CN114512279B - Preparation method of double-fold metal film stretching electrode - Google Patents
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Abstract
A preparation method of a double-fold film electrode comprises the steps of preparing an original substrate by taking sand paper as a template through spin coating, depositing a metal layer on the surface of the original substrate through magnetron sputtering, preparing a WPU film on the outermost surface, and finally stripping the WPU film with the metal layer from the surface of the original substrate, wherein the original substrate is made of Ecoflex platinum silica gel or SEBS thermoplastic elastomer. The metal film electrode prepared by the invention has a double fold structure, is suitable for stretching deformation in different directions and dimensions, has stable resistance without change under the same stretching rate in different directions, and has the resistance change rate of 13.7 when being stretched by 50%, and the stretching rate can reach more than 100%. As an electrode material, it has a small resistance change and a high stability with an increase in tensile deformation.
Description
Technical Field
The invention relates to the technical field of stretching electrode preparation, in particular to a preparation method of a double-fold metal film stretching electrode.
Background
As an emerging promising field of research, flexible electronic products have raised a concern about how to manufacture high performance flexible electronic materials that are durable under high stress conditions. The traditional flexible electrode is fragile, and can break under a small strain, so that the requirement of the wearable flexible electronic product on mechanical flexibility in the future can not be met. The flexible electrode applied to the elastic substrate mainly undergoes four deformation modes of bending, folding, twisting and stretching, and stretching is a mode in which stress strain is the greatest on the material. Flexible electrodes with high tensile properties can also withstand bending, folding and twisting. The rapid issuing of the stretchable electrode promotes the product fields of wearable electronic products, electronic skin, implanted medical electronic equipment, soft robots, novel flexible human-computer interfaces and the like.
In recent years, the great demand for flexible conductive materials has led to extensive research into several classes of nanomaterials. Such as Carbon Nanotubes (CNTs), graphene, metal nanowires, organic polymer thin films, and composites thereof. Among them, graphene, as a monoatomic layer two-dimensional (2D) material with excellent mechanical and electrical properties, has shown great potential in the field of flexible electronic devices, and is one of candidate materials for flexible electrodes. Another widely used FTEs film material is poly (3, 4-ethylenedioxythiophene) polystyrene sulfonate (PEDOT: PSS), which also has excellent sheet resistance and stretchability, is widely used in Polymer Light Emitting Diodes (PLEDs), organic solar cells, organic transistors, and supercapacitors. However, the relatively low conductivity of graphene and PEDOT: PSS thin film materials limits their further application in high performance optoelectronic devices. The metal electrode has excellent conductivity but does not have flexibility itself, and a certain flexibility can be obtained by thickness reduction but stretching cannot be performed. In the prior art, a metal layer is prepared on the surface of a pre-stretched elastic matrix by a pre-stretching elastomer technology, so that the metal layer forms a fold structure, and therefore, the metal film prepared by the method has certain stretching performance, but the metal film prepared by the method can only carry out stretching strain in a single direction, can not realize uniform stretching deformation in all directions, and has orientation; and the single-layer fold structure has larger resistance change and poorer stability along with the increase of the stretching rate.
Disclosure of Invention
The invention aims to provide a preparation method of a double-fold film stretching electrode. The double unoriented fold structure can achieve uniform deformation of the electrode material in all directions, and maintains excellent conductivity.
The invention aims at realizing the following technical scheme:
a preparation method of a double-fold membrane electrode is characterized by comprising the following steps: preparing an original substrate by taking sand paper as a template, depositing a metal layer on the surface of the original substrate by magnetron sputtering, preparing a WPU film on the outermost surface, and finally stripping the WPU film with the metal layer from the surface of the original substrate, wherein the original substrate is made of Ecoflex platinum silica gel or SEBS thermoplastic elastomer.
Further, the deposited metal layer is a Cu layer, a Mn layer or an Au layer.
Further, the magnetron sputtering is performed with an evacuation degree of 10 -3 ～10 -2 Pa, ar is introduced to adjust the air pressure to be 3Pa, the current is 10-25 mA, the voltage is 250-300V, the sputtering power is 20-40W, and the sputtering time is 110-160 s.
In the process of preparing the film, the method for depositing the film by magnetron sputtering is found to generate local uneven heat in the process of depositing metal film layers such as Cu, mn, au and the like on the surface of a substrate, so that the specific metal film generates non-directional shrinkage, thereby forming an irregular fold structure in each direction, and the fold structure can generate corresponding strain without structural fracture when the metal layer is stretched under the action of external forces in different directions.
Further preferably, the metal layer is an Au layer, the magnetron sputtering current is 20mA, the voltage is 260V, the sputtering power is 22.5W, and the sputtering time is 150s.
Further, the original substrate is prepared by spin coating Ecoflex platinum silica gel or SEBS thermoplastic elastomer on the surface of sand paper with the mesh number of 60-600, the spin coating speed is 5000-6000 rpm, and the spin coating time is 10-20 s.
Before the magnetron sputtering metal layer is adopted, sand paper with certain roughness is used as a template to prepare an original substrate, the original substrate is subjected to the repeated etching of the sand paper to form a certain fold structure, the surface metal layer is subjected to the repeated etching of the fold structure of the original substrate in the process of the magnetron sputtering metal layer, an unoriented secondary fold structure is formed on the surface of the surface metal layer, uneven local heat in the magnetron sputtering process is regulated and controlled by concave-convex folds on the original substrate, the secondary folds on the surface of the metal layer are promoted to be further deepened, and accordingly the metal layer is suitable for a larger tensile strain range and has smaller resistance change.
The A and the B in the Ecoflex platinum silica gel are mixed according to the mass ratio of 1:1.
The SEBS (polystyrene-polyethylene-polybutene-polystyrene) elastomer is dissolved in a mixture consisting of hexane and cyclohexane in any ratio, toluene or tetrahydrofuran, and the prepared solution with the mass percentage concentration of 8-15% is subjected to spin coating.
Further preferably, when Ecoflex platinum silica gel is spin-coated, the spin-coating rate is 5500-6000 rpm, the spin-coating time is 10-20 s, and the curing is performed at room temperature for 3-12 h after the spin-coating is completed.
It is further preferred that when spin coating the SEBS thermoplastic elastomer, the spin coating rate is 5000-5800 rpm, the spin coating time is 10-15 s, and the temperature is kept at 60-80 ℃ for 5-20 min.
Further, after the metal layer is deposited, WPU solution with the concentration of 18 to 25 percent is mixed with the metal layer at the concentration of 320 to 380 mu L/cm 2 Dripping onto the surface of the metal layer, naturally drying at room temperature, and then peeling the WPU film with the metal layer from the original substrate surface.
The WPU is an aqueous polyurethane elastomer.
After the original substrate is subjected to rough surface structure of the re-engraved abrasive paper, as the metal thin layer forms secondary folds under magnetron sputtering, an obvious gap structure is formed between the metal film layer and the original substrate, so that the interface bonding force of the metal film layer and the original substrate is extremely poor, and the metal layer can be directly used and can fall off from the surface of the original substrate.
The preparation method of the double-fold electrode film is characterized by comprising the following steps of:
step 1: the method comprises the steps of spin-coating Ecoflex platinum silica gel or an SEBS thermoplastic elastomer on the surface of sand paper with the mesh number of 60-600, wherein when the Ecoflex platinum silica gel is spin-coated, the spin-coating speed is 5500-6000 rpm, the spin-coating time is 10-20 s, then the solid is cured for 3-12 h at room temperature, when the SEBS is spin-coated, the mass percentage concentration of the SEBS is 8-15%, the spin-coating speed is 5000-5800 rpm, the spin-coating time is 10-15 s, and after the spin-coating is finished, the solid is heated to 60-80 ℃, and the heat is preserved for 5-20 min, so that an original substrate is formed;
step 2: performing magnetron sputtering to deposit a metal layer on the surface of the original substrate, wherein the metal layer is a Cu layer, a Mn layer or an Au layer, and the vacuum degree is 10 during deposition -3 ～10 -2 Pa, introducing Ar to adjust the air pressure to be3Pa, the current is 10-25 mA, the voltage is 250-300V, the sputtering power is 20-40W, and the sputtering time is 110-160 s;
step 3: after the metal layer is deposited, WPU solution with the concentration of 18-25% is mixed with the solution at the concentration of 320-380 mu L/cm 2 Dripping onto the surface of the metal layer, naturally drying at room temperature, and then peeling the WPU film with the metal layer from the original substrate surface.
The invention has the following technical effects:
the metal film electrode prepared by the invention has a double fold structure, is suitable for stretching deformation in different directions and dimensions, has stable resistance without change under the same stretching rate in different directions, and has the resistance change rate of 13.7 when being stretched by 50%, and the stretching rate can reach more than 100%. As an electrode material, it has a small resistance change and a high stability with an increase in tensile deformation.
Drawings
Fig. 1: single fold and double fold comparison schematic in the present invention.
Fig. 2: in the invention, the Ecoflex platinum silica gel is adopted as an original substrate material to prepare the double-fold membrane electrode flow chart.
Fig. 3: the invention provides a microscopic scanning electron microscope image of a double-fold film electrode.
Fig. 4: the double-fold film electrode prepared by the invention has resistance change under different stretching ratios.
Detailed Description
The present invention is described in detail below by way of examples, which are necessary to be pointed out herein for further illustration of the invention and are not to be construed as limiting the scope of the invention, since numerous insubstantial modifications and adaptations of the invention will be to those skilled in the art in light of the foregoing disclosure.
Example 1
The preparation method of the double-fold electrode film comprises the following steps:
step 1: the method comprises the steps of spin-coating Ecoflex platinum silica gel on the surface of sand paper with the mesh number of 200, wherein the spin-coating speed is 6000rpm, the spin-coating time is 10s, then curing for 8h at room temperature to form an original substrate, and mixing A and B in the Ecoflex platinum silica gel according to the mass ratio of 1:1;
step 2: performing magnetron sputtering to deposit a Cu metal layer on the surface of the original substrate, wherein the vacuum degree is 10 during deposition -2 Pa, ar is introduced to adjust the air pressure to be 3Pa, the current is 10mA, the voltage is 300V, the sputtering power is 40W, and the sputtering time is 110s;
step 3: after deposition of the Cu metal layer, a WPU solution with a mass concentration of 25% was applied at 320. Mu.L/cm 2 Dripping onto the surface of the metal layer, naturally drying at room temperature, and then stripping the WPU film with the Cu metal layer from the original substrate surface.
The Cu metal electrode prepared by the embodiment and taking the WPU as the substrate has consistent surface resistance change and stable performance after being stretched at different angles. The metal electrode prepared by the invention has no orientation in the stretching dimension, and can achieve uniform stretching in all directions. The resistance change of the electrode is stable in the stretching deformation process.
Example 2
The preparation method of the double-fold electrode film comprises the following steps:
step 1: the method comprises the steps of heating SEBS solution on the surface of sand paper with the mesh number of 60 to 80 ℃ after spin coating for 15 seconds at a spin coating speed of 5000rpm for 5 minutes to form an original substrate, wherein the SEBS solution is prepared by dissolving SEBS in toluene to prepare a solution with the mass percentage concentration of 8%;
step 2: performing magnetron sputtering to deposit Mn metal layer on the surface of the original substrate, wherein vacuum degree is 10 during deposition -3 Pa, ar is introduced to adjust the air pressure to be 3Pa, the current is 25mA, the voltage is 250V, the sputtering power is 20W, and the sputtering time is 160s;
step 3: after deposition of the Mn metal layer, a WPU solution having a concentration of 18% was applied at 380. Mu.L/cm 2 Dripping onto the surface of the metal layer, naturally drying at room temperature, and then peeling the WPU film with the Mn metal layer from the surface of the original substrate.
Mn metal electrodes prepared by the embodiment and taking WPU as a substrate are subjected to stretching at different angles, so that the surface resistance changes tend to be consistent, and the performance tends to be stable. The metal electrode prepared by the invention has no orientation in the stretching dimension, and can achieve uniform stretching in all directions. The resistance change of the electrode is stable in the stretching deformation process.
Example 3
The preparation method of the double-fold electrode film comprises the following steps:
step 1: the method comprises the steps of spin-coating Ecoflex platinum silica gel on the surface of sand paper with the mesh number of 600, wherein the spin-coating speed is 5500rpm, the spin-coating time is 15s, then curing for 12h at room temperature, and curing to form an original substrate, wherein A and B in the Ecoflex platinum silica gel are mixed according to the mass ratio of 1:1;
step 2: performing magnetron sputtering deposition on the surface of the original substrate to form an Au metal layer, wherein the vacuum degree is 10 during deposition -2 Pa, ar is introduced to adjust the air pressure to 3Pa, the current is 20mA, the voltage is 260V, the sputtering power is 22.5W, and the sputtering time is 150s;
step 3: after deposition of the Au metal layer, a WPU solution with a concentration of 22% was applied at 350. Mu.L/cm 2 Dripping onto the surface of the metal layer, naturally drying at room temperature, and peeling the WPU film with the Au metal layer from the original substrate surface.
As shown in figure 1, the invention further forms an irregular and unoriented second heavy fold structure on the surface of the original substrate fold structure, has a larger tensile strain range than a single fold structure, and has lower sensitivity of double folds and higher resistance change stability under the same tensile rate. The surface morphology of the Au film prepared by the invention is shown in figure 3, and the double-fold structure is obvious. The resistance change of the Au thin film electrode prepared in this example after being stretched in different directions is shown in table 1.
Table 1: surface resistance value change (Ω/≡) of Au electrode under tensile strain in different directions
The Au metal film was subjected to tensile tests of different degrees with respect to the rotation angle in the counterclockwise direction with the horizontal direction as 0 °. The electrodes are pulled at the same time under different anglesAfter extension strain, the surface resistance changes tend to be consistent; the resistance change rate is slowly increased along with the increase of the tensile deformation, and when the deformation is increased to 50%, the resistance change rate delta R/R is increased 0 The specific resistance change rate of the structure was 13.7, which was significantly lower than that of the single fold structure, and the stability was excellent. The stretchability of the Au thin film electrode in different directions can reach more than 100%.
Comparative example 1
Compared with example 3, the PDMS solution is adopted to rotate on the surface of sand paper with the mesh number of 60, (the mass ratio of PDMS to curing agent is 1:1), the spin coating speed is 5500rpm, the spin coating time is 15s, and then the original substrate is obtained after curing for 4h at 80 ℃; the remaining steps remain the same as in example 3.
The Au thin film electrode material prepared by the comparative example only forms a single fold structure, when the Au thin film is subjected to a tensile test, the resistance change is larger in the tensile process, and when the Au thin film is stretched to 50%, the resistance change rate delta R/R is higher than that of the Au thin film 0 Up to about 800, the resistance change is extremely sensitive, and the material is not suitable for being used as an electrode material, and is more suitable for being used as a sensor material.
Comparative example 2
A preparation method of a double-fold film electrode comprises the following steps:
on the basis of example 3, the Au layer deposited by magnetron sputtering in step 2 was replaced with an Ag layer, and the rest of the steps were the same as those of example 3.
In the comparative example, the surface of the Ag film electrode is basically free of wrinkles, when the Ag film is subjected to a tensile test by the film electrode, obvious cracks appear when the film electrode is stretched to about 10%, the resistance change is large in the stretching process, and when the film electrode is stretched to 20%, the resistance change rate DeltaR/R is high 0 When reaching infinity, the stability is extremely poor, and when stretched to 40%, the film breaks.
In the research process, only the original matrix prepared by the specific material can be completely etched to form the rough surface of the template, thereby contributing to the subsequent formation of a double fold structure and the promotion of magnetron sputtering to form a second double fold. And the surface morphology of the sand paper is re-carved by adopting PDMS, so that the result shows that the fold structure of the surface of the prepared PDMS matrix is not obvious, can be basically ignored, and has little influence on the secondary fold structure formed in the subsequent magnetron sputtering process. Meanwhile, the formation of folds by magnetron sputtering is also aimed at different metal materials, and the Ag layer is prepared by magnetron sputtering, so that the expected fold structure cannot be formed, and the Ag layer does not have better tensile strain.
Example 4
The preparation method of the double-fold electrode film is characterized by comprising the following steps of:
step 1: the method comprises the steps of spin coating Ecoflex platinum silica gel with the mesh number of 100 on the surface of sand paper, spin coating speed of 5800rpm, spin coating time of 20s, and curing for 3h at room temperature to form an original substrate, wherein A and B in the Ecoflex platinum silica gel are mixed according to the mass ratio of 1:1;
step 2: performing magnetron sputtering to deposit a Cu metal layer on the surface of the original substrate, wherein the vacuum degree is 10 during deposition -3 Pa, ar is introduced to adjust the air pressure to be 3Pa, the current is 25mA, the voltage is 280V, the sputtering power is 30W, and the sputtering time is 160s;
step 3: after the metal layer is deposited, WPU solution with the concentration of 18-25% is mixed with the solution at the concentration of 320-380 mu L/cm 2 Dripping onto the surface of the metal layer, naturally drying at room temperature, and then stripping the WPU film with the Cu metal layer from the original substrate surface.
Example 5
The preparation method of the double-fold electrode film is characterized by comprising the following steps of:
step 1: spin-coating SEBS solution on the surface of the abrasive paper with the mesh number of 500, wherein the spin-coating speed is 5500rpm, the spin-coating time is 12s, heating to 70 ℃ after the spin-coating is completed, and preserving heat for 10min to form an original substrate, wherein the SEBS solution is prepared by dissolving SEBS in toluene to prepare a solution with the mass percentage concentration of 10%;
step 2: performing magnetron sputtering to deposit a Cu metal layer on the surface of the original substrate, wherein the vacuum degree is 10 during deposition -2 Pa, ar is introduced to adjust the air pressure to be 3Pa, the current is 10mA, the voltage is 300V, the sputtering power is 40W, and the sputtering time is 110s;
step 3: after the metal layer deposition, a WPU solution with a concentration of 25% was applied at 320. Mu.L/cm 2 Dripping into goldThe surface of the layer is naturally dried at room temperature, and then the WPU film with the Cu metal layer is peeled off from the original substrate surface.
Example 6
The preparation method of the double-fold electrode film is characterized by comprising the following steps of:
step 1: spin-coating SEBS solution on the surface of sand paper with the mesh number of 60-600, wherein the spin-coating speed is 5800rpm, the spin-coating time is 10s, heating to 60 ℃ after the spin-coating is completed, and preserving heat for 20min to form an original substrate, wherein the SEBS solution is prepared by dissolving SEBS in tetrahydrofuran, and the mass concentration is 15%;
step 2: performing magnetron sputtering deposition on the surface of the original substrate to form an Au metal layer, wherein the vacuum degree is 10 during deposition -3 Pa, ar is introduced to adjust the air pressure to 3Pa, the current is 20mA, the voltage is 280V, the sputtering power is 30W, and the sputtering time is 150s;
step 3: after the metal layer was deposited, a WPU solution having a concentration of 20% was applied at 350. Mu.L/cm 2 Dripping onto the surface of the metal layer, naturally drying at room temperature, and peeling the WPU film with the Au metal layer from the original substrate surface.
Claims (1)
1. A preparation method of a double-fold membrane electrode is characterized by comprising the following steps: preparing an original substrate by spin coating with sand paper as a template, depositing a metal layer on the surface of the original substrate by magnetron sputtering, preparing a WPU film on the outermost surface, and finally stripping the WPU film with the metal layer from the surface of the original substrate, wherein the original substrate is made of Ecoflex platinum silica gel or SEBS thermoplastic elastomer, and the deposited metal layer is a Cu layer, an Mn layer or an Au layer, and specifically comprises the following steps:
step 1: the method comprises the steps of spin-coating Ecoflex platinum silica gel or an SEBS thermoplastic elastomer on the surface of sand paper with the mesh number of 60-600, wherein when the Ecoflex platinum silica gel is spin-coated, the spin-coating speed is 5500-6000 rpm, the spin-coating time is 10-20 s, then the sand paper is cured for 3-12 h at room temperature, when the SEBS is spin-coated, the mass percentage concentration of the SEBS is 8-15%, the spin-coating speed is 5000-5800 rpm, the spin-coating time is 10-15 s, and after the spin-coating is finished, the sand paper is heated to 60-80 ℃, and the temperature is kept for 5-20 min, so that an original substrate is formed;
step (a)2: performing magnetron sputtering to deposit a metal layer on the surface of the original substrate, wherein the metal layer is a Cu layer, a Mn layer or an Au layer, and the vacuum degree is 10 during deposition -3 ~10 -2 Pa, ar is introduced to adjust the air pressure to be 3Pa, the current is 10-25 mA, the voltage is 250-300V, the sputtering power is 20-40W, and the sputtering time is 110-160 s;
step 3: after the metal layer is deposited, the WPU solution with the concentration of 18-25% is processed at 320-380 mu L/cm 2 Dripping onto the surface of the metal layer, naturally drying at room temperature, and then peeling the WPU film with the metal layer from the original substrate surface.
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| AU2020101866A4 (en) * | 2020-08-18 | 2020-09-24 | Xiangtan University | A method for preparing ferroelectric thin film by magnetron sputtering and ferroelectric thin film |
| CN112026420A (en) * | 2020-09-09 | 2020-12-04 | 浙江驰怀烫印科技股份有限公司 | Highlight gold stamping foil |
| WO2020263014A1 (en) * | 2019-06-28 | 2020-12-30 | 주식회사 아모그린텍 | Thin film foil and method for manufacturing thin film foil |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109671534A (en) * | 2017-10-13 | 2019-04-23 | 北京航空航天大学 | A kind of fexible film electrode and preparation method thereof |
| WO2020263014A1 (en) * | 2019-06-28 | 2020-12-30 | 주식회사 아모그린텍 | Thin film foil and method for manufacturing thin film foil |
| CN110967131A (en) * | 2019-12-24 | 2020-04-07 | 中国科学院深圳先进技术研究院 | Flexible conductive composite film and preparation method thereof, and flexible pressure sensor and preparation method thereof |
| AU2020101866A4 (en) * | 2020-08-18 | 2020-09-24 | Xiangtan University | A method for preparing ferroelectric thin film by magnetron sputtering and ferroelectric thin film |
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