CN113644192B - Preparation method of asymmetric electrode IPMC and prepared asymmetric electrode IPMC - Google Patents

Preparation method of asymmetric electrode IPMC and prepared asymmetric electrode IPMC Download PDF

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CN113644192B
CN113644192B CN202110913560.6A CN202110913560A CN113644192B CN 113644192 B CN113644192 B CN 113644192B CN 202110913560 A CN202110913560 A CN 202110913560A CN 113644192 B CN113644192 B CN 113644192B
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CN113644192A (en
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常龙飞
王冬平
宋伟
胡颖
朱子才
王延杰
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Hefei University of Technology
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/48—Electroplating: Baths therefor from solutions of gold
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Abstract

The invention discloses a preparation method of an asymmetric electrode IPMC, which relates to the technical field of asymmetric electrode ionic polymer-metal composite materials, and comprises the following steps: (1) Mixing a matrix film solution with an electrode material, and layering to obtain a film solution; (2) subjecting the film solution to film casting treatment to obtain a matrix film; (3) After the substrate film is subjected to reduction plating treatment, an electrode layer is formed on the surface of the film, namely the asymmetric electrode IPMC. The invention also provides the IPMC prepared by the method. The invention has the beneficial effects that: an asymmetric electrode IPMC may be designed, including different materials and asymmetric morphology of the electrode. Therefore, the electrode structure with a specific structure is realized, the adhesive force between the electrode and the matrix film is enhanced, the depth of the permeated electrode is increased, the morphology of the permeated electrode is improved, and the electrochemical performance and the electromechanical performance of the IPMC material are further improved.

Description

Preparation method of asymmetric electrode IPMC and prepared asymmetric electrode IPMC
Technical Field
The invention relates to the technical field of asymmetric electrode ionic polymer-Metal Composites (Ionic Polymer-Metal Composites, IPMC), in particular to a preparation method of an asymmetric electrode IPMC and the prepared asymmetric electrode IPMC.
Background
The core technology of IPMC manufacturing process is to achieve efficient bonding of electrode and matrix film. Studies have shown that: only if electrode particles penetrate into the ionic membrane matrix to form a certain interface layer, the IPMC can exhibit excellent transduction function.
The method for preparing the IPMC material disclosed in the patent application number 201811220201.7 comprises the following steps: the roughening treatment of the base film occurs after the first ion exchange treatment of the base film and before the first reduction treatment of the base film. Also disclosed are a method for preparing an intermediate of the IPMC material, and an IPMC material prepared by the method for preparing the IPMC material. The method has the advantages of realizing the enhancement of the adhesive force between the electrode and the matrix film, increasing the depth of the permeated electrode and improving the morphology of the permeated electrode, thereby further improving the electrochemical performance and the electromechanical performance of the IPMC material.
In the preparation of IPMC materials in the prior art, in the soaking reduction method and the autocatalysis reduction method, an ionic polymer matrix membrane is soaked in an ionic complex solution (such as platinum, gold, palladium, silver and other ionic complexes), ion exchange is performed, and then a layer of electrode is deposited and permeated on the upper surface and the lower surface of the matrix membrane through chemical reduction, so that a composite material with a sandwich structure is formed.
However, with the expansion of application fields, the IPMC requirements on the electrode are not limited to the double-layer electrode, for example, a single-layer electrode type IPMC structure and a preparation process thereof are disclosed in patent application No. 201710058364.9, which is characterized in that: one surface of the matrix film layer is coated with a packaging layer, and the other surface is provided with an electrode layer, and the preparation process comprises the following steps: masking one surface of the substrate film layer with a masking material, and then plating the electrode material on the other surface of the substrate film layer. In addition, as in paper Wang Maolin, what is known as Qigong, etc., IPMC unidirectional bending is realized through an asymmetric electrode [ J ]. Manned spaceflight, 2017,23 (004): 541-545. An asymmetric electrode IPMC is disclosed, wherein one side electrode is covered by a mask method on the basis of IPMC with platinum electrodes coated on two sides, copper is plated on one side of the platinum electrode surface by an electroplating method, and an electrode layer is plated on two sides of a film or one side of the film is covered as required to prepare the electrode layer with one side.
However, the above prior art preparation method mainly combines a mask method or a laser cutting electrode method to realize two-side patterned electrodes, and the electrode plating method used by the method is still a traditional IPMC soaking reduction plating method. Thus, the interface of the two layers of electrodes and the membrane remains symmetrical. Aiming at the application requirement of a curled IPMC driver, the invention provides a novel IPMC preparation method, wherein a direct fusion method is used for replacing an ion exchange process in the traditional process, and the dissymmetry of electrode interfaces at two sides is realized by utilizing the density difference of electrode complex salt and matrix film solution. The IPMC material prepared by the method has excellent performance and simple preparation method, and the interface between the prepared IPMC electrode and the matrix film has obvious gradient distribution, so that the asymmetric electrode can be realized.
Disclosure of Invention
The technical problem to be solved by the invention is that the electrode layers are plated on the two sides of the membrane in the method in the prior art, one side of the membrane can be covered up only according to the requirement to prepare the electrode layer with a single side, the operation is complex, and the preparation method of the asymmetric electrode IPMC and the prepared asymmetric electrode IPMC are provided.
The invention solves the technical problems by the following technical means:
A preparation method of an asymmetric electrode IPMC comprises the following steps:
(1) Mixing a matrix film solution with an electrode material, and layering to obtain a film solution;
(2) Carrying out film casting treatment on the film solution obtained in the step (1) to obtain a matrix film;
(3) And (3) after the substrate film is subjected to reduction plating treatment, forming an electrode layer on the surface of the film, namely the asymmetric electrode IPMC.
The beneficial effects are that: the electrode material required by IPMC is doped into the matrix film solution to form a film, and then the electrode is formed on the surface of the film through chemical reduction plating, so that the asymmetric electrode IPMC can be designed, wherein the electrode material comprises different materials and the electrode is asymmetric in morphology. Therefore, the electrode structure with a specific structure is realized, the adhesive force between the electrode and the matrix film is enhanced, the depth of the permeated electrode is increased, the morphology of the permeated electrode is improved, and the electrochemical performance and the electromechanical performance of the IPMC material are further improved.
The asymmetric electrode IPMC prepared by the invention does not need to carry out mask design on one side of the membrane, can directly generate a single-side electrode on one side of the matrix membrane, and can carry out electrode design on the other side of the membrane according to the need. Compared with the prior art, the preparation process has remarkable innovation and effect improvement.
Preferably, the electrode material is selected from, but not limited to: one or more of the complex salts of Pd 2+、Ag+、Au+、Pt+、Ni+、Cu2+.
Preferably, the matrix film solution is selected from, but not limited to: a Nafion series ion exchange membrane solution from Dupont, an Aciplex series ion exchange membrane solution from ASAHI CHEMICAL, a Flemion series ion exchange membrane solution from ASAHI GLASS, or an Aquivion series ion exchange membrane solution from Solvay Solexis.
Preferably, the step (3) is performed with ion exchange treatment after the plating.
The beneficial effects are that: the ion exchange treatment changes the driving ions in the membrane into Na + or other ions, so that the hydrated cations in the membrane move under the action of an electric field to cause the IPMC to deform.
Preferably, the electrode material deposition surface of the base film after the casting film treatment of step (2) is roughened.
The beneficial effects are that: the formation of a transition layer between the base film and the electrode by roughening enhances the performance of the electrode.
Preferably, the roughening treatment comprises one of sand blasting, sanding, microneedle roughening, and plasma etching.
Preferably, a layer of conductive silver paste is printed on the electroless surface of the substrate film after electroplating, and then dried.
The beneficial effects are that: the asymmetric electrode IPMC in the present invention is provided with an electrode layer on one side, and may be provided with a different electrode layer on the other side of the film as needed.
Preferably, DMAC is added to the base film solution in a mass ratio of 3:1.
Preferably, the casting film treatment is carried out under vacuum condition, the treatment temperature is 90-120 ℃, and the treatment time is 15-30 h.
Preferably, the reduction treatment in the step (3) includes the steps of: mixing ultrapure water with ammonia water to prepare plating solution, adding NaBH 4 reducing solution under the oscillating condition, then adding the matrix film, and adding NaBH 4 reducing solution again after a period of time for treatment.
Preferably, the ultrapure water and the ammonia water are mixed according to the volume ratio of 300:1, 5wt% of NaBH 4 reducing solution is added under the oscillation condition at the temperature of 40-60 ℃, then the substrate film is put, 5wt% of NaBH 4 reducing solution is added once every 5-30 min, and the reduction reaction is carried out under the environment that the concentration of NaBH 4 is 0.05 g/L-1 g/L, and the total time is 2-4 h; the mass concentration of the ammonia water is 25-28%.
Preferably, the electroplating in the step (3) includes the steps of: and (3) placing the substrate film subjected to the reduction treatment in electrolyte for electroplating treatment.
Preferably, the cathode adopted by the electroplating is an array needle, the anode is a titanium net, and the current is 0.1-0.3A.
Preferably, the electrolyte is gold water.
Preferably, the mass ratio of the matrix film solution to the electrode material is 36-144:1.
An asymmetric electrode IPMC manufactured by the method.
The beneficial effects are that: the asymmetric electrode IPMC prepared by the invention has excellent electrochemical performance and electromechanical performance.
The invention has the advantages that: the electrode material required by IPMC is doped into the matrix film solution to form a film, and then the electrode is formed on the surface of the film through chemical reduction plating, so that the asymmetric electrode IPMC can be designed, wherein the electrode material comprises different materials and the electrode is asymmetric in morphology. Therefore, the electrode structure with a specific structure is realized, the adhesive force between the electrode and the matrix film is enhanced, the depth of the permeated electrode is increased, the morphology of the permeated electrode is improved, and the electrochemical performance and the electromechanical performance of the IPMC material are further improved.
Drawings
FIG. 1 is a schematic view of the process flow for preparing an IPMC material according to the present invention.
FIG. 2 is a block diagram of an IPMC in accordance with embodiment 1 of the present invention;
FIG. 3 is a block diagram of an IPMC in accordance with embodiment 3 of the present invention;
FIG. 4 is a graph showing the displacement performance under DC 5V excitation in example 1 of the present invention;
FIG. 5 is a graph showing the displacement performance under DC 5V excitation in example 2 of the present invention;
In the figure: 1 is a first electrode layer; 2 is a matrix film layer; and 3, a second electrode layer.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The test materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
Those of skill in the art, without any particular mention of the techniques or conditions, may follow the techniques or conditions described in the literature in this field or follow the product specifications.
Example 1
The embodiment discloses a preparation process of a single-sided electrode Pd-Au-IPMC material, wherein the preparation process is shown in a figure 1, one side of a matrix film layer 2 is a first electrode layer 1, the first electrode layer 1 contains metal electrodes Pd and Au, and an inner layer is a Pd electrode; the outer layer is an Au electrode as shown in fig. 2. The method specifically comprises the following steps:
(1) And (3) mixing: 24.48g Nafion D520 solution, 8.16g DMAC organic solvent and 169.95mg Pd (NH 3)4Cl2 palladium complex salt) were added to a beaker, and the mixture was stirred and mixed well at 50℃and 600r/min for a period of 5h.
(2) Standing the solution: pouring the mixed solution into a 61mm x 61mm x 40mm die, maintaining for 15min under vacuum, removing gas entrained in the solution, and layering, and precipitating or floating the ionic complex. In order to allow the electrode material to be added to be sufficiently dispersed in the diluted solution, it is then uniformly distributed at the bottom or surface of the solution under a standing condition.
(3) And (3) casting film treatment: and (3) putting the die containing the mixed solution into a vacuum drying oven, setting the temperature to 90 ℃, keeping the temperature for about 20 hours, and carrying out annealing treatment when the film is observed to be basically solidified, wherein the temperature is set to 120 ℃, and the annealing time is set to 2 hours.
(4) Ion reduction: measuring 186mL of DI water and 0.62mL of ammonia water (the content is 25% -28%) in a beaker to prepare a plating solution, adding 0.6mL of 5wt% of NaBH 4 reducing solution under the condition of a water bath constant temperature oscillator at 50 ℃ and 300r/min, putting the film cast in the step (3), and adding 0.6mL of 5wt% of NaBH 4 reducing solution once every 5min for 24 times, wherein the total time is 2h.
(5) Electroplating: and (3) trimming the film treated in the step (4), and carrying out gold plating treatment on the surface of the sample wafer under the action of current of 0.2A by taking 1.6g/L of gold water (100 mL) as electrolyte and selecting an array needle as a sound pole and a titanium mesh as an anode.
(6) Ion exchange: and (3) placing the film electroplated in the step (5) into a 0.2mol/L NaOH solution, and exchanging for 2 hours in a magnetic stirrer with the temperature of 50 ℃ and the speed of 300r/min to convert driving ions in the film into Na +.
FIG. 4 is a graph showing the displacement curve of example 1 at a DC 5V voltage. The electromechanical properties of the samples were analyzed mainly by measuring the end displacement of the samples with cantilever beam structures. Cutting the sample into strips with the size of 35mm x 5mm, clamping a position 5mm away from the tail end of the sample piece by a copper clamp, connecting one side with an electrode layer with the positive electrode, and connecting the other free end with the length of 30mm. The direct current 5V excitation voltage is output through the digital source meter, the IPMC material generates deformation of different degrees after receiving corresponding electric signals, the laser displacement sensor can accurately detect the deformation displacement value of the sample wafer, the displacement signal is collected through matched software, and finally the collected displacement information is processed and analyzed.
The measurement result shows that the sample piece generates displacement deformation of maximum 1.103mm under the direct current 5V voltage.
Example 2
The embodiment discloses a preparation process of a single-sided electrode Pd-Au-IPMC material, which specifically comprises the following steps:
(1) And (3) mixing: 24.48g Nafion D520 solution, 8.16g DMAC organic solvent and 169.95mg Pd (NH 3)4Cl2 palladium complex salt) were added to a beaker and mixed with stirring thoroughly at 50℃and 600r/min for 5h.
(2) Standing the solution: pouring the mixed solution into a 61mm x 61mm x 40mm die, maintaining for 15min under vacuum, removing gas entrained in the solution, standing the die on a horizontal position for 6h, and fully precipitating Pd (NH 3)4Cl2 palladium complex salt) at the bottom of the solution.
(3) And (3) casting film treatment: and (3) putting the die containing the mixed solution into a vacuum drying oven, setting the temperature to 90 ℃, keeping the temperature for about 20 hours, and carrying out annealing treatment when the film is observed to be basically solidified, wherein the temperature is set to 120 ℃, and the annealing time is set to 2 hours.
(4) Roughening treatment: the Pd (NH 3)4Cl2 palladium complex salt deposition surface of the film was roughened with a microneedle roller, the four edges of the base film were held in place by tape, and the surface of the base film was roughened back and forth for 100 cycles.
(5) Ion reduction: measuring 186mL of DI water and 0.62mL of ammonia water (the content is 25% -28%) in a beaker to prepare a plating solution, adding 1.2mL of 5wt% of NaBH 4 reducing solution under the condition of a water bath constant temperature oscillator at 50 ℃ and 300r/min, putting the film cast in the step (3), and adding 1.2mL of 5wt% of NaBH 4 reducing solution every 10min for 12 times, wherein the total time is 2h.
(6) Electroplating: and (3) trimming the film treated in the step (4), and carrying out gold plating treatment on the surface of the sample wafer under the action of current of 0.2A by taking 1.6g/L of gold water (100 mL) as electrolyte and selecting an array needle as a sound pole and a titanium mesh as an anode.
(7) Ion exchange: and (3) placing the film electroplated in the step (5) into a 0.2mol/L NaOH solution, and exchanging for 2 hours in a magnetic stirrer with the temperature of 50 ℃ and the speed of 300r/min to convert driving ions in the film into Na +.
FIG. 5 is a graph showing the displacement curve of example 2 at a DC 5V voltage. The electromechanical properties of the samples were analyzed mainly by measuring the end displacement of the samples with cantilever beam structures. Cutting the sample into strips with the size of 35mm x 5mm, clamping a position 5mm away from the tail end of the sample piece by a copper clamp, connecting one side with an electrode layer with the positive electrode, and connecting the other free end with the length of 30mm. The direct current 5V excitation voltage is output through the digital source meter, the IPMC material generates deformation of different degrees after receiving corresponding electric signals, the laser displacement sensor can accurately detect the deformation displacement value of the sample wafer, the displacement signal is collected through matched software, and finally the collected displacement information is processed and analyzed.
The measurement result shows that the sample piece generates maximum displacement deformation of 2.034mm under the direct current 5V voltage.
Example 3
The embodiment discloses a preparation process of an asymmetric electrode Pd-Au-Ag-IPMC material, as shown in FIG. 3, one side of a substrate film layer 2 is a first electrode layer 1 containing metal electrodes Pd and Au, wherein an inner layer (close to the substrate film layer 2) is a Pd electrode; the outer layer is an Au electrode; the other surface of the substrate film layer 2 is a second electrode layer 3 containing a metal electrode Ag. The method specifically comprises the following steps:
(1) And (3) mixing: 24.48g Nafion D520 solution, 8.16g DMAC organic solvent and 169.95mg Pd (NH 3)4Cl2 palladium complex salt) were added to a beaker and mixed with stirring thoroughly at 50℃and 600r/min for 5h.
(2) Standing the solution: pouring the mixed solution into a 61mm x 61mm x 40mm die and keeping the die under vacuum for 15min, and removing gas entrained in the solution.
(3) And (3) casting film treatment: and (3) putting the die containing the mixed solution into a vacuum drying oven, setting the temperature to 90 ℃, keeping the temperature for about 20 hours, and carrying out annealing treatment when the film is observed to be basically solidified, wherein the temperature is set to 120 ℃, and the annealing time is set to 2 hours.
(4) Ion reduction: measuring 186mL of DI water and 0.62mL of ammonia water (the content is 25% -28%) in a beaker to prepare a plating solution, adding 0.6mL of 5wt% of NaBH 4 reducing solution under the condition of a water bath constant temperature oscillator at 50 ℃ and 300r/min, putting the film cast in the step (3), and adding 0.6mL of 5wt% of NaBH 4 reducing solution once every 5min for 24 times, wherein the total time is 2h.
(5) Electroplating: and (3) trimming the film treated in the step (4), and carrying out gold plating treatment on the surface of the sample wafer under the action of current of 0.2A by taking 1.6g/L of gold water (100 mL) as electrolyte and selecting an array needle as a sound pole and a titanium mesh as an anode.
(6) Electrode coating: printing a layer of conductive silver paste on the electrode-free surface of the film, and drying for 4 hours at 40 ℃ on a drying and heating table.
(7) Ion exchange: and (3) placing the film electroplated in the step (5) into a 0.2mol/L NaOH solution, and exchanging for 2 hours in a magnetic stirrer with the temperature of 50 ℃ and the speed of 300r/min to convert driving ions in the film into Na +.
The technical core of the invention is that the electrode material required by IPMC is firstly put forward to be doped into a matrix film solution for film formation, then the electrode is formed on the surface of the film through chemical reduction plating, and thus, the asymmetric electrode IPMC can be designed, including the electrode with different materials and asymmetric morphology. Therefore, the electrode structure with a specific structure is realized, the adhesive force between the electrode and the matrix film is enhanced, the depth of the permeated electrode is increased, the morphology of the permeated electrode is improved, and the electrochemical performance and the electromechanical performance of the IPMC material are further improved.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims (8)

1. A preparation method of an asymmetric electrode IPMC is characterized in that: the method comprises the following steps:
(1) Mixing a matrix film solution with an electrode material, standing the mixed solution under vacuum, and layering to obtain a film solution;
(2) Carrying out film casting treatment on the film solution obtained in the step (1) to obtain a matrix film;
(3) After the substrate film is subjected to reduction plating treatment, an electrode layer is formed on the surface of the film, namely an asymmetric electrode IPMC;
The electrode material comprises one or more of the complex salts of Pd 2+、Ag+、Au+、Pt+、Ni+、Cu2+;
The matrix membrane solution comprises Nafion series ion exchange membrane solution of Dupont company, aciplex series ion exchange membrane solution of ASAHI CHEMICAL company, flemion series ion exchange membrane solution of ASAHI GLASS company or Aquivion series ion exchange membrane solution of Solvay Solexis company.
2. The method for manufacturing an asymmetric electrode IPMC according to claim 1, wherein: and (3) roughening the electrode material deposition surface of the substrate film after the film casting treatment in the step (2).
3. The method for manufacturing an asymmetric electrode IPMC according to claim 1, wherein: and (3) performing ion exchange treatment after electroplating in the step (3).
4. The method for manufacturing an asymmetric electrode IPMC according to claim 1, wherein: printing a layer of conductive silver paste on the electrode-free surface of the electroplated substrate film, and then drying.
5. The method for manufacturing an asymmetric electrode IPMC according to claim 1, wherein: the reduction treatment in the step (3) comprises the following steps: mixing ultrapure water with ammonia water to prepare plating solution, adding NaBH 4 reducing solution under the oscillating condition, then adding the matrix film, and adding NaBH 4 reducing solution again after a period of time for treatment.
6. The method for manufacturing an asymmetric electrode IPMC according to claim 1, wherein: the electroplating in the step (3) comprises the following steps: and (3) placing the substrate film subjected to the reduction treatment in electrolyte for electroplating treatment.
7. The method for manufacturing an asymmetric electrode IPMC according to claim 6, wherein: the electrolyte is gold water.
8. Asymmetric electrode IPMC manufactured by the method of any one of claims 1-7.
CN202110913560.6A 2021-08-10 2021-08-10 Preparation method of asymmetric electrode IPMC and prepared asymmetric electrode IPMC Active CN113644192B (en)

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