CN114334212A - Liquid metal nanowire elastic electrode and preparation method thereof - Google Patents
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Abstract
The invention relates to the technical field of flexible elastic materials, and particularly provides a liquid metal nanowire elastic electrode and a preparation method thereof. The liquid metal nanowire elastic electrode provided by the invention has the characteristics of smooth surface, high conductivity, good stretchability and low temperature resistance. The preparation method of the liquid metal nanowire elastic electrode provided by the invention forms the liquid metal nanowire grids in a shell breaking mode of the nanoparticles with the core-shell structure, and has the advantages of simple method, no need of complex and expensive equipment and low manufacturing cost.
Description
Technical Field
The invention relates to the technical field of flexible elastic materials, in particular to a liquid metal nanowire elastic electrode and a preparation method thereof.
Background
Elastic electronics refers to the technology of building electronic circuits by depositing elastic electronic devices and circuits onto an elastic substrate or embedding them completely into an elastic material (a thermoplastic elastomer such as silicone or polyurethane). The elastic electronic equipment can be used for bionic stimulation of human skin and muscle, and can maintain charge transfer and transport functions while bearing large strain. The elastic electrode is the most basic and essential part of an elastic electronic device.
The functional layer of the existing elastic electronic device is usually a thin film, and the structure of the device requires that the electrode is relatively flat. The smoother the electrode surface is, the more uniform the contact resistance distribution with the functional layer is, the more effective the voltage can be applied to the functional layer, and the local aging or fatigue of the functional layer caused by the local electric field can not be formed. In the prior art, the surfaces of the metal nanowires and the nanoparticles, the carbon nanotubes and the elastic electrodes formed by folds are rough, so that the functional layer cannot effectively form uniform surface contact with the electrodes, and local fatigue of devices is easily caused. In addition, the elastic electrodes also have low conductivity and high resistance, which results in high voltage consumed on the electrodes in electronic devices, and further results in high working voltage of the whole devices, and simultaneously results in most of energy waste on the electrode parts, and the high heat generation of the electrodes also results in reduced service life of the elastic electrodes.
The elastic electronic device requires that each part of the device can bear larger strain, for example, the strain of the elastic device for monitoring human body movement or health signals should meet certain requirements, the strain of the elastic device for human body skin should reach 20%, the strain of the elastic device for human body joints should reach 50%, the strain of the elastic device for human body stomach should reach 300%, and the strain of the elastic device for sports equipment should reach 500%. Meanwhile, the elastic device needs to be normally used in various natural climatic conditions, such as north and south poles, various frozen soil zones and deep sea, and even in space. This requires that the elastic electrode operate effectively at low or even very low temperatures, with the lowest temperatures reported in the literature for elastic electrodes being used at-twenty degrees below zero. This is because its conductive component becomes brittle and no longer elastic when the temperature is reduced.
Disclosure of Invention
The invention solves the problem of providing an elastic electrode with smooth surface, high conductivity, large strain resistance and low temperature resistance.
In order to solve the problems, the invention provides a liquid metal nanowire elastic electrode which comprises an elastic support body and liquid metal nanowires, wherein the liquid metal nanowires form a liquid metal nanowire grid on the elastic support body, the liquid metal nanowires are 3nm-200nm in diameter and 5nm-5mm in length, and the surface roughness of the elastic electrode is smaller than 100 nm.
Compared with the prior art, the invention adopts the liquid metal nano wire as the conductive component, and the liquid metal is in a liquid state at the use temperature and has better fluidity, so that the surface smoothness of the elastic electrode is determined, and the elastic electrode has the nanoscale surface roughness; meanwhile, compared with other metal nanowires, metal nanoparticles and graphene, the flowability of the liquid metal at the use temperature is higher, and the conductivity of the elastic electrode can reach 1.6 multiplied by 105S/cm; due to the size effect, the liquid metal nanowire with the diameter of 3nm-200nm and the length of 5nm-5mm can still keep liquid at extremely low temperature, presents elasticity and flowability, and the use temperature can be reduced to 15K.
Preferably, the liquid metal nanowire network is formed by the liquid metal nano particles with the core-shell structure being broken and the liquid metal jets being communicated with each other. The nano particles with the core-shell structure can protect liquid metal inside the shell, and the liquid metal is prevented from being oxidized due to exposure to air in the process of preparing the electrode.
Preferably, the core of the liquid metal nanoparticle with the core-shell structure is liquid metal, and the shell is selected from at least one of liquid metal oxide and organic compound. The liquid metal oxide and the organic compound can form a thin shell on the surface of the liquid metal, so that the subsequent shell breaking treatment is facilitated.
Preferably, the liquid metal is selected from at least one of gallium, gallium indium alloy, and gallium indium tin alloy. Because the metal gallium, the gallium-indium alloy and the gallium-indium-tin alloy are in liquid state at room temperature, the liquid metal nanowire elastic electrode is convenient to use at room temperature.
Preferably, the elastic support is one or more of polyurethane elastomer, styrene elastomer, polyolefin elastomer, polyamide elastomer, polyester elastomer and silicone rubber elastomer. The elastomer has heat resistance, compression deformation resistance and excellent mechanical properties, so when the elastomer is used as an elastic electrode, the elastomer is favorable for realizing the long-term operation stability of the elastic electrode.
The invention also provides a preparation method for preparing the liquid metal nanowire elastic electrode, which is characterized by comprising the following steps of:
s1: placing liquid metal or alloy thereof in an aqueous solution/solution containing at least one of an organic compound and a surfactant under an air atmosphere/inert atmosphere, and enabling the liquid metal to form a nanoparticle dispersion liquid with a core-shell structure under the action of ultrasonic vibration or stirring;
s2: depositing the nanoparticle dispersion liquid of the core-shell structure in the step S1 on an elastic support body in a solution processing mode to form a film with the thickness of 10nm-500nm or a required pattern;
s3: and (3) breaking the core-shell structure nano particles, and communicating liquid metal after the liquid metal is sprayed in space to form a grid, so as to obtain the liquid metal nanowire elastic electrode.
According to the method for preparing the liquid metal nanowire elastic electrode, the liquid metal nanowire grids are formed in a mode of breaking the shells of the nanoparticles with the core-shell structure, the method is simple, complex and expensive equipment is not needed, and the manufacturing cost is low; the electric conductivity of the prepared liquid metal nanowire elastic electrode can reach 1.6 multiplied by 105S/cm, tensile range up to 2000%, surface roughness less than 100nm, and low temperature resistance up to 15K.
Preferably, the organic compound is selected from at least one of organic amine, mercapto compound, hydroxyl-containing compound, or amino-, mercapto-and hydroxyl-containing polymer. The organic compound can act with the liquid metal to form a shell layer on the surface of the liquid metal, and the nano particles have better dispersibility in the solvent and can stably exist for a long time, so that the thin film electrode is processed and prepared by a low-cost solution processing method. Is beneficial to the formation of the liquid metal into the nano particles.
Preferably, the solution processing mode is selected from one of spin coating, drop coating, blade coating, ink-jet printing and screen printing. The solution processing modes of spin coating, drop coating, blade coating, ink-jet printing and screen printing have the advantages of simple and convenient operation and low cost.
Preferably, the surfactant is at least one selected from DMF, NMP, DMSO, DMAc, toluene, xylene, chlorobenzene, dichlorobenzene, hydrocarbons, alcohols, esters. The surfactant is a common chemical reagent, is safe, low in cost and easy to purchase.
Preferably, the breaking mode of the core-shell structure nano particles is selected from one of mechanical sintering, microwave sintering, low-temperature freezing and infrared sintering. The shell of the core-shell structure can be cracked under the action of stress by means of sintering or low-temperature freezing, and then liquid metals in the core are connected with each other to form a grid.
In summary, the present invention provides an elastic electrode using a network formed by liquid metal nanowires as a conductive component and an elastic support as a substrate. Because the liquid metal is in a liquid state at room temperature, the liquid metal has better fluidity and processability and good stress bearing capacity, the prepared elastic electrode has the characteristics of smooth surface, high conductivity, good stretchability and low temperature resistance. The elastic electrode can be applied to elastic sensors, elastic field effect transistors, elastic light emitting diodes, elastic organic solar cells and the like, can effectively improve the efficiency of devices and widen the use scenes of the devices, and has important significance and value.
Drawings
FIG. 1 is a TEM image of a liquid metal nanoparticle prepared in example 2;
FIG. 2 is an AFM image of the surface topography of the liquid metal nanowire elastic electrode in example 2;
FIG. 3 is a graph of the strain-conductivity relationship of the liquid metal nanowire elastic electrode in example 2;
FIG. 4 is a graph of temperature-conductivity relationship of the liquid metal nanowire elastic electrode in example 2;
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
Example 1
The embodiment provides a liquid metal nanowire elastic electrode, which comprises an elastic support body and liquid metal nanowires, wherein the liquid metal nanowires form a liquid metal nanowire grid on the elastic support body, the structure of the liquid metal nanowire grid is shown in fig. 1, an elastic body is filled in gaps among the liquid metal nanowires, the diameter of each liquid metal nanowire is 3nm-200nm, the length of each liquid metal nanowire is 5nm-5mm, and the surface roughness of the elastic electrode is smaller than 100 nm.
In the embodiment, the liquid metal nanowires are used as the conductive components, and the liquid metal is liquid at the use temperature and has good fluidity, so that the surface smoothness of the elastic electrode is determined, and the elastic electrode has nanoscale surface roughness; meanwhile, the liquidity of the liquid metal at the use temperature is higher than that of other metal nanowires and metal nanoparticle graphene, and the conductivity of the elastic electrode can reach 5.4 multiplied by 104S/cm; due to the size effect, the liquid metal nanowire with the diameter of 3nm-200nm and the length of 5nm-5mm can still keep liquid at extremely low temperature, presents elasticity and flowability, and the use temperature can be reduced to 15K.
Example 2
The embodiment provides a preparation method of a gallium nanowire elastic electrode, which comprises the following specific steps:
1) weighing 0.2g of gallium, 10mL of tetrahydrofuran and 0.1g of 1-octadecanethiol, continuously carrying out ultrasonic treatment for 30min under 650W of power, centrifuging for 2000 r/min, and discarding trace precipitates at the bottom of a centrifugal tube; the supernatant was concentrated to about 2mL and allowed to stand to obtain a dispersion. The dispersion can be left at room temperature in an atmospheric environment for more than 6 months without bottom precipitation; after bubbling with argon for 10 minutes, the dispersion was left at 4 ℃ for more than one year without bottom precipitation being observed, and the average particle size of the nanoparticles in the dispersion was about 50 nm.
2) The dispersion is processed into a film. 0.2mL of the dispersion was spin-coated on a polyurethane substrate at 2000 rpm for 30 seconds, and then dried in a vacuum oven overnight to obtain a film having a thickness of about 80nm on the elastic substrate.
3) And (3) placing the film obtained in the step (2) in a molding press, applying a pressure of 10kPa, keeping for 1 minute, and then carrying out morphology, electricity and low temperature resistance tests.
A TEM image of the liquid metal nanoparticles prepared in step 1 of this embodiment is shown in fig. 1, an AFM image of the surface topography of the liquid metal nanowire mesh of the elastic electrode prepared in this embodiment is shown in fig. 2, and the conductivity at room temperature is about 2.5 × 105S/cm, an electrical conductivity at 80K of 1.45X 10 at a tensile strain of 150%5S/cm. The electrical conductivities of the obtained elastic electrodes at different tensile strains are shown in fig. 3, and the electrical conductivities at different temperatures are shown in fig. 4.
Example 3
1) Weighing 0.3g of gallium indium tin alloy, wherein the ratio of gallium indium tin is 7: 2: 1, 10ml N, N' -dimethylformamide and 0.1g polyethylene glycol (molecular weight 650Da) under 950W power for continuous ultrasonic treatment for 30min, centrifuging for 5000 r/min, and discarding the micro-precipitate at the bottom of the centrifugal tube; the supernatant was concentrated to about 4mL and allowed to stand until use, with the nanoparticles having an average particle size of about 20 nm.
2) The dispersion was processed by ink jet printing to form a patterned electrode, which was then dried overnight in a vacuum oven to obtain a film with a thickness of about 80nm on the elastomeric substrate.
3) And (3) placing the film obtained in the step (2) in a molding press, applying a pressure of 240kPa, keeping for 5 minutes, and then carrying out morphology, electrical and low temperature resistance tests. Conductivity of about 4.6X 10 at room temperature4S/cm, conductivity at 30K of 3.8X 104S/cm。
Example 4
1) Weighing 0.3g of gallium indium tin alloy, wherein the ratio of gallium indium tin is 7: 2: 1, 10ml N, N' -dimethylformamide and 0.1g polyethylene glycol (molecular weight 650Da) under 950W power for continuous ultrasonic treatment for 30min, centrifuging for 5000 r/min, and discarding the micro-precipitate at the bottom of the centrifugal tube; the supernatant was concentrated to about 4mL and allowed to stand until use, with the nanoparticles having an average particle size of about 20 nm.
2) The dispersion was processed by ink jet printing to form a patterned electrode, which was then dried overnight in a vacuum oven to obtain a film with a thickness of about 80nm on the elastomeric substrate.
3) And (3) placing the film obtained in the step (2) in a molding press, applying a pressure of 240kPa, keeping for 5 minutes, and then carrying out morphology, electrical and low temperature resistance tests. Conductivity of about 4.6X 10 at room temperature4S/cm, conductivity at 30K of 1.2X 105S/cm。
Example 5
1) Weighing 0.3g of gallium indium tin alloy, wherein the ratio of gallium indium tin is 7: 2: 1, 10ml N, N' -dimethylformamide and 0.1g polyethylene glycol (molecular weight 650Da) under 950W power for continuous ultrasonic treatment for 30min, centrifuging for 5000 r/min, and discarding the micro-precipitate at the bottom of the centrifugal tube; the supernatant was concentrated to about 4mL and allowed to stand until use, with the nanoparticles having an average particle size of about 20 nm.
2) The dispersion was processed by ink jet printing to form a patterned electrode, which was then dried overnight in a vacuum oven to obtain a film with a thickness of about 80nm on the elastomeric substrate.
3) And (3) placing the film obtained in the step (2) in a molding press, applying a pressure of 240kPa, keeping for 5 minutes, and then carrying out morphology, electrical and low temperature resistance tests. Conductivity of about 4.6X 10 at room temperature4S/cm, conductivity at 30K of 1.1X 105S/cm。
Although the present disclosure has been described above, the scope of the present disclosure is not limited thereto. Those skilled in the art can make various changes and modifications without departing from the spirit and scope of the present disclosure, and such changes and modifications will fall within the scope of the present invention.
Claims (10)
1. The liquid metal nanowire elastic electrode is characterized by comprising an elastic support body and liquid metal nanowires, wherein liquid metal nanowire grids are formed on the elastic support body by the liquid metal nanowires, the liquid metal nanowires are 3nm-200nm in diameter and 5nm-5mm in length, and the surface roughness of the elastic electrode is smaller than 100 nm.
2. The liquid metal nanowire elastic electrode according to claim 1, wherein the liquid metal nanowire network is formed by the liquid metal nanoparticles of the core-shell structure being broken and the liquid metal being sprayed and then communicated with each other.
3. The liquid metal nanowire elastic electrode according to claim 2, wherein the core of the liquid metal nanoparticles with the core-shell structure is liquid metal, and the shell is at least one selected from liquid metal oxides and organic compounds.
4. The liquid metal nanowire elastic electrode according to claim 1, wherein the liquid metal is selected from at least one of gallium, gallium indium alloy, and gallium indium tin alloy.
5. The liquid metal nanowire elastic electrode of claim 1, wherein the elastic support is at least one selected from the group consisting of polyurethane elastomers, styrene elastomers, polyolefin elastomers, polyamide elastomers, polyester elastomers, and silicone rubber elastomers.
6. A method for preparing a liquid metal nanowire elastic electrode as claimed in any one of claims 1 to 5, characterized by comprising the following steps:
s1: placing liquid metal or alloy thereof in an aqueous solution/solution containing at least one of an organic compound and a surfactant under an air atmosphere/inert atmosphere, and enabling the liquid metal to form a nanoparticle dispersion liquid with a core-shell structure under the action of ultrasonic vibration or stirring;
s2: depositing the nanoparticle dispersion liquid of the core-shell structure in the step S1 on an elastic support body in a solution processing mode to form a film with the thickness of 10nm-500nm or a required pattern;
s3: and (3) breaking the core-shell structure nano particles, and communicating liquid metal after the liquid metal is sprayed in space to form a grid, so as to obtain the liquid metal nanowire elastic electrode.
7. The method for preparing a liquid metal nanowire elastic electrode according to claim 6, wherein the organic compound is at least one selected from organic amines, mercapto compounds, hydroxyl-containing compounds, and amino, mercapto and hydroxyl-containing polymers.
8. The method for preparing the liquid metal nanowire elastic electrode according to claim 6, wherein the surfactant is selected from one or more of DMF, NMP, DMSO, DMAc, toluene, xylene, chlorobenzene, dichlorobenzene, hydrocarbons, alcohols and esters.
9. The method for preparing a liquid metal nanowire elastic electrode according to claim 6, wherein the solution processing manner is selected from one of spin coating, drop coating, blade coating, ink-jet printing and screen printing.
10. The method for preparing a liquid metal nanowire elastic electrode according to claim 6, wherein the core-shell structure nanoparticle fracture mode is selected from one of mechanical sintering, microwave sintering, low-temperature freezing and infrared sintering.
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| CN110240830A (en) * | 2018-03-09 | 2019-09-17 | 国家纳米科学中心 | The conductive ink of sintering certainly, preparation method and application based on liquid metal particle |
| KR102051134B1 (en) * | 2018-07-03 | 2019-12-17 | 고려대학교 산학협력단 | Method for manufacturing liquid metal mixed electrode |
| US20200139329A1 (en) * | 2018-11-02 | 2020-05-07 | Government Of The United States, As Represented By The Secretary Of The Air Force | Articles comprising core shell liquid metal encapsulate networks and method to control alternating current signals and power |
| CN113527862A (en) * | 2020-04-17 | 2021-10-22 | 北京化工大学 | Stretchable conductive composite material based on liquid metal and preparation method thereof |
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