CN115722432B - Metal nanowire flexible electrode facing ion sensor and preparation method thereof - Google Patents
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Abstract
The invention discloses a preparation method of a metal nanowire flexible electrode facing an ion sensor, which comprises the following steps: placing the treated matrix film on a glass plate horizontally, then uniformly depositing an ionic polymer/organic solvent mixed solution on the matrix film by using a spray gun, and then drying the matrix film by using a heating platform to form a bonding layer on the matrix film; uniformly depositing the metal nanowire dispersion liquid on the bonding layer by using a spray gun to form a metal nanowire embedded layer, and then drying the matrix film by using a heating platform; rare metal ions are electrodeposited onto the metal nanowires exposed at the surface of the bonding layer by an electroplating process. The invention also discloses the metal nanowire flexible electrode prepared by the preparation method. The metal nanowire flexible electrode facing the ion sensor and the preparation method thereof provided by the invention have good stability and higher binding force, and meanwhile, harsh environment and equipment are not needed, and the preparation process is simple, convenient, rapid and efficient.
Description
Technical Field
The invention relates to a metal nanowire flexible electrode facing an ion sensor and a preparation method thereof, and belongs to the technical field of ion sensors.
Background
The ion flexible sensor has vivid characteristics such as deformability, super hydrophilicity, biocompatibility and the like, and has wide application prospect in the fields such as medical monitoring, man-machine interaction technology, electronic skin and the like. Flexible electrodes are facing new challenges as one of the key elements in ion flexible sensors to collect ion charge and transmit signals. Standard flexible electrodes are typically prepared by sputtering Indium Tin Oxide (ITO) thin films with excellent conductivity. However, since the ITO film is too brittle to meet the demands of next-generation flexible electronic products, researchers are looking for alternatives to ITO. In the last decade, carbon nanotubes, graphene, metal nanowires and poly (3, 4-ethylenedioxythiophene): polystyrene-sulfonate (PEDOT: PSS) have been used as flexible electrodes. Among them, since metal nanowires have excellent electrical conductivity, thermal conductivity and mechanical flexibility, they can be dispersed in some solvents and printed or coated on different flexible substrates at room temperature to realize low-cost and high-yield production of flexible electrodes, and thus are widely used.
Despite considerable efforts by researchers to develop metal nanowire flexible electrodes with good flexibility and stability, a number of challenges still prevent their use in flexible sensors. First, poor adhesion between the metal nanowire flexible electrode and the substrate can reduce the mechanical stability of the ion sensor. Recently, some researchers have attempted to enhance adhesion by surface modification, using thin polymer layer encapsulation, rapid photon sintering techniques, inversion layer processing methods, and hot pressing. However, adhesion is limited because the interaction between the metal nanowire flexible electrode and the matrix is still caused by poor van der waals forces. At the same time, complex procedures and harsh conditions limit the high-yield production of flexible electrodes of metal nanowires. Second, the poor chemical stability of metal nanowire flexible electrodes is also one of the challenges that hampers their application in flexible sensors. The electrical conductivity of flexible electrodes of metal nanowires is easily deteriorated when exposed to chemically aggressive environments, even when exposed to air for long periods of time. Although embedding metal nanowires into a polymer matrix [ Polyurethane (PU), polydimethylsiloxane (PDMS) ] or mixing metal nanowires with a polymer (PEDOT: PSS) is a promising approach to improve chemical stability, polymers can reduce the conductivity of flexible electrodes and the chemical stability of metal nanowires is still unsatisfactory due to incomplete encapsulation of the polymer.
Disclosure of Invention
The invention aims to solve the technical problem of providing the metal nanowire flexible electrode facing the ion sensor and the preparation method thereof, which have good stability and higher binding force, and meanwhile, no harsh environment and equipment are needed, and the preparation process is simple, convenient, rapid and efficient.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a metal nanowire flexible electrode comprises the following steps:
placing the pretreated matrix film on a glass plate horizontally, uniformly depositing an ionic polymer/organic solvent mixed solution on the matrix film by using a spray gun, drying the matrix film by using a heating platform, and solidifying the ionic polymer after the organic solvent is evaporated to form a bonding layer on the matrix film;
uniformly depositing a metal nanowire dispersion liquid on the bonding layer by using a spray gun, wherein an organic solvent in the metal nanowire dispersion liquid can remelt the surface of the solidified bonding layer to form a colloidal layer, partially embedding the metal nanowire into the colloidal layer under the action of speed and gravity to form a metal nanowire embedded layer, drying a matrix film by using a heating platform, and re-solidifying the colloidal layer after the organic solvent is evaporated;
rare metal ions are electrodeposited onto the metal nanowires exposed at the surface of the bonding layer by an electroplating process.
The pretreatment of the matrix film comprises the following steps:
polishing the front and back surfaces of the matrix film by adopting a sand blasting treatment mode;
carrying out ultrasonic cleaning treatment on the polished substrate film;
performing hydrochloric acid boiling and washing treatment on the ultrasonic-cleaned matrix film;
and (3) performing deionized water boiling treatment on the substrate film after hydrochloric acid boiling.
The sand blasting treatment specifically comprises the following steps: the sand blasting adopts quartz sand of No. 120, the sand blasting pressure is 0.4MPa, each side of the matrix film is polished for 30 seconds, and a sand blaster does Z-shaped uniform motion in the polishing process.
The ultrasonic cleaning treatment specifically comprises the following steps: deionized water was heated to 60 c and then the substrate film was placed therein for a cleaning time of 30 minutes.
The hydrochloric acid boiling and washing treatment specifically comprises the following steps: the hydrochloric acid concentration was such that 0.2mol/L HCl was heated to 100℃and then the base film was put therein for a boiling time of 30 minutes.
The deionized water is boiled and washed specifically as follows: the matrix film was boiled in deionized water heated to 100 ℃ for 30min.
The preparation of the ionic polymer/organic solvent mixed solution comprises the following steps: firstly, mixing a certain amount of ionic polymer liquid with an organic solvent a, wherein the organic solvent a is a high-boiling point organic solvent, and then sequentially carrying out magnetic stirring and ultrasonic dispersion to ensure that the ionic polymer liquid is completely dispersed in the organic solvent a to form an ionic polymer/organic solvent mixed solution.
The preparation of the metal nanowire dispersion liquid comprises the following steps: firstly, mixing the metal nanowires with an organic solvent b, wherein the organic solvent b is a low-boiling-point organic solvent, and then stirring the mixture at room temperature by ultrasonic waves to ensure that the silver nanowires are completely dispersed in the organic solvent b to form a metal nanowire dispersion liquid.
The aperture of the spray gun is smaller than 0.5mm, and the pressure is 0.15Mpa.
The metal nanowire flexible electrode is prepared by the preparation method of the metal nanowire flexible electrode, and the metal nanowire flexible electrode comprises a bonding layer, a metal nanowire embedded layer and a metal nanowire network layer.
The invention has the beneficial effects that: the invention provides a metal nanowire flexible electrode facing an ion sensor and a preparation method thereof, which are inspired by a biological hair structure,the spraying process and the electroplating process are integrated, so that the bonding layer is firmly attached to the surface of the matrix film, one half of the metal nanowire is embedded in the bonding layer to fix the flexible electrode, and the other half of the metal nanowire is exposed on the surface of the bonding layer, so that the flexible electrode has good conductivity; compared with the traditional metal nanowire flexible electrode, the electrode prepared by the process has good stability, the binding power can reach 358KPa, and the electrode can bear hundreds of washing cycles and can be soaked in water for a long time; meanwhile, as the metal nanowire is wrapped by gold, the electrode has excellent chemical stability and is characterized in H 2 O 2 After corrosion in medium corrosion for 200s or in HCl for 1500s, the conductivity is hardly changed; compared with the traditional flexible sensor electrode preparation process, the technology does not need harsh environment and equipment, has the characteristics of simplicity, convenience, rapidness, high efficiency and the like, has very high universality, and lays a foundation for industrial assembly line preparation.
Drawings
In fig. 1, part a is the structure of biological hair, and part b is a schematic diagram of the structure of the metal nanowire flexible electrode with the structure similar to the biological hair, which is prepared by the invention;
FIG. 2 is a schematic cross-sectional view of a flexible electrode with a metal nanowire having a biological hair-like structure prepared by the method;
FIG. 3 is a schematic view of the microstructure of the surface of the flexible electrode with the metal nanowire having the biological hair-like structure prepared by the invention.
Detailed Description
The present invention will be further described with reference to the accompanying drawings, and the following examples are only for more clearly illustrating the technical aspects of the present invention, and are not to be construed as limiting the scope of the present invention.
Taking an ion flexible sensor for preparing a metal nanowire flexible electrode with a biological hair-like structure, the size of which is about 3cm multiplied by 2cm, as an example, the preparation method of the invention specifically comprises the following steps:
step one, pretreatment of a matrix film.
The matrix membrane adopted by the invention is a Nafion membrane, and pretreatment is needed before use, and mainly comprises sand blasting treatment and surface cleaning. The sand blasting is to form a large number of grooves and undercuts (see position 5 in fig. 2) on the surface of the base film to increase the surface roughness of the base film and to increase the contact point density of the adhesive layer. Firstly, cutting a piece of matrix film with the thickness of 3.5cm multiplied by 2.5cm, fixing the matrix film by adopting a special clamping device, only exposing the area with the thickness of 3cm multiplied by 2cm, polishing, and cutting out more matrix films with the thickness of 0.5cm for the convenience of fixing. During sand blasting, quartz sand of No. 120 is adopted for sand blasting. The pressure of sand blasting is 0.4MPa, each side of the matrix film is polished for 30 seconds, a sand blaster does Z-shaped uniform motion in the polishing process, and after polishing, a part of 0.5cm for clamping is cut off.
The surface cleaning comprises ultrasonic cleaning, hydrochloric acid boiling cleaning and ion water boiling cleaning.
a. Ultrasonic cleaning: the step adopts an ultrasonic cleaner to clean the matrix film, mainly for removing impurities remained on the surface of the matrix film in the roughening process. In ultrasonic cleaning, deionized water is heated to 60 ℃ and then the substrate film is put in the ultrasonic cleaning device for about 30 minutes.
b. Boiling and washing with hydrochloric acid: the step is mainly used for removing impurity ions and other ions in the matrix film, purifying counter ions H-in the matrix film, converting the counter ions into H+, increasing the content of hydrogen ions in the matrix film, and facilitating ion exchange reaction in the soaking reduction plating process. The hydrochloric acid is boiled and washed by adopting 0.2mol/L HCl, 200ml of the HCl is taken and placed in a beaker, the mixture is heated to be close to 100 ℃ in a constant-temperature water bath, and then the substrate film with the surface cleaned is placed in the beaker for 30min.
c. Boiling and washing with deionized water: this step is to increase the water storage capacity of the IPMC material. The deionized water is boiled and washed for 30min in deionized water heated to 100 deg.c after the hydrochloric acid boiling and washing is completed.
Preparing a metal nanowire flexible electrode to prepare a required solution, wherein the solution comprises an ionic polymer/organic solvent mixed solution required by a bonding layer and a metal nanowire dispersion liquid.
a. Solution required for tie layer (Nafion/DMAC solution):
the ionic polymer liquid used in this example was Nafion solution (20% strength) and the high boiling point organic solvent was DMAC solution (99.5% purity). First, 2g of a Nafion solution and 10g of a DMAC solution were mixed, and then the mixed solution was sequentially magnetically stirred (room temperature, 2 hours) and ultrasonically dispersed (room temperature, 2 hours) so that the Nafion solution was completely dispersed in the DMAC solution, forming a Nafion/DMAC mixed solution required for the adhesive layer.
b. Metal nanowire dispersion (AgNWs/EtOH dispersion):
the metal nanowires used in this example were silver nanowires (AgNWs, concentration 20%), the low boiling point organic solvent was absolute ethanol (EtOH, purity 99%). The AgNWs solution (1 mL) and EtOH solvent (50 mL) were first mixed and then sonicated at room temperature for 1 hour to allow the AgNWs to fully disperse in the EtOH solvent, forming an AgNWs/EtOH dispersion.
Step three, the preparation flow is as follows:
a. preparation of an adhesive layer:
this step is to form an adhesive layer on the surface of the base film. The treated Nafion film is horizontally placed on a glass plate, and the two sides of the film are clamped by using a clamp, so that the Nafion film is prevented from swelling and deforming after absorbing DMAC solvent. The Nafion/DMAC solution was then deposited uniformly on the surface of the Nafion film using a spray gun (0.3 mm nozzle, 0.15 MPa). At the same time, drying was performed using a heated platen. After the DMAC solution is evaporated, the Nafion solution in the Nafion/DMAC solution solidifies to form the tie layer (see position 4 in fig. 2).
Preparation of AgNWs embedded layer:
the AgNWs/EtOH dispersion was deposited uniformly on the tie layer using a spray gun (0.3 mm nozzle, 0.15 Mpa). The EtOH solvent in AgNWs/EtOH dispersion re-melts the surface of the already cured tie layer, presenting a thin gel-like layer. AgNWs can intercalate into the gel-like layer under the action of velocity and gravity, forming an AgNWs intercalation layer (see position 8 in fig. 3), which is important for improving the ion storage capacity and stability of the electrode. In addition, agNWs are not fully embedded in the adhesive layer, and a significant portion of AgNWs are not fully encapsulated by the adhesive layer, and are exposed on the surface of the adhesive layer to form an AgNWs network layer (see position 9 in fig. 3), which is beneficial for signal transmission. At the same time, drying was performed using a heated platen. After the EtOH solvent was evaporated, the gum layer was re-solidified, at which point the AgNWs embedded in the gum layer was firmly fixed.
Agnws plating layer:
in this example, gold ions are used for electroplating, and the gold ions are electrodeposited onto AgNWs exposed on the surface of the adhesive layer by an electroplating process. During the electroplating process, gold ions in the solution are reduced to gold atoms. Since only the mutually overlapping AgNWs are conductive, gold atoms are selectively deposited on the AgNWs, forming a protective gold shell on the AgNWs surface. At the same time, after electrodeposition, the gold atoms crystallize and fill the gaps between AgNWs and weld them tightly together (see position 10 in fig. 3).
Part a of fig. 1 shows the structure of a biological hair, macroscopically composed of three functional layers, including a tip layer, a root insert layer, and a skin layer. The hair roots are wrapped in the skin to prevent hair from falling off, and the hair tips are exposed on the surface of the skin to maintain the body temperature and protect the skin. Similar to the biological hair structure, the electrode prepared by this process also has three functional layers, including an adhesive layer, an AgNWs intercalating layer (see position 3 in fig. 1) and an AgNWs network layer (see positions 1 and 2 in fig. 1), corresponding to the skin layer, the root intercalating layer, and the tip layer, respectively, of the biological hair structure. Compared with the traditional metal nanowire flexible electrode, the electrode has excellent binding force and ultralow surface resistance.
Fig. 2 shows a cross section of the prepared electrode. The highlight part is the electrode (see position 4 in fig. 2) and the black part with the corrugation is the matrix film (see position 6 in fig. 2). It can be clearly observed that the undercut and the groove of the surface of the base film are filled with the adhesive layer, and that there is no gap between the adhesive layer and the base film (see position 5 in fig. 2). Fig. 3 shows the microscopic morphology and corresponding schematic of the prepared electrode. The transparent part is an adhesive layer (see position 7 in fig. 3). It can be clearly observed that one end of AgNWs is firmly embedded in the adhesive layer (see position 8 in fig. 3), similar to the root of a biological hair, for fixationElectrodes and increase the contact area of the interface layer. The other end is exposed at the surface of the adhesive layer and overlaps each other (see position 9 in fig. 3), similar to the tip of a biological hair, for transmitting a sensing signal. This structure effectively enhances the adhesion and contact area between the flexible electrode and the membrane compared to the original AgNWs flexible electrode. Furthermore, it was found that after electrodeposition of gold, the diameter of the AgNWs exposed at the surface of the adhesive layer was significantly larger than the AgNWs embedded in the adhesive layer, since the former was surrounded by a protective shell of gold. And after electrodeposition, the edge profile of AgNWs disappeared at the junction, indicating that gold atoms filled in the gaps at the nanowire-nanowire junction and welded them together. Notably, the sheet resistance of the flexible electrode can be reduced from 1500Ω/≡to 4Ω/≡by the electroplating step, mainly due to the welded connection of AgNWs after electrodeposition. Experiments prove that the binding power of the prepared electrode can reach 358Kpa, and the relative change (delta R/R0) of the resistance is about 14.6 percent after 100 washing cycles are carried out in deionized water. Meanwhile, the AgNWs are wrapped by gold, so that the electrode has excellent chemical stability and is characterized by H 2 O 2 After 200s corrosion or 1500s corrosion in HCl, the conductivity was hardly changed. Finally, a self-powered ion flexible sensor is prepared by using the electrode so as to realize double sensing of mechanical strain and environmental humidity. The prepared sensor shows satisfactory stability and durability, and still has good perceptibility after being stored in air for two months, which further indicates the potential application of the metal nanowire flexible electrode with the biological hair-like structure in the next-generation multifunctional flexible electronic device.
The foregoing is only a preferred embodiment of the invention, it being noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the invention.
Claims (7)
1. A preparation method of a metal nanowire flexible electrode is characterized by comprising the following steps of: the method comprises the following steps:
placing the pretreated matrix film on a glass plate, uniformly depositing an ionic polymer/organic solvent mixed solution on the matrix film by using a spray gun, drying the matrix film by using a heating platform, and solidifying the ionic polymer after the organic solvent is evaporated to form a bonding layer on the matrix film, wherein the preparation of the ionic polymer/organic solvent mixed solution comprises the following steps: firstly, mixing a certain amount of ionic polymer liquid with an organic solvent a, and then sequentially carrying out magnetic stirring and ultrasonic dispersion to ensure that the ionic polymer liquid is completely dispersed in the organic solvent a to form an ionic polymer/organic solvent mixed solution, wherein the ionic polymer liquid is a Nafion solution, and the organic solvent a is a DMAC solution;
uniformly depositing a metal nanowire dispersion liquid on the adhesive layer by using a spray gun, wherein the aperture of a nozzle of the spray gun is smaller than 0.5mm, the pressure is 0.15Mpa, an organic solvent in the metal nanowire dispersion liquid can remelt the surface of the cured adhesive layer to present a colloidal layer, the metal nanowire is partially embedded into the colloidal layer under the action of speed and gravity to form a metal nanowire embedded layer, then drying a matrix film by using a heating platform, and resolidifying the colloidal layer after the organic solvent is evaporated, wherein the preparation of the metal nanowire dispersion liquid comprises the following steps: firstly, mixing a metal nanowire with an organic solvent b, and then stirring the mixture at room temperature by ultrasonic waves to ensure that the silver nanowire is completely dispersed in the organic solvent b to form a metal nanowire dispersion liquid, wherein the metal nanowire is silver nanowire AgNWs, and the organic solvent b is absolute ethyl alcohol;
rare metal ions, which are gold ions, are electrodeposited onto the metal nanowires exposed at the surface of the bonding layer by an electroplating process, and the gold atoms crystallize and fill the gaps between AgNWs and weld them tightly together.
2. The method for preparing the metal nanowire flexible electrode according to claim 1, wherein the method comprises the following steps: the pretreatment of the matrix film comprises the following steps:
polishing the front and back surfaces of the matrix film by adopting a sand blasting treatment mode;
carrying out ultrasonic cleaning treatment on the polished substrate film;
performing hydrochloric acid boiling and washing treatment on the ultrasonic-cleaned matrix film;
and (3) performing deionized water boiling treatment on the substrate film after hydrochloric acid boiling.
3. The method for preparing the metal nanowire flexible electrode according to claim 2, wherein the method comprises the following steps: the sand blasting treatment specifically comprises the following steps: the sand blasting adopts quartz sand of No. 120, the sand blasting pressure is 0.4MPa, each side of the matrix film is polished for 30 seconds, and a sand blaster does Z-shaped uniform motion in the polishing process.
4. The method for preparing the metal nanowire flexible electrode according to claim 2, wherein the method comprises the following steps: the ultrasonic cleaning treatment specifically comprises the following steps: deionized water was heated to 60 c and then the substrate film was placed therein for a cleaning time of 30 minutes.
5. The method for preparing the metal nanowire flexible electrode according to claim 2, wherein the method comprises the following steps: the hydrochloric acid boiling and washing treatment specifically comprises the following steps: the hydrochloric acid concentration was such that 0.2mol/L HCl was heated to 100℃and then the base film was put therein for a boiling time of 30 minutes.
6. The method for preparing the metal nanowire flexible electrode according to claim 2, wherein the method comprises the following steps: the deionized water is boiled and washed specifically as follows: the matrix film was boiled in deionized water heated to 100 ℃ for 30min.
7. A metal nanowire flexible electrode, characterized by: a metal nanowire flexible electrode prepared by the method for preparing a metal nanowire flexible electrode according to any one of claims 1 to 6, wherein the metal nanowire flexible electrode comprises a bonding layer, a metal nanowire embedded layer and a metal nanowire network layer.
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| CN106910551A (en) * | 2017-02-14 | 2017-06-30 | 哈尔滨工业大学深圳研究生院 | One kind plating metal enhancing nesa coating and preparation method thereof |
| CN109426386A (en) * | 2017-08-31 | 2019-03-05 | 宸鸿光电科技股份有限公司 | Touch panel and preparation method thereof |
| CN109559843A (en) * | 2018-11-23 | 2019-04-02 | 合肥京东方光电科技有限公司 | Transparent flexible electrode film, production method and transparent flexible electrode |
| CN111830088A (en) * | 2020-07-30 | 2020-10-27 | 河海大学常州校区 | Ionic type film humidity sensor and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106910551A (en) * | 2017-02-14 | 2017-06-30 | 哈尔滨工业大学深圳研究生院 | One kind plating metal enhancing nesa coating and preparation method thereof |
| CN109426386A (en) * | 2017-08-31 | 2019-03-05 | 宸鸿光电科技股份有限公司 | Touch panel and preparation method thereof |
| CN109559843A (en) * | 2018-11-23 | 2019-04-02 | 合肥京东方光电科技有限公司 | Transparent flexible electrode film, production method and transparent flexible electrode |
| CN111830088A (en) * | 2020-07-30 | 2020-10-27 | 河海大学常州校区 | Ionic type film humidity sensor and preparation method thereof |
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