flexible dielectric composite material is prepared by taking silicone rubber DC3481 of Dow Corning company as an elastomer matrix.
(1) 1g of Galinstan liquid metal (liquid metal available from alfa having a composition of Ga: In: Sn: 62 wt%: 22 wt%: 16 wt%, density 6.359 g/cm)3Melting point of 10.7 ℃), 0.02g of 3-mercaptopropyltriethoxysilane (KH580) is added into 70mL of absolute ethyl alcohol, ice-water bath and 2000W ultrasonic pulverization is carried out for 30min, and liquid metal is dispersed into spherical liquid drops with average particle size of about 85nm to obtain stable nano liquid metal emulsion;
(2) inverting the obtained nano liquid metal emulsion into a centrifuge tube, carrying out mild centrifugation at 3000r/min for 30min, removing supernatant, carrying out centrifugal washing for 2-3 times by using absolute ethyl alcohol, and adding 50mL of ethyl acetate to obtain dispersed nano liquid metal emulsion after washing is finished;
(3) dissolving 3g of DC3481 in 20mL of ethyl acetate, mixing the obtained solution with the nano liquid metal emulsion, adding a crosslinking system DC3481B component prepared by Dow Corning company, an ethyl orthosilicate crosslinking agent and 0.3g of dibutyltin dilaurate catalyst, and curing at room temperature to obtain the liquid metal/silicon rubber flexible dielectric elastomer composite material.
Example 2: M/R100: 100
The preparation method is the same as example 1, except that the content of Galinstan liquid metal in the step (1) is 3g, the content of KH580 is 0.06g, the content of absolute ethyl alcohol is 100mL, the content of ethyl acetate in the step (2) is 70mL, and the average particle size of the liquid metal is 99 nm. The test method was the same as in example 1, and the test results are shown in Table 1.
Example 3: M/R300: 100
The preparation method is the same as example 1, except that the content of Galinstan liquid metal in the step (1) is 9g, the content of KH580 is 0.09g, the content of absolute ethyl alcohol is 150mL, and the content of ethyl acetate in the step (2) is 100 mL. The average particle size of the liquid metal was 95nm, the test method was the same as in example 1, and the test results are shown in Table 1.
Example 4: M/R900: 100
The preparation method is the same as example 1, except that the content of Galinstan liquid metal in the step (1) is 27g, the content of KH580 is 0.27g, the content of absolute ethyl alcohol is 250mL, and the content of ethyl acetate in the step (2) is 150 mL. The average particle size of the liquid metal was 106nm, the test method was the same as in example 1, and the test results are shown in Table 1.
Comparative example 1:
the comparative example adopts a simple mechanical blending method, and the liquid metal is blended with a silicon rubber DC3481 elastomer matrix in the size of tens of microns to prepare the liquid metal/elastomer dielectric composite material.
(1) 3g of Galinstan liquid metal and 3gDC3481 silicon rubber matrix are added into a mortar for shearing and blending for 10min, and the particle size of the liquid metal is less than 30 mu m;
(2) and (2) adding 0.3g of a crosslinking system into the blend obtained in the step (1), wherein the crosslinking agent is ethyl orthosilicate and the catalyst is dibutyltin dilaurate, uniformly mixing, placing in a vacuum oven, removing bubbles for 5min, and curing at room temperature to form a film to obtain the composite material. The average particle size of the liquid metal dispersed phase was 20 μm.
The dielectric property and the mechanical property of the obtained liquid metal elastomer composite material are tested by the same test method as in example 1, and the test results are shown in table 1.
Table 1: comparison of the Performance of examples 1-4 with that of comparative example 1
As can be seen from the data in Table 1, the liquid metal flexible dielectric elastomer composite material prepared by the method provided by the invention has the advantages that the dielectric constant is improved by 825% at most compared with the dielectric constant of pure DC3481 (the dielectric constant of pure DC3481 is 4), the dielectric loss is kept at a lower level (the dielectric loss is less than or equal to 0.02), the elastic modulus of the system is not remarkably increased, the value is always less than 1.5MPa, the liquid metal flexible dielectric elastomer composite material is kept very flexible, and the elongation at break is more than 200%.
Example 5: M/R33: 100
The thermoplastic polyurethane elastomer TPU 45A (purchased from Basff) with Tetrahydrofuran (THF) solubility of 98% is used as an elastomer matrix to prepare the nano liquid metal/elastomer flexible dielectric composite material.
(1) 1g of Galinstan liquid metal (the liquid metal is purchased from alfa company and contains Ga: In: Sn: 62 wt%: 22 wt%: 16 wt%, density of 6.359g/cm3 and melting point of 10.7 ℃), 0.02g of 3-mercaptopropyltriethoxysilane (KH580) are added into 70mL of absolute ethyl alcohol, the mixture is subjected to ice-water bath and ultrasonic pulverization at 2000W for 30min, and the liquid metal is dispersed into spherical liquid drops with the average particle size of about 105nm by dynamic light scattering technology, so that stable nano liquid metal emulsion is obtained;
(2) inverting the obtained nano liquid metal emulsion into a centrifuge tube, carrying out mild centrifugation at 3000r/min for 30min, removing supernatant, carrying out centrifugal washing for 2-3 times by using absolute ethyl alcohol, and adding 50mL of tetrahydrofuran after the washing is finished to obtain nano liquid metal emulsion;
(3) dissolving 3g of TPU in 30mL of tetrahydrofuran, mixing the obtained solution with a liquid metal solution, slowly volatilizing at room temperature, basically completely volatilizing THF after 24 hours, and drying the sample in a forced air oven at 80 ℃ for 4 hours;
(4) and (3) hot-pressing the composite material obtained by spreading the solution into a film at the temperature of 170 ℃ and under the pressure of 0.5MPa to obtain the liquid metal/elastomer composite material with a smooth surface.
The obtained composite material was tested for dielectric properties and mechanical properties in the same manner as in example 1, and the test results are shown in table 2.
Example 6: M/R100: 100
The preparation method is the same as example 5, except that the content of Galinstan liquid metal in the step (1) is 3g, the content of KH580 is 0.06g, the content of absolute ethyl alcohol is 100mL, the content of tetrahydrofuran in the step (2) is 70mL, and the average particle size of the liquid metal is 110 nm. The test method was the same as in example 1, and the test results are shown in Table 2.
Example 7: M/R is 200:100
The preparation method is the same as example 5, except that the content of Galinstan liquid metal in the step (1) is 6g, the content of KH580 is 0.09g, the content of absolute ethyl alcohol is 150mL, the content of tetrahydrofuran in the step (2) is 100mL, and the average particle size of the liquid metal is 121 nm. The test method was the same as in example 1, and the test results are shown in Table 2.
Comparative example 2:
the comparative example was prepared in the same manner as example 5 except that the KH580 was used in the step (1) at 0, the ultrasonic power was changed to 1000W, and the average particle size of the liquid metal was about 5 μm. The composite test results are shown in table 2.
Table 2: comparison of the Performance of examples 5-7 with that of comparative example 2
As can be seen from the data in Table 2, the liquid metal flexible dielectric elastomer composite material prepared by the method provided by the invention has the advantages that the dielectric constant is obviously improved, the dielectric loss is also maintained at about 0.01, the dielectric loss is similar to that of pure TPU (0.01 at 1000 Hz), the elastic modulus of the system is not remarkably increased, and the liquid metal flexible dielectric elastomer composite material has good flexibility.
Claims (8)
1. A flexible dielectric elastomer composite based on nanometer liquid metal comprises the following blended components in parts by weight:
100 parts of elastomer;
100-400 parts of liquid metal;
wherein the liquid metal is eutectic alloy with the melting point lower than 20 ℃, and the average particle size of the liquid metal and the elastomer is 20 nm-200 nm when the liquid metal and the elastomer are mixed;
the elastomer is at least one of room temperature vulcanized silicone rubber and thermoplastic polyurethane elastomer;
the liquid metal is gallium, indium and tin eutectic alloy or gallium and indium eutectic alloy;
the flexible dielectric elastomer composite material is prepared by the following steps:
step 1, dispersing the liquid metal and mercaptan in a dispersing agent, and performing ultrasonic crushing to obtain stable mercaptan-coated liquid metal nano-droplet emulsion, wherein the volume ratio of the liquid metal to the dispersing agent is 0.2-2%; the mass ratio of the mercaptan to the liquid metal is 0.5-10%;
step 2, centrifugally separating the liquid metal emulsion to remove supernatant, adding the dispersing agent again, centrifugally washing for 2-3 times, and adding the solvent to obtain emulsion a, wherein the volume ratio of the liquid metal to the solvent is 0.2% -2%;
step 3, dissolving the elastomer in the same solvent as in the step 2 to obtain a completely dissolved solution b, wherein the mass ratio of the elastomer to the solvent is 8-30%; mixing the emulsion a and the solution b according to the mass ratio of the elastomer to the liquid metal, and uniformly stirring to obtain a liquid metal/elastomer/solvent suspension;
step 4, forming a film by the liquid metal/elastomer/solvent suspension through a hot pressing method or curing at room temperature to obtain the flexible dielectric elastomer composite material;
in the step 1, the power of ultrasonic crushing is 1000W-2000W, and the time is 0.5-3 h;
in the step 2, the liquid metal emulsion is subjected to mild centrifugation for 20-40min at the centrifugation speed of 1000-3000r/min, the supernatant is removed, and the liquid metal emulsion is subjected to centrifugal washing again for 2-3 times under the same conditions.
2. The flexible dielectric elastomer composite of claim 1, wherein:
the average particle size of the liquid metal and the elastomer when mixed is 60 nm-120 nm.
3. The method of any one of claims 1-2, comprising the steps of:
step 1, dispersing the liquid metal and mercaptan in a dispersing agent, and performing ultrasonic crushing to obtain stable mercaptan-coated liquid metal nano-droplet emulsion, wherein the volume ratio of the liquid metal to the dispersing agent is 0.2-2%; the mass ratio of the mercaptan to the liquid metal is 0.5-10%;
step 2, centrifugally separating the liquid metal emulsion to remove supernatant, adding the dispersing agent again, centrifugally washing for 2-3 times, and adding the solvent to obtain emulsion a, wherein the volume ratio of the liquid metal to the solvent is 0.2% -2%;
step 3, dissolving the elastomer in the same solvent as in the step 2 to obtain a completely dissolved solution b, wherein the mass ratio of the elastomer to the solvent is 8-30%; mixing the emulsion a and the solution b according to the mass ratio of the elastomer to the liquid metal, and uniformly stirring to obtain a liquid metal/elastomer/solvent suspension;
step 4, forming a film by the liquid metal/elastomer/solvent suspension through a hot pressing method or curing at room temperature to obtain the flexible dielectric elastomer composite material;
in the step 1, the power of ultrasonic crushing is 1000W-2000W, and the time is 0.5-3 h;
in the step 2, the liquid metal emulsion is subjected to mild centrifugation for 20-40min at the centrifugation speed of 1000-3000r/min, the supernatant is removed, and the liquid metal emulsion is subjected to centrifugal washing again for 2-3 times under the same conditions.
4. A method of preparing a dielectric elastomer composite as claimed in claim 3, wherein:
the mercaptan in the step 1 is selected from at least one of alkyl mercaptan, furfuryl mercaptan and organic siloxane containing a mercapto functional group; the dispersing agent is at least one of tetrahydrofuran, acetone, ethanol, methanol, toluene or ethyl acetate;
the solvent in the step 2 and the step 3 is an organic solvent with a boiling point of less than 80 ℃ under the standard atmospheric pressure.
5. The method of preparing a flexible dielectric elastomer composite of claim 3, wherein:
in the step 1, the volume ratio of the liquid metal to the dispersing agent is 1-2%; the mass ratio of the mercaptan to the liquid metal is 1-5%;
in the step 2, the volume ratio of the liquid metal to the solvent is 0.5-1%;
in the step 3, the mass ratio of the elastomer to the solvent is 10-15%.
6. The method of preparing a flexible dielectric elastomer composite of claim 4, wherein:
the organic solvent is at least one of ethyl acetate, tetrahydrofuran and toluene.
7. The method of preparing a flexible dielectric elastomer composite of claim 3, wherein:
in the step 4, if the elastomer is room temperature vulcanized silicone rubber, adding a crosslinking system into the liquid metal/elastomer/solvent suspension, wherein the mass ratio of the crosslinking system to the elastomer is 3-10%, and curing at room temperature to obtain the flexible dielectric elastomer composite material with a smooth surface; if the elastomer is a thermoplastic elastomer, the flexible dielectric elastomer composite material is obtained by adopting a hot-pressing method to form a film.
8. A method of preparing a dielectric elastomer composite as claimed in claim 3, wherein:
in the film forming by the hot pressing method, the pressure is 0.5MPa to 1MPa, and the temperature is 20 ℃ to 30 ℃ higher than the melting temperature of the thermoplastic elastomer.
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| CN114694898B (en) * | 2022-06-01 | 2022-10-14 | 西北工业大学 | Preparation method of MLCC nickel inner electrode slurry |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746595A (en) * | 2012-07-19 | 2012-10-24 | 江南大学 | Method for preparing modified liquid metal soap thermal stabilizer through potassium ion characteristic doping |
| CN104072820A (en) * | 2014-07-03 | 2014-10-01 | 北京化工大学 | Graphene-based dielectric elastomer composite material and preparation method thereof |
-
2017
- 2017-09-07 CN CN201710799538.7A patent/CN109467931B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746595A (en) * | 2012-07-19 | 2012-10-24 | 江南大学 | Method for preparing modified liquid metal soap thermal stabilizer through potassium ion characteristic doping |
| CN104072820A (en) * | 2014-07-03 | 2014-10-01 | 北京化工大学 | Graphene-based dielectric elastomer composite material and preparation method thereof |
Non-Patent Citations (4)
| Title |
|---|
| Directing Substrate Morphology via Self-Assembly: Ligand-Mediated;J. Nathan Hohman, Moonhee Kim et.al,;《Nano Letters》;20111124;说明书第2页第2段 * |
| Metallic nanoemulsion with galinstan for high heat-flux thermal;Yoshikazu Hayashi, Navid Saneie, Gordon Yip, Yoon Jo Kim,et.al;《Internationa Journal of Heat and mass transfer》;20160614;全文 * |
| Soft Multifunctional Composites and Emulsions;Navid Kazem, Tess Hellebrekers, Carmel Majidi;《Advanced Materials》;20170420;全文 * |
| Stretchable, High- k Dielectric Elastomers through;Michael D.Bartlett, Andrew Fassler , Navid Kazem, et.al;《Advance Materials》;20160323;说明书倒数第2页实验部分 * |
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