CN109767861B - Preparation method of planar electrode and planar electrode - Google Patents
Preparation method of planar electrode and planar electrode Download PDFInfo
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- CN109767861B CN109767861B CN201910032227.7A CN201910032227A CN109767861B CN 109767861 B CN109767861 B CN 109767861B CN 201910032227 A CN201910032227 A CN 201910032227A CN 109767861 B CN109767861 B CN 109767861B
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Abstract
The embodiment of the invention provides a preparation method of a planar electrode and the planar electrode, wherein the preparation method comprises the following steps: depositing a metal layer on the surface of the porous filter membrane; and depositing a layer of active material on the porous filter membrane coated with the metal layer by using a spray type suction filtration mode to form the planar electrode. By utilizing the embodiment of the invention, the film after suction filtration is not required to be moved and combined with the conductive layer, the conductive substrate can be directly obtained, and the use is more convenient and quicker.
Description
Technical Field
The embodiment of the invention relates to the technical field of micromachining and electrochemistry, in particular to a preparation method of a planar electrode and the planar electrode.
Background
Micro electrochemical devices, such as micro supercapacitors, micro electrochemical sensors, micro ion batteries, etc., often employ planar interdigitated structures to increase the thickness of the electrodes and reduce the diffusion distance of ions between the electrodes. Typically the electrodes of such devices comprise a substrate layer, a current collector layer and an active layer: the substrate layer is often composed of an insulating material such as silicon oxide or a polymer film; the current collecting layer is usually made of noble metal materials with good conductivity and chemical inertness, such as gold/platinum and the like; the most advanced of the active materials at present are various kinds of nano materials having a nano structure. A molding process in which an active material and a current collector layer are deposited on a substrate layer and patterned to produce a device, a so-called micro-planar device. Common microdevice formation methods currently used in the field of micromachining include spin coating/spray coating/laser direct writing/chemical vapor deposition/physical vapor deposition, and the like. On one hand, the processing method has extremely high requirements on active materials, such as spin coating/spray coating has high requirements on the viscosity and uniformity of the materials, laser direct writing is limited to graphene materials, chemical vapor deposition and physical vapor deposition are limited to only a few semiconductor process materials, on the other hand, the formed active material layer is often not compact enough, a relatively fluffy structure is formed inside the active material layer, and the contact between the active material layer and the conductive current collecting layer is not tight enough, so that the processing method can enable a device to have large contact resistance.
Conventionally, a liquid solution is filtered on a porous filter membrane substrate by using a filtering device, and then the filtered membrane is combined with a conductive layer by using a direct carbonization or a mode of removing and transferring. The film formation by suction filtration is often limited on a porous fiber substrate, and the transfer process can cause insufficient contact strength on one hand, and on the other hand, because the shape of the film formation by suction filtration is similar to that of the porous fiber substrate and has the characteristic of fluctuation, the contact area between the film formation by suction filtration and the conventional planar conductive substrate is reduced, and how to directly and rapidly form the film in one step becomes the problem which needs to be solved urgently.
Disclosure of Invention
Aiming at the technical problems in the prior art, the embodiment of the invention provides a preparation method of a planar electrode and the planar electrode.
In a first aspect, an embodiment of the present invention provides a method for preparing a planar electrode, including: depositing a metal layer on the surface of the porous filter membrane;
and depositing a layer of active material on the porous filter membrane coated with the metal layer by using a spray type suction filtration mode to form the planar electrode.
In a second aspect, an embodiment of the present invention provides a planar electrode, including: the electrode prepared by the preparation method of the planar electrode is included.
The preparation method of the planar electrode and the planar electrode provided by the embodiment of the invention deposit a metal layer on the surface of the porous filter membrane; and depositing a layer of active material on the porous filter membrane coated with the metal layer by using a spray type suction filtration mode to form the planar electrode. By utilizing the embodiment of the invention, the membrane after suction filtration is not required to be moved to be combined with the conductive layer, the conductive substrate can be directly obtained, and the use is more convenient and quicker.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and those skilled in the art can also obtain other drawings according to the drawings without creative efforts.
Fig. 1 is a schematic flow chart of a method for manufacturing a planar electrode according to an embodiment of the present invention;
fig. 2 is a process flow of directly forming a flexible planar interdigital device on a porous conductive substrate according to an embodiment of the present invention;
FIG. 3a is a cross-sectional view of a porous substrate having a conductive gold layer deposited thereon according to an embodiment of the present invention;
FIG. 3b is a cross-sectional view of an original porous substrate without a deposited conductive layer;
FIG. 3c is an enlarged cross-sectional view of a porous substrate having a conductive gold layer deposited thereon according to an embodiment of the present invention;
FIG. 3d is a perspective cross-sectional view of a porous substrate having a conductive gold layer deposited thereon according to an embodiment of the present invention;
FIG. 4a is a cross-sectional view of a planar electrode provided in accordance with an embodiment of the present invention;
FIG. 4b is a cross-sectional view of a planar electrode provided in accordance with an embodiment of the present invention;
fig. 5 is a schematic view showing that the planar electrode provided by the embodiment of the present invention is not mechanically damaged in a bent state.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Fig. 1 is a schematic flow chart of a method for manufacturing a planar electrode according to an embodiment of the present invention, as shown in fig. 1, the method includes:
s101, depositing a metal layer on the surface of the porous filter membrane;
s102, depositing a layer of active material on the porous filter membrane coated with the metal layer by using a spray type suction filtration mode to form the planar electrode.
The embodiment of the invention provides a preparation method of a planar electrode, which is characterized in that a layer of nano metal particles is deposited on a fiber porous filter membrane with the pore diameter larger than 0.2 micrometer to form a conductive structure. As the size distribution of the metal particles is 30-50 nm, the nano-pores of the porous filter membrane can not be blocked, so that the filter membrane has excellent conductivity and can still be used for the suction filtration process. Whether the filter is plasma treated or not can then be determined based on the hydrophilicity or hydrophobicity of the active material to be deposited.
And (3) realizing suction filtration and deposition of the electrode active material on the conductive substrate of the deposited metal layer. The filter membrane on which the conductive layer is deposited is placed in a vacuum filtration apparatus while an unlimited variety of electrode active materials are uniformly dispersed in a corresponding solution, and then charged into a commercial atomizer. And starting the suction filtration equipment, and uniformly spraying the active material on the filter membrane of the conductive layer by using a sprayer, so that the active material can be suction-filtered on the conductive substrate to obtain the planar electrode. In this process, the purpose of the spraying device is to prevent lateral diffusion of the active material solution in the filter membrane to avoid electrode shorting. The thickness of the active material is determined by the concentration of the solution and the suction filtration time.
The preparation method of the planar electrode provided by the embodiment of the invention is characterized in that a metal layer is deposited on the surface of the porous filter membrane; and depositing a layer of active material on the porous filter membrane coated with the metal layer by using a spray type suction filtration mode to form the planar electrode. By utilizing the embodiment of the invention, the membrane after suction filtration is not required to be moved to be combined with the conductive layer, the conductive substrate can be directly obtained, and the use is more convenient and quicker.
Optionally, sputtering a metal layer on the surface of the porous filter membrane specifically includes:
and depositing a metal particle layer on the fiber porous filter membrane by using a sputtering or evaporation method to form a conductive structure.
On the basis of the embodiment, the metal particles are deposited on the fiber porous filter membrane in a sputtering or evaporation mode, and the thickness of the metal particles can be selected from 30-200 nanometers, so that a conductive structure is formed.
Optionally, the depositing a metal particle layer on the fiber porous filter membrane by using a sputtering or evaporation method to form a conductive structure further includes:
and fixing a metal mask plate with patterns to be tightly attached to the fiber porous filter membrane, and depositing a metal particle layer by using a sputtering or evaporation method to form the conductive structure with the mask plate patterns.
On the basis of the embodiment, before the metal layer is deposited on the fiber porous filter membrane, a metal mask plate with a pattern is attached to the filter membrane, and after the mask plate is fixed, a metal particle layer is deposited by adopting a sputtering or evaporation method, so that a conductive structure with a mask plate pattern is formed. A
Optionally, the pattern of the metal mask plate is an interdigitated and hollowed pattern.
On the basis of the above embodiment, preferably, the pattern and the size of the metal mask plate can be set according to needs, and in the embodiment of the present invention, preferably, the pattern of the metal mask plate is an interdigital structure and is in a hollow state.
Optionally, the metal mask plate with the pattern is fixed and closely attached to the fiber porous filter membrane, and specifically comprises:
and closely attaching a hollow metal mask plate with an interdigital structure to the fiber porous filter membrane by using a PI adhesive tape.
On the basis of the above embodiment, a mask plate is fixed on the fiber porous filter membrane with the pore diameter larger than 0.2 μm, and PI tape or other tapes or adhesive rods can be used as long as the fiber porous filter membrane can be tightly attached to the filter plate, which is not specifically limited in the embodiment of the present invention.
Optionally, a layer of active material is deposited on the porous filter membrane coated with the metal layer by using a spray suction filtration manner to form the planar electrode, specifically:
after the active material solution is subjected to ultrasonic treatment, the active material solution is placed into an atomizer;
placing the porous filter membrane coated with the metal layer and provided with the mask plate on a vacuum filtration device, and spraying the active material solution on the porous filter membrane by adopting the atomizer and the vacuum filtration device;
and removing and drying the sprayed porous filter membrane to form the planar electrode with the mask plate pattern.
On the basis of the embodiment, the suction filtration and deposition of the electrode active material are realized on the deposited interdigital conductive substrate by means of an unreleased mask. The filter membrane attached with the mask plate and the conductive layer deposited is placed in vacuum filtration equipment, meanwhile, electrode active materials of unlimited types are uniformly dispersed in corresponding solution, and then the solution is filled into a commercial sprayer.
And starting the suction filtration equipment, and uniformly spraying the active material on the hollowed-out area of the mask plate by using a sprayer, so that the active material can be suction-filtered on the conductive substrate and keeps an interdigital structure. In this process, the purpose of the spraying device is to prevent lateral diffusion of the active material solution in the filter membrane to avoid electrode shorting. The thickness of the active material is determined by the concentration of the solution and the suction filtration time.
And after the deposition of the active material is finished, the filter membrane is moved out of the vacuum filtration equipment, natural drying is carried out at normal temperature, then the adhesive tape is removed, and the mask plate is taken down, so that the planar electrode can be obtained.
Optionally, the active material solution is a mixed solution of metal alkene and carbon nanotubes.
Optionally, the metal layer is gold, platinum or chromium.
In addition to the above embodiments, the metal layer deposited on the filter membrane may be an inert metal such as gold, platinum or chromium.
The planar electrode obtained by the preparation method of the planar electrode provided by the embodiment of the invention has a shape structure almost the same as the hollow part of the mask, and short circuit between the electrodes can not occur. The active material and the conductive current collector layer form a conformal and tight attachment, and the contact resistance is tested to be less than 1 ohm. The active material itself will have a very high bulk density, and especially when using two-dimensional nanomaterials as active materials, very compact and regular nanostructures can be produced.
Optionally, the fibrous porous filter membrane is Nylon, PVDF, PTFE.
Based on the above embodiments, the fiber porous filter membrane can be Nylon, PVDF, PTFE, but not limited to these, and different types of filter membranes correspond to different types of electrolytes.
Fig. 2 is a processing and manufacturing flow of directly forming a flexible planar interdigital device on a porous conductive substrate according to an embodiment of the present invention, and the specific method is as follows:
1) preparing a porous filter membrane with the pore diameter of more than 0.2 micron, and tightly adhering the filter membrane on a silicon wafer (or other planar materials) by using a PI adhesive tape (or other adhesive tapes or adhesive sticks);
2) adhering the metal mask plate to the surface of the filter membrane by using a PI adhesive tape (or other adhesive tapes or adhesive bars);
3) sputtering a gold layer with the thickness of 100 nanometers on the filter membrane together with the silicon chip substrate;
4) using oxygen plasma for five minutes to make the gold layer have better hydrophilicity;
5) the active material solution (a mixed solution of metal alkene and carbon nanotube used in this example) was sonicated for 2 hours, albeit in a commercial atomizer;
6) placing the filter membrane adhered with the mask plate on a vacuum filtration device, starting the filtration device, and spraying an active material in an opening area of the mask plate, wherein the spraying time is determined according to the required thickness of an electrode;
7) and (3) turning off the vacuum filtration device and the atomizer, removing the filter membrane, naturally drying, and then removing the mask plate to obtain the planar interdigital structure electrode.
FIG. 3a is a cross-sectional view of a porous substrate having a conductive gold layer deposited thereon according to an embodiment of the present invention; fig. 3b is a cross-sectional view of an original porous substrate without a deposited conductive layer. By comparing fig. 3a-3b, it can be seen that the gold layer is uniformly and conformally deposited on the fibers, forming a connected conductive network, while not blocking the pores of the filter membrane, and fig. 3c and 3d are an enlarged view and a perspective view, respectively, of the deposited conductive layer.
As can be confirmed by fig. 4a and 4b, the active material layer, the conductive current collecting layer, and the substrate layer are closely attached to each other. As can be seen from fig. 4b, when a two-dimensional material is used as the active material, the obtained active material layer has a very compact structure.
The embodiment of the present invention further provides a planar electrode, which is prepared by using the above method for preparing a planar electrode, as shown in fig. 5, and a schematic diagram of the planar electrode provided in the embodiment of the present invention shown in fig. 5 that is not mechanically damaged in a bent state is clearly shown. The prepared planar electrode has good flexibility, and particularly shows that the electrochemical performance of the planar electrode can not be obviously attenuated when the planar electrode is bent to 180 degrees.
The above-described embodiments of the apparatus are merely illustrative, and the units described as separate parts may or may not be physically separate, and parts displayed as units may or may not be physical units, may be located in one place, or may be distributed on a plurality of network units. Some or all of the modules may be selected according to actual needs to achieve the purpose of the solution of the present embodiment. One of ordinary skill in the art can understand and implement it without inventive effort.
Through the above description of the embodiments, those skilled in the art will clearly understand that each embodiment can be implemented by software plus a necessary general hardware platform, and certainly can also be implemented by hardware. With this understanding in mind, the above-described technical solutions may be embodied in the form of a software product, which can be stored in a computer-readable storage medium such as ROM/RAM, magnetic disk, optical disk, etc., and includes instructions for causing a computer device (which may be a personal computer, a server, or a network device, etc.) to execute the methods described in the embodiments or some parts of the embodiments.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present 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 solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (5)
1. A method of making a planar electrode, comprising:
fixing a metal mask plate with patterns to be tightly attached to the fiber porous filter membrane, and depositing a metal particle layer by using a sputtering or evaporation method to form a conductive mechanism with the mask plate patterns, wherein the metal particles are nano metal particles;
depositing a layer of active material on the porous filter membrane coated with the metal layer by using a spray type suction filtration mode to form the planar electrode;
the pattern of the metal mask plate is an interdigital structure and hollow pattern;
the method comprises the following steps of depositing a layer of active material on a porous filter membrane coated with a metal layer by using a spray type suction filtration mode to form the planar electrode, wherein the spray type suction filtration mode specifically comprises the following steps:
after the active material solution is subjected to ultrasonic treatment, the active material solution is placed into an atomizer;
placing the porous filter membrane coated with the metal layer and provided with the mask plate on a vacuum filtration device, and spraying the active material solution on the porous filter membrane by adopting the atomizer and the vacuum filtration device;
removing and drying the sprayed porous filter membrane to form a planar electrode with a mask plate pattern;
the fiber porous filter membrane is made of Nylon, PVDF and PTFE.
2. The preparation method according to claim 1, wherein the metal mask plate with patterns is fixed and tightly attached to the fiber porous filter membrane, and specifically comprises:
and closely attaching a hollow metal mask plate with an interdigital structure to the fiber porous filter membrane by using a PI adhesive tape.
3. The production method according to claim 1, wherein the active material solution is a mixed solution of a metal alkene and a carbon nanotube.
4. The method of claim 1, wherein the metal layer is gold, platinum, or chromium.
5. A planar electrode, comprising a planar electrode produced by the method for producing a planar electrode according to any one of claims 1 to 3.
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| CN104396067B (en) * | 2012-07-13 | 2018-07-13 | 古河电气工业株式会社 | Collector foil, electrode assembly, lithium secondary battery or double layer capacitor |
| CN106910897A (en) * | 2017-03-02 | 2017-06-30 | 宁德时代新能源科技股份有限公司 | Current collector, pole piece thereof and battery |
| CN108641482A (en) * | 2018-05-28 | 2018-10-12 | 中国科学技术大学 | A kind of high-performance can ink-jet ink and preparation method thereof and the application in flexible all-solid-state supercapacitor |
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| CN1577916A (en) * | 2003-07-02 | 2005-02-09 | 三星Sdi株式会社 | Microporous film containing nano particles and its forming method, and fuel cell containing the same |
| CN102568865A (en) * | 2012-02-22 | 2012-07-11 | 华中科技大学 | Preparation method of flexible super capacitor based on paper and application thereof |
| CN103021663A (en) * | 2012-12-20 | 2013-04-03 | 同济大学 | Novel method for preparing counter electrode material of carbon nanotube thin-film solar cell |
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