CN112570230A

CN112570230A - Method for coating film on surface of micro electrode

Info

Publication number: CN112570230A
Application number: CN201910944917.XA
Authority: CN
Inventors: 王蕾; 林万钟; 卢陆旺; 李清
Original assignee: Shenzhen Sibionics Technology Co Ltd
Current assignee: Shenzhen Sibionics Technology Co Ltd
Priority date: 2019-09-30
Filing date: 2019-09-30
Publication date: 2021-03-30

Abstract

The disclosure provides a method for coating a film on the surface of a micro electrode, which is characterized by comprising the following steps: (a) preparing a microelectrode to be coated; (b) fixing the micro-electrode; (c) preparing a membrane solution and a cross-linking agent, and mixing to obtain a pulling liquid, wherein the viscosity of the pulling liquid is 0.1-20 cP; (d) immersing and pulling the microelectrode from the pulling liquid in a preset program under the atmosphere protection, wherein the gas in the atmosphere protection has the same composition as the solvent of the membrane solution; and (e) curing the microelectrode in a vacuum environment. The method disclosed by the invention is used for coating the surface of the micro electrode, so that the film on the surface of the micro electrode is good in consistency, uniform in thickness and smooth in appearance.

Description

Method for coating film on surface of micro electrode

Technical Field

The disclosure particularly relates to a method for coating a film on the surface of a micro electrode.

Background

Common coating liquid phase coating techniques include brush coating, dip coating, and spray coating. The dipping and pulling method is characterized in that a cleaned substrate is immersed into a prepared solution, then the substrate is stably pulled out of the solution at a precisely controlled uniform speed, a uniform liquid film is formed on the surface of the substrate under the action of viscosity and gravity, and the solution attached to the surface of the substrate rapidly gels along with the rapid volatilization of the solvent to form a gel film. The dip-coating method is a commonly used film preparation method, can be used for coating uniform and consistent films on a base cloth substrate and a base film, and is widely applied to the dip-coating film formation of sol-gel, solution and suspension.

The dip-coating method has been widely used because of its higher coating quality compared to the brush coating method and its advantage of simple and inexpensive equipment compared to the spray coating method.

In the mass coating production process, for coating technologies such as sol-gel method and slurry method which are coated in a liquid phase, it is a key and difficult point of the coating process to ensure the consistency and uniformity of the coating thickness and prevent the coating from cracking and failing in the drying process. Meanwhile, for the dip-draw method, it is also critical to improve coating quality to reduce coating unevenness due to the sagging effect of the coating solution.

Disclosure of Invention

The present disclosure has been made in view of the above-mentioned state of the art, and an object of the present disclosure is to provide a method for plating a surface of a micro-electrode, which can improve uniformity of a thin film and can make the thickness of the thin film uniform and the appearance flat.

Therefore, the disclosure provides a method for coating a film on the surface of a micro electrode, which is characterized by comprising the following steps: comprises (a) preparing a microelectrode to be coated; (b) fixing the micro-electrode; (c) preparing a membrane solution and a cross-linking agent, and mixing to obtain a pulling liquid, wherein the viscosity of the pulling liquid is 0.1-20 cP; (d) immersing and pulling the microelectrode from the pulling liquid in a preset program under the atmosphere protection, wherein the composition of gas in the atmosphere protection is the same as the solvent of the membrane solution; and (e) curing the microelectrode in a vacuum environment.

In the method for dip-coating the surface of the micro electrode, the micro electrode is fixed, then a film solution with a proper concentration is prepared and mixed with a proper amount of cross-linking agent to obtain a dip-coating solution with the viscosity of 0.1-20 cP, and then the micro electrode is dip-coated, wherein the dip-coating solution can be protected by the atmosphere during the dip-coating process, and the components of the atmosphere are the same as the solvent of the film solution.

Further, in the method according to the present disclosure, optionally, the predetermined program includes a pulling step of immersing the microelectrode in the pulling liquid at an immersion rate of 2mm/s to 8mm/s for 1s to 60s, followed by pulling the microelectrode out of the pulling liquid at a pulling rate of 2mm/s to 8 mm/s. Thereby, a thin film having a constant thickness can be formed on the surface of the microelectrode.

In addition, in the method according to the present disclosure, optionally, the predetermined procedure further includes repeating the pulling step at least 1 time, and when the number of repetitions is greater than 5 times, decreasing the pulling rate in the pulling step from 6 th time. Therefore, a multilayer film can be formed, the surface of the micro electrode is smoother, and the performance is more stable.

In addition, in the method according to the present disclosure, in the step (d), the saturation degree of the gas may be 90% to 100%. In this case, the gas can effectively suppress volatilization of the solution, and thus the concentration of the drawing liquid can be maintained during the dipping and drawing.

Additionally, in methods contemplated by the present disclosure, optionally, the solute of the membrane solution is selected from poly-4-vinylpyridine, poly-4-vinylpyridine-SO₃The solvent is at least one of ethanol, water, tetrahydrofuran, acetone, ethyl acetate, diethyl ether, turpentine, mineral solvent and volatile oil. In this case, the membrane solution can have one or more different solutes, whereby,different solutes can be selected as desired.

In addition, in the method related to the present disclosure, optionally, the ingredient of the cross-linking agent is selected from at least one of polyethylene glycol dimethyl ether, polyethylene glycol, boric acid, adipic acid dihydrazide, polyacrylic amine, and polyisocyanate. Therefore, the tensile strength, water resistance and viscosity of the film can be improved.

In addition, in the methods contemplated by the present disclosure, the concentration of the membrane solution may be 1mg/ml to 150 mg/ml. Thus, a film solution having an appropriate viscosity can be selected as needed.

In addition, in the method according to the present disclosure, the crosslinking agent may be added in an amount of 1mg/ml to 25mg/ml in the pulling liquid. Therefore, the tensile strength and the water resistance of the film can be improved, and the pulling liquid with proper viscosity can be formed.

In addition, in the method according to the present disclosure, optionally, in the step (a), the microelectrode is washed with deionized water for 1 to 10min after being washed with ethanol for 1 to 10 min. Therefore, foreign matters on the surface of the micro electrode can be removed, and a flat film can be formed.

Further, in the method according to the present disclosure, optionally, in the step (e), the microelectrode is cured in a vacuum environment for 20 to 30 hours. This enables the film to be more favorably condensed on the surface of the microelectrode.

According to the method, the film coating on the surface of the micro electrode can be improved in film consistency, and the film is uniform in thickness and smooth in appearance.

Drawings

Fig. 1 shows a schematic flow diagram of a method for plating a surface of a micro-electrode according to an example of the present disclosure.

Fig. 2 shows a perspective view of a dip coater according to an example of the present disclosure.

Fig. 3 shows a schematic diagram of an impregnation lift process according to an example of the present disclosure.

Fig. 4 shows a perspective view of a jig according to an example of the present disclosure.

Fig. 5 shows a partial schematic view of a jig according to another example of the present disclosure.

Detailed Description

Hereinafter, preferred embodiments of the present disclosure will be described in detail with reference to the accompanying drawings. In the following description, the same components are denoted by the same reference numerals, and redundant description thereof is omitted. The drawings are schematic and the ratio of the dimensions of the components and the shapes of the components may be different from the actual ones.

Fig. 1 shows a schematic flow diagram of a method for plating a surface of a micro-electrode according to an example of the present disclosure. Fig. 3 shows a schematic diagram of an impregnation lift process according to an example of the present disclosure.

As shown in fig. 1, a method for coating a surface of a micro-electrode according to the present embodiment may include preparing a micro-electrode to be coated (step S10); fixing the micro-electrodes (step S20); preparing a membrane solution and a cross-linking agent, and mixing to obtain a pulling liquid, wherein the viscosity of the pulling liquid can be 0.1-20 cP (step S30); immersing and pulling the microelectrode from the pulling liquid in a predetermined procedure under an atmosphere protection in which the composition of the gas is the same as the solvent of the film solution (step S40); and the microelectrodes are cured in a vacuum environment (step S50).

In the method for plating a film on the surface of a microelectrode according to this embodiment, the microelectrode is fixed, a film solution having an appropriate concentration is prepared and mixed with an appropriate amount of a crosslinking agent to obtain a draw solution having a viscosity of 0.1 to 20cP, and the microelectrode is subjected to dip-drawing, wherein the draw solution is protected by an atmosphere during the dip-drawing process, and the composition of the atmosphere is the same as the solvent of the film solution.

In this embodiment, the surface of the micro-electrode may be coated by dip-coating. As shown in fig. 3, the dipping and pulling process may be such that the member to be coated is dipped in a solution and then pulled out of the solution, and the solution attached to the surface of the member to be coated is formed into a thin film under the action of viscosity and gravity and accompanied by volatilization of the solvent.

In the present embodiment, a microelectrode to be coated may be prepared in step S10. In addition, in some examples, the prepared micro-electrodes to be coated may be washed in step S10. In other examples, in step (a), the microelectrode may be washed with ethanol for 1 to 10min and then with deionized water for 1 to 10 min. Therefore, foreign matters on the surface of the micro electrode can be removed, and a flat film can be formed. For example, the microelectrode may be rinsed with ethanol for 1min and then with deionized water for 5 min.

In some examples, the microelectrode may be rinsed with ethanol for 5min and then with deionized water for 1 min. In other examples, the microelectrode may be rinsed with ethanol for 10min, followed by deionized water for 10min, and so on.

In addition, in the present embodiment, the roughness of the surface of the micro-electrode in step S10 may be 0.01 μm to 10 μm. This can facilitate the formation of a thin film on the surface of the microelectrode by the drawing liquid.

In some examples, the roughness of the surface of the microelectrode may be 0.01 μm. In other examples, the surface roughness of the microelectrode may be 10 μm. In addition, in some examples, the roughness of the surface of the microelectrode may be 0.05 μm, 0.1 μm, 0.5 μm, 1 μm, 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, or 8 μm.

In the present embodiment, the material of the microelectrode is not particularly limited, and may be selected according to actual needs. In some examples, the microelectrode may be made of a biosafety material. Thereby, can be implanted or acted on the human body.

In some examples, the micro-electrodes may be made of a metallic material. Additionally, in some examples, the microelectrodes may be made of at least one of platinum, nickel, cobalt, titanium, tantalum, niobium, zirconium. For example, the microelectrode may be made of platinum metal, niobium metal, or an alloy of nickel and cobalt, etc.

In the present embodiment, the shape of the microelectrode is not particularly limited, and may be selected according to actual needs. For example, the microelectrode may be needle-shaped, sheet-shaped, or the like.

In some examples, the micro-electrodes may be connected to pads. Additionally, in some examples, the pads may be circular or polygonal. In other examples, the sizes of the micro-electrodes and the pads may not be uniform. For example, the pads may be wider than the microelectrodes. In addition, the micro-electrodes and the bonding pads can be integrally formed. In some examples, the micro-electrodes may be electrode sheets to which pads are connected. In other examples, the micro-electrodes may include pads.

In this embodiment, the microelectrode is fixed in step S20. Specifically, the microelectrode obtained in step S10 may be mounted on the coated jig 1 to be fixed, and then the coated package may be obtained.

The jig 1 used in step 20 according to the present embodiment will be described in detail below with reference to the drawings.

FIG. 2 shows a perspective view of a dip coater 2 according to an example of the present disclosure. Fig. 4 shows a perspective view of the jig 1 according to the example of the present disclosure, in which fig. 4(a) shows a perspective view of the jig 1 according to the example of the present disclosure, fig. 4(b) shows a schematic configuration of the connection portion 30 according to the example of the present disclosure, fig. 4(c) shows a schematic configuration of the loading portion 10 according to the example of the present disclosure, and fig. 4(d) shows a schematic configuration of the cover plate 20 according to the example of the present disclosure.

In the present embodiment, as shown in fig. 4, the jig 1 for coating (hereinafter, sometimes referred to as "jig 1") may include a loading portion 10 and a cover plate 20. In some examples, the loading portion 10 has a first loading surface 11 and a bottom surface (not shown) intersecting the first loading surface 11. A plurality of positioning grooves 111 for fixing the micro electrodes are arranged in parallel on the first loading surface 11, and the positioning grooves 111 penetrate through the bottom surface in a direction parallel to the first loading surface 11. In addition, in some examples, the cover plate 20 cooperates with the first loading surface 11 of the loading part 10 to fix the micro-electrodes located at the positioning grooves 111.

In the coating jig 1 according to the present embodiment, the first mounting surface 11 of the mounting portion 10 includes a plurality of positioning grooves 111 for placing the microelectrodes in parallel. In this case, the jig 1 can simultaneously place a plurality of micro electrodes, and the positions of the micro electrodes fixed on the jig 1 are consistent, so that the micro electrodes before coating can be relatively consistent, and the consistency of coating is improved. In addition, in some examples, the jig 1 has a cover plate 20 that is fitted with the first loading surface 11 of the loading portion 10. In this case, the micro-electrodes can be fixed more favorably, which is advantageous for improving the coating quality, and thus the jig 1 for coating can be provided in which the coating uniformity can be improved while coating in batches.

In addition, in some examples, the jig 1 may further include a connection portion 30. In addition, an end of the loading part 10 away from the positioning groove 111 may be engaged with the connecting part 30. In this case, the jig 1 can be attached to the coating machine through the connecting portion 30, and thus the coating machine can control the jig 1 to coat a film. In addition, the bottom surface of the loading portion 10 is distant from the connection portion 30.

In addition, in some examples, as shown in fig. 4(b), the connection part 30 may be a combined structure. In this case, the connecting portion 30 can connect the coating machine and fix the loading portion 10 (described later in detail). Additionally, in some examples, the connection portion 30 may be assembled from flat plates. This facilitates connection of the connection portion 30 to the coating machine. For example, in some examples, the connection portion 30 may be formed by combining a first plate 31 and a second plate 32.

In addition, in some examples, as shown in fig. 4(b), the first plate 31 may have a first type fixing hole 311, and the second plate 32 may be engaged with the first type fixing hole 311. In some examples, the first plate 31 and the second plate 32 may be fixed using screws. In other examples, the connection portion 30 may be formed by combining a flat plate and a cylinder. Additionally, in some examples, the connection portion 30 may be integrally formed.

In some examples, the first plate 31 may have a plurality of first-type fixing holes 311. In addition, in some examples, the first plate 31 may have 2 to 10 first-type fixing holes 311. For example, the first plate 31 may have 2, 3, 4, 5, 6, 7, 8, 9 or 10 first-type fixing holes 311. In other examples, the plurality of first-type fixing holes 311 may be located on the same horizontal line.

In addition, in some examples, as shown in fig. 4(b), the connection part 30 may have a groove 321 to be fitted with the loading part 10. In some examples, the connecting portion 30 may have a plurality of grooves 321 to be fitted with the loading portion 10. For example, the connecting portion 30 may have 2 to 8 grooves 321 to be fitted with the loading portion 10. Additionally, in some examples, the connection 30 may have 1, 2, 3, 4, 5, 6, 7, or 8 grooves 321.

In addition, in some examples, the groove 321 may have a second type fixing hole 322 therein for fixing the loading portion 10, and the loading portion 10 may be matched with the second type fixing hole 322.

In some examples, the groove 321 may have a plurality of second type fixing holes 322. In addition, in some examples, the groove 321 may have 2 to 10 second-type fixing holes 322. For example, the groove 321 may have 2, 3, 4, 5, 6, 7, 8, 9, or 10 second type of fixation holes 322. In other examples, the plurality of second-type fastening holes 322 may be located on the same horizontal line.

In addition, in some examples, the loading part 10 may be mounted to the connection part 30 by a fixing mechanism. In this case, the mounting portion 10 can be well mounted to the connection portion 30. Additionally, in some examples, the securing mechanism may be a snap fit structure or a threaded structure. In this case, the mounting portion 10 can be more favorably fixed to the connecting portion 30. For example, in some examples, the loading portion 10 may be mounted to the connecting portion 30 using screws. In other examples, the loading portion 10 may be mounted to the connection portion 30 by a snap-fit structure.

In addition, in some examples, the connection portion 30 may be fixed to the coating machine using a screw fixing method, a snap-fit method, or a magnetic attraction method. In this case, the jig 1 for coating can be fixed to the coating machine, and the microelectrodes can be coated satisfactorily by the coating machine thereafter. Additionally, in some examples, the coating machine may be a dip coater 2 (see fig. 2). In some examples, the connection 30 may be secured to the dip coater 2 using a screw-on fastening. In other examples, the connection portion 30 may be magnetically secured to the dip coater 2.

In addition, in some examples, as shown in fig. 4, the jig 1 may have a plurality of loading parts 10 in a plate shape. In this case, the plate-shaped mounting portion 10 facilitates the fixing with the cover plate 20, and thus more micro-electrodes can be fixed to the jig 1 well. In some examples, the jig 1 may have 2 to 12 loading portions 10. For example, the jig 1 may have 2, 4, 5, 6, 8, 10, or 12 loading portions 10. In other examples, the jig 1 may have only 1 loading portion 10.

In some examples, the loading portion 10 may have a first loading surface 11. In addition, in some examples, the loading part 10 may further have a bottom surface intersecting the first loading surface 11.

In some examples, as shown in fig. 4(c), the loading part 10 may have a positioning groove 111. In addition, in some examples, the loading part 10 may be provided with a plurality of positioning grooves 111. As shown in fig. 4(c), the first loading surface 11 may be provided with a plurality of positioning grooves 111. In other examples, a plurality of positioning grooves 111 may be arranged side by side on the first loading surface 11.

In some examples, the positioning groove 111 may be used to fix the microelectrode. Additionally, in some examples, the microelectrode may be placed within the detent 111. In other examples, pads that may be connected to micro-electrodes are placed in the positioning grooves 111. Thus, the micro-electrode can be fixed by the fixing pad.

In some examples, one loading portion 10 may have 2, 4, 6, 8, 10, 12, 14, 16, 18, 20, 22, or 24 positioning slots 111. In other examples, one loading part 10 may have 1 positioning groove 111.

In some examples, as shown in fig. 4(c), the positioning groove 111 may penetrate the bottom surface in a direction parallel to the first loading surface 11. Additionally, in some examples, the shape of the detents 111 may match the shape of the microelectrode. In other examples, the portion of the positioning groove 111 near the bottom surface may be larger than the portion far from the bottom surface.

In addition, in some examples, the shape and depth of the positioning groove 111 may be substantially the same as the contact portion of the micro-electrode with the cover plate 20 and the loading part 10. This can facilitate fixation of the microelectrode. In other examples, the shape and depth of the positioning groove 111 may be slightly larger than the contact portion of the micro-electrode with the cover plate 20 and the loading portion 10. In some examples, the orientation of the positioning groove 111 may be a direction perpendicular to the bottom surface.

In addition, in some examples, the loading portion 10 further includes a second loading surface (not shown) parallel to the first loading surface 11, a bottom surface connecting the first loading surface 11 and the second loading surface, and an edge of a cover 20 (described in detail later) does not exceed the bottom surface. Therefore, more micro electrodes can be fixed, the interference of the micro electrodes in the coating process can be reduced, and the coating consistency of the micro electrodes can be improved. In some examples, the edges of the cover plate 20 may be aligned with the bottom surface.

In addition, in some examples, the second loading surface is provided with a plurality of positioning grooves 111 for placing the micro-electrodes side by side, like the first loading surface 11. For example, in some examples, the first loading surface 11 of the loading portion 10 may have 1, 2, 4, 6, 8, 10, 12, 14, or 16 positioning slots 111, and the second loading surface of the loading portion 10 may have the same 1, 2, 4, 6, 8, 10, 12, 14, or 16 positioning slots 111.

In addition, in some examples, the first loading surface 11 of the loading part 10 may have the positioning groove 111, and the second loading surface of the loading part 10 may not have the positioning groove 111. For example, the first loading surface 11 of the loading part 10 may have 1, 3, 5, 7, 9, 11, 13, 15, or 16 positioning grooves 111, and the second loading surface of the loading part 10 may not have the positioning grooves 111.

In addition, in some examples, the second loading surface of the loading part 10 may have the positioning groove 111, and the first loading surface 11 of the loading part 10 may not have the positioning groove 111. For example, the second loading surface of the loading part 10 may have 1, 3, 5, 7, 9, 11, 13, 15, or 16 positioning grooves 111, and the first loading surface 11 of the loading part 10 may not have the positioning grooves 111.

In addition, in some examples, the jig 1 may further include a back plate 40 engaged with the second loading surface of the loading portion 10, and an edge of the back plate 40 does not exceed the bottom surface. In this case, the micro-electrodes placed in the second loading surface can be well fixed. In some examples, the edges of the back plate 40 may be aligned with the bottom surface. Additionally, in some examples, the cover plate 20 may have the same structure as the back plate 40. This enables more microelectrodes to be fixed more effectively.

In addition, in some examples, as shown in fig. 4(c) and 4(d), the loading part 10 may have a third type fixing hole 12, and the cover plate 20 (described in detail later) may have a fourth type fixing hole 21 to be matched with the third type fixing hole 12. Thereby, the cover plate 20 can be fixed to the mounting portion 10.

In some examples, the loading part 10 may have a plurality of third type fixing holes 12. In addition, in some examples, the loading part 10 may have 2 to 10 third-type fixing holes 12. For example, the loading portion 10 may have 2, 3, 4, 5, 6, 7, 8, 9, or 10 third type of fixation holes 12. In other examples, the plurality of third type fixing holes 12 may be located on the same or different horizontal lines.

In some examples, the cover plate 20 may have a plurality of fourth type fixing holes 21. In addition, in some examples, the cover plate 20 may have 2 to 10 fourth-type fixing holes 21. For example, the cover plate 20 may have 2, 3, 4, 5, 6, 7, 8, 9 or 10 fourth type fixing holes 21. In other examples, the plurality of fourth type fixing holes 21 may be located on the same or different horizontal lines.

In some examples, the cover plate 20 may be mated with the loading portion 10. In other words, the third type of fixing holes 12 can be fitted with the fourth type of fixing holes 21. Thereby, the cover plate 20 can be fixed to the loading part 10. In addition, in some examples, the cover plate 20 may be engaged with the loading portion 10 using a screw fastening method, a magnetic attraction method, or a snap structure. In this case, the cover plate 20 can be well fitted to the loading part 10, and thus the micro-electrodes located at the positioning grooves 111 can be well fixed.

In some examples, the cover plate 20 may be engaged with the loading part 10 using a screw fixing manner. For example, the loading part 10 and the cover plate 20 may be fastened by screws via the third type fixing holes 12 and the fourth type fixing holes 21. In other examples, the cover plate 20 may be magnetically engaged with the loading portion 10. For example, the mounting portion 10 and the cover plate 20 may be fixed by a magnet through the third type fixing hole 12 and the fourth type fixing hole 21.

In addition, in some examples, the cover plate 20 may cooperate with the first loading surface 11 of the loading part 10 to fix the micro-electrodes located at the positioning grooves 111. In some examples, the cover plate 20 may have an abutting surface 22 that cooperates with the first loading surface 11.

In addition, in some examples, the cover plate 20 may have a protrusion 221 that mates with the positioning groove 111. This enables the microelectrode to be fixed more favorably. In some examples, the protrusion 221 may be disposed on the abutting surface 22 of the cover plate 20.

Additionally, in some examples, the protrusion 221 may be a flexible substance. In this case, when the cover plate 20 is engaged with the positioning groove 111, the protrusion 221 is adaptively deformed, thereby better fixing the micro-electrode. For example, in some examples, the protrusion 221 may be an adhesive tape.

In addition, in some examples, the flexible substance may be selected from at least one of silicone, rubber, parylene, polyimide, polytetrafluoroethylene, and polyvinyl alcohol. This can further fix the microelectrode. For example, in some examples, the flexible substance may be silicone. In other examples, the flexible substance may be polyimide. Additionally, in still other examples, the flexible substance may be polyvinyl alcohol.

In addition, in some examples, as shown in fig. 4(d), the protrusion 221 of the cover plate 20 that mates with the positioning groove 111 may be continuous, for example, the cover plate 20 may have a strip of adhesive tape that mates with the positioning groove 111. In other examples, the protrusion 221 of the cover plate 20 that mates with the positioning slot 111 may be discontinuous, for example, the cover plate 20 has a silicone pad only at a position corresponding to the positioning slot 111.

In addition, in some examples, the fixture 1 may not include the connection portion 30, and the loading portion 10 may be directly fixed to the dip coater 2 by a magnetic attraction method.

Fig. 5 shows a partial schematic view of a jig 1 according to another example of the present disclosure. Wherein, fig. 5(a) shows a schematic structural view of a loading part 10A according to another example of the present disclosure, fig. 5(b) shows a schematic structural view of a cover plate 20A according to another example of the present disclosure,

in other examples, as shown in fig. 5, the jig 1 may include a loading part 10A and a cover plate 20A. In some examples, the jig 1 may include a loading part 10A without the positioning groove 111 and a cover plate 20A without the protrusion 221. In addition, in some examples, the cover plate 20A and the loading part 10A may be fixed using a magnetic attraction method or a screw fixing method.

In some examples, as shown in fig. 5(a), the loading part 10A may include a first-type stopper hole 13. In addition, in some examples, as shown in fig. 5(b), the cover plate 20A may include a second type of stopper hole 23.

In some examples, the loading portion 10A may include a plurality of first type restraint holes 13, and the cover plate 20A may include a plurality of second type restraint holes 23. Additionally, in some examples, the first type of retention apertures 13 may mate with the second type of retention apertures 23. This can be used to assist in fixing the microelectrode.

In some examples, the microelectrode may have a through hole that mates with the first type of position-limiting hole 13 and the second type of position-limiting hole 23. In other examples, the microelectrode may have a plurality of through holes. I.e. each microelectrode may have a plurality of through holes.

In some examples, the microelectrode may have 2 to 5 vias. For example, the microelectrode may have 2, 3, 4 or 5 through holes. Additionally, in some examples, the microelectrode may have 1 through hole.

In other examples, the pads may have through holes that mate with the first type of retention holes 13 and the second type of retention holes 23. In this case, if the pad is placed in the positioning groove 111, the pad can be fitted into the first-type stopper hole 13 and the second-type stopper hole 23 to fix the pad, thereby fixing the micro-electrode. Additionally, in some examples, the pad may have a plurality of vias. I.e., each pad may have a plurality of vias.

In other examples, the pad may have 2 to 5 vias. For example, the pad may have 2, 3, 4, or 5 vias. Additionally, in some examples, the pad may have 1 via.

In some examples, the jig 1 may include a plurality of limiting posts (not shown). In other examples, the spacing post may be cylindrical or prismatic. Additionally, the diameter of the restraint posts may be slightly smaller than the diameter of the first type of restraint holes 13 and the second type of restraint holes 23.

In some examples, the restraint posts may extend through the first type restraint holes 13, the second type restraint holes 23, and the through holes. In addition, in some examples, the micro-electrode can be mounted on the jig 1 through the first type of limiting hole 13, the second type of limiting hole 23, the through hole and the limiting post.

In some examples, each of the restraint posts may simultaneously extend through the first type of restraint hole 13 and the second type of restraint hole 23 to secure the microelectrode. In other examples, each of the position-limiting pillars may pass through only a portion of the first-type position-limiting holes 13 and a portion of the second-type position-limiting holes 23 to fix the micro-electrodes.

In addition, in some examples, the jig 1 may further include a pressing plate (not shown). In addition, the pressing plate may have the same structure as the cover plate 20A. For example, the platen may have a third type of retention hole (not shown) that mates with the first type of retention hole 13. In addition, the pressing plate may be engaged with the second surface of the loading part 10A.

In some examples, each of the limiting posts may simultaneously penetrate the first type of limiting hole 13, the second type of limiting hole 23 and the third type of limiting hole to fix two micro-electrodes. In other examples, each of the retention posts may extend through the first type of retention hole 13 and extend partially into the second type of retention hole 23 and the third type of retention hole to secure two microelectrodes.

In addition, in some examples, one of the first type limiting hole 13, the second type limiting hole 23 and the third type limiting hole may be provided to penetrate the first type limiting hole 13 and extend partially into the second type limiting hole 23 to fix the microelectrode, and the other limiting column may penetrate the first type limiting hole 13 and extend partially into the third type limiting hole to fix the other microelectrode.

In addition, in some examples, the jig 1 can fix 1 to 200 micro-electrodes. In this case, the subsequent simultaneous batch coating of a plurality of microelectrodes can be facilitated, and the pre-coating states of the microelectrodes within and between batches can be relatively consistent, so that the uniformity of the thin films formed by the microelectrodes within and between batches can be good.

In addition, in the present embodiment, in step S20, the micro-electrodes may be fixed at substantially the same position in the jig 1. In this case, the consistency of the clamping before coating each micro-electrode can be improved, and the state of each micro-electrode coated can be made consistent.

In some examples, a membrane solution may be prepared in step S30. Specifically, in step S30, a membrane solution may be prepared by dissolving a solute in a solvent. In addition, the concentration of the membrane solution may be 1mg/ml to 150 mg/ml. Thus, a film solution having an appropriate viscosity can be selected as needed.

In some examples, the concentration of the membrane solution may be 64 mg/ml. In other examples, the concentration of the membrane solution may be 150 mg/ml. Additionally, in some examples, the concentration of the membrane solution may be 1mg/ml, 5mg/ml, 10mg/ml, 20mg/ml, 40mg/ml, 60mg/ml, 70mg/ml, 80mg/ml, 100mg/ml, 120mg/ml, or 140 mg/ml.

In addition, in the present embodiment, in step S30, the solute of the membrane solution may be selected from poly 4-vinylpyridine (P4VP), poly 4-vinylpyridine-SO₃(P4VP-SO₃) Polyvinylpyrrolidone (PVP) and polyurethaneAt least one of ester (PU), polypropylene (PP), polyethylene oxide (PEO), polyvinyl alcohol (PVA), Polyacrylate (PEA), polyacrylic acid (PAA). In this case, the membrane solution can have one or more different solutes, whereby the different solutes can be selected as desired.

In some examples, the solute of the membrane solution may be poly-4-vinylpyridine-SO₃. In other examples, the solute of the membrane solution may be polyethylene oxide. Additionally, in still other examples, the solute of the membrane solution may be polyvinylpyrrolidone.

In addition, in the present embodiment, the solvent may be selected from ethanol and water in step S30, thereby being capable of dissolving the solute well to form the membrane solution. In addition, since the solvent has volatility, it can contribute to the generation of atmosphere protection and can contribute to the drying of the film. For example, in some examples, the solvent may be ethanol. In other examples, the solvent may be tetrahydrofuran. Additionally, in some examples, the solvent may be a mixture of ethanol and water.

In the present embodiment, a cross-linking agent may be mixed with the membrane solution in step S30 to obtain a draw solution. Specifically, in step S30, a draw solution may be formed by adding a cross-linking agent to the prepared membrane solution and mixing. In addition, the viscosity of the pulling liquid may be 0.1 to 20 cP. Thereby, a thin film can be formed on the surface of the microelectrode.

In some examples, the viscosity of the draw solution may be 0.1 cP. In other examples, the viscosity of the draw solution may be 20 cP. Additionally, in some examples, the viscosity of the pulling fluid can be 0.2cP, 0.5cP, 1cP, 2cP, 5cP, 8cP, 10cP, 12cP, 15cP, or 18 cP.

In addition, in some examples, in step S30, the ingredient of the cross-linking agent may be selected from at least one of polyethylene glycol dimethyl ether, polyethylene glycol, boric acid, adipic acid dihydrazide, polyacrylic amine, and polyisocyanate. Therefore, the tensile strength, water resistance and viscosity of the film can be improved. For example, in some examples, the component of the crosslinking agent may be dimethyl ether of polyethylene glycol. In other examples, the cross-linking agent may be a adipic acid dihydrazine. Additionally, in still other examples, the ingredient of the crosslinking agent may be polyethylene glycol.

In addition, in the present embodiment, in step S30, the amount of the crosslinking agent added to the pulling liquid may be 1mg/ml to 25 mg/ml. Therefore, the tensile strength and the water resistance of the film can be improved, and the pulling liquid with proper viscosity can be formed. For example, in some examples, the crosslinker may be added in an amount of 6 mg/ml. In other examples, the crosslinker may be added in an amount of 25 mg/ml. Additionally, in still other examples, the crosslinker may be added in an amount of 1mg/ml, 2mg/ml, 5mg/ml, 7mg/ml, 10mg/ml, 12mg/ml, 15mg/ml, 20mg/ml, or 22 mg/ml.

Additionally, in some examples, the crosslinking agent may be a solid. In other examples, the crosslinking agent may be a crosslinking agent solution. In some examples, the solvent of the crosslinker solution may be the same as the solvent of the membrane solution.

In some examples, in step S40, the microelectrodes may be dip-pulled under an atmosphere protection. In addition, in some examples, in step S40, the micro-electrodes may be immersed and pulled out from the pulling liquid in a predetermined procedure under the atmosphere protection.

In addition, in some examples, in step S40, the predetermined program may include a pulling step of immersing the microelectrodes in the draw solution at an immersion rate of 2mm/S to 8mm/S for a time of 1S to 60S, followed by pulling the microelectrodes out of the draw solution at a draw rate of 2mm/S to 8 mm/S. Thereby, a thin film having a constant thickness can be formed on the surface of the microelectrode.

In some examples, the dip rate, pull rate, and dip time may affect the film thickness. In addition, in some examples, the appropriate dipping rate, pulling rate, and dipping time may be selected according to actual needs.

In some examples, the predetermined program may include immersing the microelectrode into the draw solution at an immersion rate of 6mm/s for a period of 5s, followed by pulling out from the draw solution at a pull rate of 6 mm/s.

In some examples, the parameters of the pulling step may be: the descending rate was 4mm/s, the lifting rate was 4mm/s, and the dipping time was 8 s. In addition, in some examples, the parameters of the pulling step may be: the descending rate is 5mm/s, the lifting rate is 5mm/s, and the dipping time is 12 s. In other examples, the parameters of the pulling step may be: the descending rate was 7mm/s, the lifting rate was 7mm/s, and the dipping time was 15 s.

In some examples, in step S40, the predetermined procedure may further include repeating the pulling step at least 1 time. Therefore, a multilayer film can be formed, the surface of the micro electrode is smoother, and the performance is more stable. In addition, in some examples, when the number of repetitions is more than 5 times, the pulling rate in the pulling step may be reduced from 6 th. In this case, since the uniformity of the coating film decreases as the pull rate increases, the film formed on the surface of the microelectrodes can be made more uniform by decreasing the pull rate on the basis of a multi-layer film, i.e., the uniformity of the film on the microelectrodes can be improved.

In some examples, the predetermined procedure may include repeating the pulling step 1 to 30 times. For example, the pulling step may be repeated 1 time, 5 times, 6 times, 8 times, 10 times, 12 times, 15 times, 20 times, 25 times, 30 times, or the like. In some examples, the number of repetitions may be selected based on the desired thickness of the surface of the microelectrode.

In some examples, when the 1 st to 5 th pulling steps are repeated, the micro-electrodes may be immersed in the pulling liquid at an immersion rate of 6mm/s for 5s, and then pulled out from the pulling liquid at a pulling rate of 6 mm/s; when the pulling steps are repeated 6 to 10 times, the microelectrodes may be dipped into the pulling solution at a dipping rate of 6mm/s for 5s, and then pulled out from the pulling solution at a pulling rate of 3 mm/s.

In some examples, when the pulling steps are repeated 1 to 5 times, the micro-electrodes may be immersed in the pulling solution at an immersion rate of 8mm/s for 4s, and then pulled out from the pulling solution at a pulling rate of 6 mm/s; when the pulling steps are repeated 6 to 15 times, the microelectrodes may be dipped into the pulling solution at a dipping rate of 6mm/s for 4s, and then pulled out from the pulling solution at a pulling rate of 2 mm/s.

In some examples, since the number of repetitions is more than 5, the parameters of the pulling step may also be adjusted according to actual needs from the 6 th time. For example, the rate of immersion may be increased, the time of immersion may be extended, and the like.

In addition, in some examples, the predetermined procedure may be performed by the dip coater 2 in step S40. Thus, dip-drawing can be performed satisfactorily. In addition, in some examples, dip coater 2 may have equipment to create an atmosphere shield. This enables step S40 to be performed under an atmosphere protection. For example, in some instances, dip coater 2 may have a chamber that may be sealed to perform dip coating.

In addition, in some examples, step S40 may include fixing the coating to be coated in the dip coater 2. In this case, the batch of the micro-electrodes can be preferably dip-drawn.

In addition, in some examples, step S40 may include placing the dip prepared in step S30 in a hermetically sealable dip coating chamber of the dip coater 2. In addition, in some examples, the pulling liquid may be contained in only one container in the dip coater 2, in which case all the micro-electrodes fixed in the jig 1 may be dip-pulled in the pulling liquid in one container. In other examples, the pulling liquid may be contained in a plurality of containers and placed in the dip coater 2, in which case, each row (column) of micro-electrodes fixed in the jig 1 may be dip-pulled in the pulling liquid in one container, or each micro-electrode fixed in the jig 1 may be dip-pulled in the pulling liquid in a corresponding one container.

In addition, in some examples, in step S40, the composition of the gas in the atmosphere shield may be the same as the solvent of the film solution. In this case, it is possible to suppress an increase in the concentration of the film solution due to volatilization of the solvent, that is, it is possible to reduce a variation in the concentration of the pulling liquid during the dip pulling. For example, in some examples, the solvent may be ethanol and the component of the atmosphere may be ethanol.

In addition, in the present embodiment, the saturation of the gas may be 90% to 100% in step S40. In this case, the gas can effectively suppress volatilization of the solution, and thus the concentration of the drawing liquid can be maintained during the dipping and drawing.

Additionally, in some examples, the saturation of the atmosphere may be 90% as preferred; more preferably, the saturation of the atmosphere may be 95%; more preferably, the saturation of the atmosphere may be 96%; more preferably, the saturation of the atmosphere may be 97%; more preferably, the saturation of the atmosphere may be 98%; more preferably, the saturation of the atmosphere may be 99%; more preferably, the saturation of the atmosphere may be 99.5%; more preferably, the saturation of the atmosphere may be 99.8%; more preferably, the saturation of the atmosphere may be 99.9%; most preferably, the saturation of the atmosphere may be 100%.

In this embodiment, the microelectrode may be cured in a vacuum environment in step S50. This makes it possible to prevent the film from being contaminated. In addition, in some examples, the micro-electrodes may be placed in a vacuum environment to be cured for 20 to 30 hours in step S50. This enables the film to be more favorably condensed on the surface of the microelectrode.

In some examples, the microelectrode may be placed in a vacuum environment to cure for 24 hours. In other examples, the microelectrode may be placed in a vacuum environment to cure for 22 hours. In addition, in still other examples, the microelectrodes may be cured for 26 hours in a vacuum environment. Additionally, in some examples, the vacuum environment may be a vacuum box, a vacuum house, or the like.

In addition, in the present embodiment, the thickness of the thin film after the plating of the surface of the micro-electrode is completed may be 50nm to 50 μm. For example, in some examples, the thickness of the film after the micro-electrode surface coating is completed may be 50 μm. In other examples, the thickness of the film after the micro-electrode surface coating is completed may be 50 nm. In addition, in some examples, the thickness of the film after the plating of the surface of the micro-electrode is completed may be 100nm, 500nm, 800nm, 1 μm, 2 μm, 5 μm, 10 μm, 20 μm, 30 μm, 40 μm, or 45 μm.

While the present disclosure has been described in detail above with reference to the drawings and the embodiments, it should be understood that the above description does not limit the present disclosure in any way. Those skilled in the art can make modifications and variations to the present disclosure as needed without departing from the true spirit and scope of the disclosure, which fall within the scope of the disclosure.

Claims

1. A method for coating a film on the surface of a micro electrode is characterized by comprising the following steps:

the method comprises the following steps:

(a) preparing a microelectrode to be coated;

(b) fixing the micro-electrode;

(c) preparing a membrane solution and a cross-linking agent, and mixing to obtain a pulling liquid, wherein the viscosity of the pulling liquid is 0.1-20 cP;

(d) immersing and pulling the microelectrode from the pulling liquid in a preset program under the atmosphere protection, wherein the composition of gas in the atmosphere protection is the same as the solvent of the membrane solution; and is

(e) And placing the microelectrode in a vacuum environment for curing.

2. The method of claim 1, wherein:

the predetermined program includes a pulling step of dipping the microelectrodes into the pulling liquid at a dipping rate of 2mm/s to 8mm/s for a dipping time of 1s to 60s, followed by pulling the microelectrodes out of the pulling liquid at a pulling rate of 2mm/s to 8 mm/s.

3. The method of claim 2, wherein:

the predetermined procedure further comprises repeating the pulling step at least 1 time, and when the number of repetitions is more than 5 times, decreasing the pulling rate in the pulling step from 6 th.

4. The method of claim 1, wherein:

in step (d), the gas has a saturation of 90% to 100%.

5. The method of claim 1, wherein:

the solute of the membrane solution is selected from poly-4-vinylpyridine and poly-4-vinylpyridine-SO₃The solvent is at least one of ethanol, water, tetrahydrofuran, acetone, ethyl acetate, diethyl ether, turpentine, mineral solvent and volatile oil.

6. The method of claim 1, wherein:

the crosslinking agent is at least one selected from polyethylene glycol dimethyl ether, polyethylene glycol, boric acid, adipic acid dihydrazide, polyacrylic amine and polyisocyanate.

7. The method of claim 1, wherein:

the concentration of the membrane solution is 1mg/ml to 150 mg/ml.

8. The method of claim 1, wherein:

in the pulling liquid, the addition amount of the cross-linking agent is 1mg/ml to 25 mg/ml.

9. The method of claim 1, wherein:

in the step (a), the microelectrode is washed by the ethanol for 1 to 10min and then by the deionized water for 1 to 10 min.

10. The method of claim 1, wherein:

in step (e), the microelectrode is cured in a vacuum environment for 20 to 30 hours.