Method for coating microelectrode surfaces
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- SHENZHEN SIBIONICS CO LTD
- Filing Date
- 2019-09-30
- Publication Date
- 2026-06-23
Smart Images
Figure CN112570230B_ABST
Abstract
Description
Technical Field
[0001] This disclosure specifically relates to a method for coating a microelectrode surface. Background Technology
[0002] Commonly used liquid phase coating techniques include brush coating, dip-coating, and spray coating. The dip-coating method involves immersing a cleaned substrate in a pre-prepared solution, then smoothly pulling the substrate out of the solution at a precisely controlled, uniform speed. Under the influence of viscosity and gravity, a uniform liquid film forms on the substrate surface. As the solvent rapidly evaporates, the solution adhering to the substrate surface quickly gels to form a gel film. The dip-coating method is a commonly used thin film preparation method. It can be used to coat uniform films onto fabric substrates and base films, and is widely applied to the formation of films from sol-gels, solutions, and suspensions.
[0003] Dip-coating has been widely used because it offers higher coating quality than brush coating and has the advantages of simpler and cheaper equipment compared to spray coating.
[0004] In mass production of coatings, for coating technologies such as sol-gel and slurry methods that are applied in the liquid phase, ensuring the consistency and uniformity of the coating thickness and preventing cracking failure during drying are the key challenges and difficulties. Meanwhile, for dip-coating methods, reducing coating inhomogeneity caused by the sagging effect of the coating solution is also crucial for improving coating quality. Summary of the Invention
[0005] This disclosure was made in view of the above-mentioned state of the prior art, and its purpose is to provide a method for coating a microelectrode surface that can improve film consistency, make the film thickness uniform and the appearance smooth.
[0006] Therefore, this disclosure provides a method for coating a microelectrode surface, characterized by comprising: (a) preparing a microelectrode to be coated; (b) fixing the microelectrode; (c) preparing a film solution and a crosslinking agent, mixing them to obtain a lifting liquid, the viscosity of the lifting liquid being 0.1 to 20 cP; (d) immersing and pulling the microelectrode from the lifting liquid in a predetermined procedure under a protective atmosphere, wherein the composition of the gas in the protective atmosphere is the same as the solvent of the film solution; and (e) placing the microelectrode in a vacuum environment for curing.
[0007] In the method of dip-coating microelectrode surface of the present disclosure, the microelectrode is fixed, and then a film solution of appropriate concentration is prepared and mixed with an appropriate amount of crosslinking agent to obtain a dipping liquid with a viscosity of 0.1 to 20 cP. The microelectrode is then dipped and dipped. During the dip-coating process, the dipping liquid is protected by an atmosphere, and the composition of the atmosphere is the same as the solvent of the film solution. Under these conditions, the concentration of the film solution can be suppressed due to the evaporation of the solvent by the atmosphere protection, thereby reducing the viscosity change of the dipping liquid and thus reducing the sagging effect. Therefore, the uniformity and consistency of the coating thickness of the film on the surface of the microelectrode can be improved. As a result, the film on the surface of the microelectrode has good consistency, uniform thickness and smooth appearance.
[0008] Additionally, in the method disclosed herein, optionally, the predetermined procedure includes immersing the microelectrode in the lifting liquid at an immersion rate of 2 mm / s to 8 mm / s for an immersion time of 1 s to 60 s, followed by a lifting step of removing the microelectrode from the lifting liquid at a lifting rate of 2 mm / s to 8 mm / s. This allows a thin film of a certain thickness to be formed on the surface of the microelectrode.
[0009] Additionally, in the method disclosed herein, optionally, the predetermined procedure further includes repeating the lifting step at least once, and when the number of repetitions exceeds five, reducing the lifting rate in the lifting step from the sixth repetition onwards. This allows for the formation of a multilayer thin film, resulting in a smoother microelectrode surface and more stable performance.
[0010] Furthermore, in the method disclosed herein, in step (d), the saturation of the gas can be 90% to 100%. In this case, the gas can effectively suppress the evaporation of the solution, thereby maintaining the concentration of the lifting liquid during the immersion lifting process.
[0011] Additionally, in the methods disclosed herein, optionally, the solute of the membrane solution is selected from at least one of poly(4-vinylpyridine), poly(4-vinylpyridine-SO3), polyvinylpyrrolidone, polyurethane, polypropylene, polyethylene oxide, polyvinyl alcohol, polyacrylate, and polyacrylic acid, and the solvent is selected from at least one of ethanol, water, tetrahydrofuran, acetone, ethyl acetate, diethyl ether, turpentine, mineral solvents, and volatile oils. In this case, the membrane solution can have one or more different solutes, thereby allowing for the selection of different solutes as needed.
[0012] Additionally, in the methods disclosed herein, optionally, the crosslinking agent is selected from at least one of polyethylene glycol dimethyl ether, polyethylene glycol, boric acid, dihydrazine adipic acid, polyacrylamide, and polyisocyanate. This improves the tensile strength, water resistance, and viscosity of the film.
[0013] Furthermore, in the methods disclosed herein, the concentration of the membrane solution can be from 1 mg / ml to 150 mg / ml. Therefore, a membrane solution of suitable viscosity can be selected as needed.
[0014] Furthermore, in the method disclosed herein, the amount of crosslinking agent added to the lifting liquid can be from 1 mg / ml to 25 mg / ml. This improves both the tensile strength and water resistance of the film, while also creating a lifting liquid with a suitable viscosity.
[0015] Additionally, in the method disclosed herein, optionally, in step (a), the microelectrode is cleaned with ethanol for 1 to 10 minutes, and then cleaned with deionized water for 1 to 10 minutes. This removes foreign matter from the surface of the microelectrode, facilitating the formation of a smooth film.
[0016] Additionally, in the method disclosed herein, optionally, in step (e), the microelectrode is placed in a vacuum environment for curing for 20 to 30 hours. This allows for better condensation of the thin film on the surface of the microelectrode.
[0017] According to this disclosure, a method for coating a microelectrode surface can be provided that can improve film consistency, make the film thickness uniform and the appearance smooth. Attached Figure Description
[0018] Figure 1 A schematic flowchart of a method for coating a microelectrode surface according to an example of this disclosure is shown.
[0019] Figure 2 A perspective view of the dip-coating machine involved in the examples of this disclosure is shown.
[0020] Figure 3 A schematic diagram of the impregnation and lifting process involved in the examples of this disclosure is shown.
[0021] Figure 4 A three-dimensional schematic diagram of the fixture involved in the examples of this disclosure is shown.
[0022] Figure 5 A partial schematic diagram of a fixture involved in another example of this disclosure is shown. Detailed Implementation
[0023] Hereinafter, preferred embodiments of the present disclosure will be described in detail with reference to the accompanying drawings. In the following description, the same reference numerals are used for the same components, and repeated descriptions are omitted. Furthermore, the drawings are merely schematic diagrams, and the proportions of the components or the shapes of the components may differ from actual figures.
[0024] Figure 1A schematic flowchart of a method for coating a microelectrode surface according to an example of this disclosure is shown. Figure 3 A schematic diagram of the impregnation and lifting process involved in the examples of this disclosure is shown.
[0025] like Figure 1 As shown, the method for coating a microelectrode surface according to this embodiment may include: preparing a microelectrode to be coated (step S10); fixing the microelectrode (step S20); preparing a film solution and a crosslinking agent, mixing them to obtain a lifting liquid, the viscosity of which may be 0.1 to 20 cP (step S30); immersing and pulling the microelectrode from the lifting liquid in a predetermined procedure under a protective atmosphere, wherein the composition of the gas in the protective atmosphere is the same as the solvent of the film solution (step S40); and placing the microelectrode in a vacuum environment for curing (step S50).
[0026] In the microelectrode surface coating method of this embodiment, the microelectrode is fixed, and then a film solution of appropriate concentration is prepared and mixed with an appropriate amount of crosslinking agent to obtain a lifting liquid with a viscosity of 0.1 to 20 cP. The microelectrode is then immersed and lifted. During the immersion and lifting process, the lifting liquid is protected by an atmosphere, and the composition of the atmosphere is the same as the solvent of the film solution. Under these circumstances, the concentration of the film solution can be suppressed due to solvent evaporation by the atmosphere protection, thereby reducing the viscosity change of the lifting liquid and reducing the sagging effect. Therefore, the uniformity and consistency of the coating thickness of the film on the surface of the microelectrode can be improved. Thus, the film on the surface of the microelectrode has good consistency, uniform thickness and smooth appearance.
[0027] In this embodiment, the microelectrode can be coated with a film on its surface by dip-coating. For example... Figure 3 As shown, the dip-coating process can involve immersing the part to be coated into a solution and then pulling it out of the solution. Under the influence of viscosity and gravity, and with the evaporation of the solvent, the solution adhering to the surface of the part to be coated forms a thin film.
[0028] In this embodiment, the microelectrode to be coated can be prepared in step S10. Additionally, in some examples, the prepared microelectrode to be coated can be cleaned in step S10. In other examples, in step (a), the microelectrode can be cleaned with ethanol for 1 to 10 minutes, followed by cleaning with deionized water for 1 to 10 minutes. This removes foreign matter from the surface of the microelectrode, facilitating the formation of a smooth film. For example, the microelectrode can be cleaned with ethanol for 1 minute, followed by cleaning with deionized water for 5 minutes.
[0029] In some examples, the microelectrode can be cleaned with ethanol for 5 minutes, followed by rinsing with deionized water for 1 minute. In other examples, the microelectrode can be cleaned with ethanol for 10 minutes, followed by rinsing with deionized water for 10 minutes, and so on.
[0030] Furthermore, in this embodiment, the surface roughness of the microelectrode in step S10 can be from 0.01 μm to 10 μm. This facilitates the formation of a thin film of the lifting liquid on the microelectrode surface.
[0031] In some examples, the surface roughness of the microelectrode can be 0.01 μm. In other examples, the surface roughness of the microelectrode can be 10 μm. Additionally, in some examples, the surface roughness of the microelectrode can 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.
[0032] In this embodiment, the material of the microelectrode is not particularly limited and can be selected according to actual needs. In some examples, the microelectrode can be made of biosafe materials. Therefore, it can be implanted or used in the human body.
[0033] In some examples, the microelectrode can be made of a metallic material. Additionally, in some examples, the microelectrode can be made of at least one of platinum, nickel, cobalt, titanium, tantalum, niobium, and zirconium. For example, the microelectrode can be made of metallic platinum, metallic niobium, or a nickel-cobalt alloy.
[0034] In this embodiment, the shape of the microelectrode is not particularly limited and can be selected according to actual needs. For example, the microelectrode can be needle-shaped, sheet-shaped, etc.
[0035] In some examples, the microelectrode can be attached to a pad. Additionally, in some examples, the pad can be circular or polygonal. In other examples, the microelectrode and the pad can be different sizes. For example, the pad can be wider than the microelectrode. Furthermore, the microelectrode and the pad can be integrally formed. In some examples, the microelectrode can be a thin electrode sheet attached to a pad. In other examples, the microelectrode can include a pad.
[0036] In addition, in this embodiment, the microelectrode is fixed in step S20. Specifically, the microelectrode obtained in step S10 can be assembled onto the coating fixture 1 and fixed to obtain the coating to be applied.
[0037] The fixture 1 used in step 20 of this embodiment will be described in detail below with reference to the illustrations.
[0038] Figure 2 A perspective view of the dip-coating machine 2 involved in the example of this disclosure is shown. Figure 4 A perspective view of jig 1, as described in the examples of this disclosure, is shown, wherein Figure 4 (a) shows a perspective view of the jig 1 involved in the example of this disclosure. Figure 4 (b) shows a schematic diagram of the structure of the connecting part 30 involved in the example of this disclosure. Figure 4 (c) shows a schematic diagram of the structure of the loading section 10 involved in the example of this disclosure. Figure 4 (d) shows a schematic diagram of the structure of the cover plate 20 involved in the example of this disclosure.
[0039] In this embodiment, such as Figure 4 As shown, the coating fixture 1 (hereinafter sometimes referred to as "fixture 1") may include a loading section 10 and a cover plate 20. In some examples, the loading section 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 microelectrodes are arranged side-by-side on the first loading surface 11, and the positioning grooves 111 penetrate the bottom surface in a direction parallel to the first loading surface 11. Additionally, in some examples, the cover plate 20 cooperates with the first loading surface 11 of the loading section 10 to fix the microelectrodes located in the positioning grooves 111.
[0040] In the coating fixture 1 of this embodiment, the first loading surface 11 of the loading section 10 has a plurality of positioning grooves 111 arranged side by side for placing microelectrodes. In this case, the fixture 1 can place multiple microelectrodes simultaneously, and the positions of the microelectrodes fixed on the fixture 1 are consistent. Therefore, the state of the microelectrodes before coating is relatively consistent, thereby improving the consistency of the coating. In addition, in some examples, the fixture 1 has a cover plate 20 that mates with the first loading surface 11 of the loading section 10. In this case, the microelectrodes can be better fixed, which is beneficial to improving the coating quality. Thus, a coating fixture 1 that can both perform batch coating and improve the consistency of the coating can be provided.
[0041] In some examples, the fixture 1 may also include a connecting portion 30. Additionally, the end of the loading portion 10 furthest from the positioning groove 111 may mate with the connecting portion 30. In this case, the fixture 1 can be mounted on a coating machine via the connecting portion 30, thereby enabling the coating machine to control the fixture 1 to perform coating. Furthermore, the bottom surface of the loading portion 10 is furthest from the connecting portion 30.
[0042] Additionally, in some examples, such as Figure 4As shown in (b), the connecting part 30 can be a combined structure. In this case, the connecting part 30 can both connect to the coating machine and fix the loading part 10 (described in detail later). In addition, in some examples, the connecting part 30 can be composed of plates. This facilitates the connection between the connecting part 30 and the coating machine. For example, in some examples, the connecting part 30 can be composed of a first plate 31 and a second plate 32.
[0043] Additionally, in some examples, such as Figure 4 As shown in (b), the first plate 31 may have a first type of fixing hole 311, and the second plate 32 may mate with the first type of fixing hole 311. In some examples, the first plate 31 and the second plate 32 may be fixed with screws. In other examples, the connecting part 30 may be composed of a plate and a cylinder. In addition, in some examples, the connecting part 30 may be integrally formed.
[0044] In some examples, the first plate 31 may have a plurality of first-type fixing holes 311. Additionally, 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.
[0045] Additionally, in some examples, such as Figure 4 As shown in (b), the connecting portion 30 may have a groove 321 that mates with the loading portion 10. In some examples, the connecting portion 30 may have multiple grooves 321 that mate with the loading portion 10. For example, the connecting portion 30 may have 2 to 8 grooves 321 that mate with the loading portion 10. In addition, in some examples, the connecting portion 30 may have 1, 2, 3, 4, 5, 6, 7, or 8 grooves 321.
[0046] In some examples, the groove 321 may have a second type of fixing hole 322 for fixing the loading part 10, and the loading part 10 may cooperate with the second type of fixing hole 322.
[0047] In some examples, the groove 321 may have multiple second-type fixing holes 322. Additionally, 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 fixing holes 322. In other examples, multiple second-type fixing holes 322 may be located on the same horizontal line.
[0048] In some examples, the loading part 10 can be mounted to the connecting part 30 using a fixing mechanism. In this case, the loading part 10 can be mounted to the connecting part 30 well. In other examples, the fixing mechanism can be a snap-fit structure or a screw-fit structure. In this case, the loading part 10 can be more securely fixed to the connecting part 30. For example, in some examples, the loading part 10 can be mounted to the connecting part 30 using screws. In other examples, the loading part 10 can be mounted to the connecting part 30 using a snap-fit structure.
[0049] Additionally, in some examples, the connecting part 30 can be fixed to the coating machine using screws, snap-fit, or magnetic attraction. In this case, the coating fixture 1 can be fixed to the coating machine, allowing for subsequent and effective coating of the microelectrode by the coating machine. Furthermore, in some examples, the coating machine can be an dip-coating machine 2 (see...). Figure 2 In some examples, the connecting part 30 can be fixed to the dip-coating machine 2 by means of screws. In other examples, the connecting part 30 can be fixed to the dip-coating machine 2 by means of magnetic attraction.
[0050] Additionally, in some examples, such as Figure 4 As shown, the fixture 1 may have multiple plate-shaped loading portions 10. In this case, the plate-shaped loading portions 10 facilitate fixation to the cover plate 20, thereby enabling more microelectrodes to be well fixed in the fixture 1. In some examples, the fixture 1 may have 2 to 12 loading portions 10. For example, the fixture 1 may have 2, 4, 5, 6, 8, 10, or 12 loading portions 10. In other examples, the fixture 1 may also have only one loading portion 10.
[0051] In some examples, the loading section 10 may have a first loading surface 11. In other examples, the loading section 10 may also have a bottom surface that intersects with the first loading surface 11.
[0052] In some examples, such as Figure 4 As shown in (c), the loading unit 10 may have a positioning groove 111. Additionally, in some examples, the loading unit 10 may be provided with multiple positioning grooves 111. For example... Figure 4 As shown in (c), the first loading surface 11 may be provided with a plurality of positioning slots 111. In other examples, the plurality of positioning slots 111 may be arranged side by side on the first loading surface 11.
[0053] In some examples, the positioning groove 111 can be used to fix the microelectrode. In other examples, the microelectrode can be placed within the positioning groove 111. In still other examples, a pad that can be connected to the microelectrode is placed within the positioning groove 111. Thus, the microelectrode can be fixed by fixing the pad.
[0054] In some examples, a loading unit 10 may have 2, 4, 6, 8, 10, 12, 14, 16, 18, 20, 22, or 24 positioning slots 111. In other examples, a loading unit 10 may have 1 positioning slot 111.
[0055] In some examples, such as Figure 4 As shown in (c), the positioning groove 111 can penetrate the bottom surface in a direction parallel to the first loading surface 11. Additionally, in some examples, the shape of the positioning groove 111 can match the shape of the microelectrode. In other examples, the portion of the positioning groove 111 near the bottom surface can be larger than the portion farther from the bottom surface.
[0056] In some examples, the shape and depth of the positioning groove 111 can be approximately the same as the contact portion between the microelectrode and the cover plate 20 and the loading portion 10. This facilitates the fixation of the microelectrode. In other examples, the shape and depth of the positioning groove 111 can be slightly larger than the contact portion between the microelectrode and the cover plate 20 and the loading portion 10. In some examples, the orientation of the positioning groove 111 can be perpendicular to the bottom surface.
[0057] In some examples, the loading section 10 also includes a second loading surface (not shown) parallel to the first loading surface 11, with its bottom surface connecting the first loading surface 11 and the second loading surface. The edge of the cover plate 20 (described in detail later) does not extend beyond the bottom surface. This allows for the fixing of more microelectrodes while reducing interference to the microelectrodes during the coating process, thus improving the consistency of the microelectrode coating. In some examples, the edge of the cover plate 20 may be aligned with the bottom surface.
[0058] In some examples, the second loading surface is provided with a plurality of side-by-side positioning slots 111 for placing microelectrodes, just like the first loading surface 11. For example, in some examples, the first loading surface 11 of the loading part 10 may have 1, 2, 4, 6, 8, 10, 12, 14 or 16 positioning slots 111, and the second loading surface of the loading part 10 may have the same 1, 2, 4, 6, 8, 10, 12, 14 or 16 positioning slots 111.
[0059] Additionally, in some examples, the first loading surface 11 of the loading unit 10 may have a positioning groove 111, while the second loading surface of the loading unit 10 may not have a positioning groove 111. For example, the first loading surface 11 of the loading unit 10 may have 1, 3, 5, 7, 9, 11, 13, 15, or 16 positioning grooves 111, while the second loading surface of the loading unit 10 may not have a positioning groove 111.
[0060] In some examples, the second loading surface of the loading unit 10 may have a positioning groove 111, while the first loading surface 11 of the loading unit 10 may not have a positioning groove 111. For example, the second loading surface of the loading unit 10 may have 1, 3, 5, 7, 9, 11, 13, 15, or 16 positioning grooves 111, while the first loading surface 11 of the loading unit 10 may not have a positioning groove 111.
[0061] Additionally, in some examples, the jig 1 may also include a back plate 40 that mates with the second loading surface of the loading section 10, the edge of the back plate 40 not extending beyond the bottom surface. In this case, the microelectrodes placed in the second loading surface can be well secured. In some examples, the edge of the back plate 40 may be flush with the bottom surface. Furthermore, in some examples, the cover plate 20 may have the same structure as the back plate 40. This allows for better securing of more microelectrodes.
[0062] Additionally, in some examples, such as Figure 4 (c) and Figure 4 As shown in (d), the loading part 10 may have a third type of fixing hole 12, and the cover plate 20 (described in detail later) may have a fourth type of fixing hole 21 that mates with the third type of fixing hole 12. Thus, the cover plate 20 can be fixed to the loading part 10.
[0063] In some examples, the loading part 10 may have multiple third-type fixing holes 12. Additionally, in some examples, the loading part 10 may have 2 to 10 third-type fixing holes 12. For example, the loading part 10 may have 2, 3, 4, 5, 6, 7, 8, 9, or 10 third-type fixing holes 12. In other examples, the multiple third-type fixing holes 12 may be located on the same or different horizontal lines.
[0064] In some examples, the cover plate 20 may have multiple Class IV fixing holes 21. Additionally, in some examples, the cover plate 20 may have 2 to 10 Class IV fixing holes 21. For example, the cover plate 20 may have 2, 3, 4, 5, 6, 7, 8, 9, or 10 Class IV fixing holes 21. In other examples, the multiple Class IV fixing holes 21 may be located on the same or different horizontal lines.
[0065] In some examples, the cover plate 20 can mate with the loading part 10. In other words, the third type of fixing hole 12 can mate with the fourth type of fixing hole 21. Thus, the cover plate 20 can be fixed to the loading part 10. In other examples, the cover plate 20 can mate with the loading part 10 using a screw fixing method, a magnetic attraction method, or a snap-fit structure. In this case, the cover plate 20 can mate well with the loading part 10, thereby effectively fixing the microelectrode located in the positioning groove 111.
[0066] In some examples, the cover plate 20 can be engaged with the loading part 10 using screws. For example, the loading part 10 and the cover plate 20 can be fastened together via third-type fixing holes 12 and fourth-type fixing holes 21 using screws. In other examples, the cover plate 20 can be engaged with the loading part 10 using magnetic attraction. For example, the loading part 10 and the cover plate 20 can be secured together via third-type fixing holes 12 and fourth-type fixing holes 21 using magnets.
[0067] Additionally, in some examples, the cover plate 20 may mate with the first loading surface 11 of the loading portion 10 to secure the microelectrode located in the positioning groove 111. In some examples, the cover plate 20 may have a mating surface 22 that mates with the first loading surface 11.
[0068] Additionally, in some examples, the cover plate 20 may have a protrusion 221 that mates with the positioning groove 111. This allows for better fixation of the microelectrode. In some examples, the protrusion 221 may be provided on the mating surface 22 of the cover plate 20.
[0069] Additionally, in some examples, the protrusion 221 can be made of a flexible material. In this case, when the cover plate 20 engages with the positioning groove 111, the protrusion 221 can adaptably deform, thereby better securing the microelectrode. For example, in some examples, the protrusion 221 can be adhesive tape.
[0070] In some examples, the flexible material may be selected from at least one of silicone, rubber, poly(p-xylene), polyimide, polytetrafluoroethylene, and polyvinyl alcohol. This allows for further fixation of the microelectrode. For example, in some examples, the flexible material may be silicone. In other examples, the flexible material may be polyimide. Furthermore, in still other examples, the flexible material may be polyvinyl alcohol.
[0071] Additionally, in some examples, such as Figure 4 As shown in (d), the protrusion 221 on the cover plate 20 that mates with the positioning groove 111 can 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 on the cover plate 20 that mates with the positioning groove 111 can be discontinuous. For example, the cover plate 20 may have a silicone pad only at the position corresponding to the positioning groove 111.
[0072] In some examples, fixture 1 may not include connecting part 30, and loading part 10 may be directly fixed to dip-coating machine 2 by magnetic attraction.
[0073] Figure 5 A partial schematic diagram of fixture 1, as described in another example of this disclosure, is shown. Figure 5(a) shows a schematic diagram of the structure of the loading section 10A according to another example of this disclosure. Figure 5 (b) shows a structural schematic diagram of cover plate 20A according to another example of this disclosure.
[0074] In other examples, such as Figure 5 As shown, the fixture 1 may include a loading portion 10A and a cover plate 20A. In some examples, the fixture 1 may include a loading portion 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 portion 10A may be fixed by magnetic attraction or by screw fixing.
[0075] In some examples, such as Figure 5 As shown in (a), the loading part 10A may include a first type of limiting hole 13. Additionally, in some examples, such as... Figure 5 As shown in (b), the cover plate 20A may include a second type of limiting hole 23.
[0076] In some examples, the loading part 10A may include a plurality of first-type limiting holes 13, and the cover plate 20A may include a plurality of second-type limiting holes 23. Additionally, in some examples, the first-type limiting holes 13 may mate with the second-type limiting holes 23. This allows for auxiliary fixation of the microelectrode.
[0077] In some examples, the microelectrode may have a through-hole that mates with the first type of limiting hole 13 and the second type of limiting hole 23. In other examples, the microelectrode may have multiple through-holes. That is, each microelectrode may have multiple through-holes.
[0078] In some examples, the microelectrode may have 2 to 5 through holes. For example, the microelectrode may have 2, 3, 4 or 5 through holes. In other examples, the microelectrode may have 1 through hole.
[0079] In other examples, the pads may have through holes that mate with the first type of locating hole 13 and the second type of locating hole 23. In this case, if the pad is placed within the positioning groove 111, the pad can mate with the first type of locating hole 13 and the second type of locating hole 23 to fix the pad, thereby fixing the microelectrode. Additionally, in some examples, the pads may have multiple through holes; that is, each pad may have multiple through holes.
[0080] In other examples, the pads may have 2 to 5 vias. For example, the pads may have 2, 3, 4, or 5 vias. Additionally, in some examples, the pads may have 1 via.
[0081] In some examples, fixture 1 may include multiple limiting posts (not shown). In other examples, the limiting posts may be cylindrical or prismatic. Additionally, the diameter of the limiting posts may be slightly smaller than the diameter of the first type of limiting hole 13 and the second type of limiting hole 23.
[0082] In some examples, the limiting post can penetrate the first type of limiting hole 13, the second type of limiting hole 23, and the through hole. Additionally, in some examples, the microelectrode can be mounted on the fixture 1 through the first type of limiting hole 13, the second type of limiting hole 23, the through hole, and the limiting post.
[0083] In some examples, each locating post can pass through both the first type of locating hole 13 and the second type of locating hole 23 to secure the microelectrode. In other examples, each locating post can pass through only a portion of the first type of locating hole 13 and a portion of the second type of locating hole 23 to secure the microelectrode.
[0084] Additionally, in some examples, the fixture 1 may also have a pressure plate (not shown). Furthermore, the pressure plate may have the same structure as the cover plate 20A. For example, the pressure plate may have a third type of limiting hole (not shown) that mates with the first type of limiting hole 13. Additionally, the pressure plate may mate with the second surface of the loading section 10A.
[0085] In some examples, each limiting post can 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 microelectrodes. In other examples, each limiting post can penetrate the first type of limiting hole 13 and extend into the second type of limiting hole 23 and the third type of limiting hole to fix two microelectrodes.
[0086] In addition, in some examples, among the mating first type limiting hole 13, second type limiting hole 23 and third type limiting hole, there may be a limiting post that passes through the first type limiting hole 13 and extends into the second type limiting hole 23 to fix the microelectrode, and another limiting post that passes through the first type limiting hole 13 and extends into the third type limiting hole to fix another microelectrode.
[0087] In addition, in some examples, fixture 1 can hold 1 to 200 microelectrodes. In this case, it is convenient to coat multiple microelectrodes in batches simultaneously, and the pre-coating state of the microelectrodes within and between batches can be relatively consistent, thereby enabling good consistency of the thin films formed by the microelectrodes within and between batches.
[0088] Furthermore, in this embodiment, in step S20, each microelectrode can be fixed in a substantially consistent position within the fixture 1. This improves the consistency of the clamping of each microelectrode before coating, thereby ensuring that the coating state of each microelectrode is consistent each time.
[0089] In some examples, the membrane solution can be prepared in step S30. Specifically, in step S30, the membrane solution can be prepared by dissolving the solute in a solvent. Furthermore, the concentration of the membrane solution can be from 1 mg / ml to 150 mg / ml. Thus, a membrane solution with a suitable viscosity can be selected as needed.
[0090] In some examples, the concentration of the membrane solution can be 64 mg / ml. In other examples, the concentration of the membrane solution can be 150 mg / ml. Additionally, in some examples, the concentration of the membrane solution can be 1 mg / ml, 5 mg / ml, 10 mg / ml, 20 mg / ml, 40 mg / ml, 60 mg / ml, 70 mg / ml, 80 mg / ml, 100 mg / ml, 120 mg / ml, or 140 mg / ml.
[0091] Furthermore, in this embodiment, in step S30, the solute of the membrane solution can be selected from at least one of poly(4-vinylpyridine) (P4VP), poly(4-vinylpyridine-SO3) (P4VP-SO3), polyvinylpyrrolidone (PVP), polyurethane (PU), polypropylene (PP), polyethylene oxide (PEO), polyvinyl alcohol (PVA), polyacrylate (PEA), and polyacrylic acid (PAA). In this case, the membrane solution can have one or more different solutes, thereby allowing different solutes to be selected as needed.
[0092] In some examples, the solute of the membrane solution can be poly(4-vinylpyridine-SO3). In other examples, the solute of the membrane solution can be polyethylene oxide. Furthermore, in still other examples, the solute of the membrane solution can be polyvinylpyrrolidone.
[0093] In this embodiment, in step S30, the solvent can be selected from ethanol and water, thereby effectively dissolving the solute to form a film solution. Furthermore, since the solvent is volatile, it facilitates the generation of a protective atmosphere and promotes film drying. For example, in some examples, the solvent can be ethanol. In other examples, the solvent can be tetrahydrofuran. Additionally, in some examples, the solvent can be a mixture of ethanol and water.
[0094] In this embodiment, the crosslinking agent can be mixed with the membrane solution in step S30 to obtain the lifting liquid. Specifically, in step S30, the lifting liquid can be formed by adding the crosslinking agent to the prepared membrane solution and mixing. Furthermore, the viscosity of the lifting liquid can be from 0.1 to 20 cP. This allows a thin film to be formed on the surface of the microelectrode.
[0095] In some examples, the viscosity of the lifting fluid can be 0.1 cP. In other examples, the viscosity of the lifting fluid can be 20 cP. Additionally, in some examples, the viscosity of the lifting fluid can be 0.2 cP, 0.5 cP, 1 cP, 2 cP, 5 cP, 8 cP, 10 cP, 12 cP, 15 cP, or 18 cP.
[0096] In some examples, in step S30, the crosslinking agent may be selected from at least one of polyethylene glycol dimethyl ether, polyethylene glycol, boric acid, dihydrazine adipic acid, polyacrylamide, and polyisocyanate. This improves the tensile strength, water resistance, and viscosity of the film. For example, in some examples, the crosslinking agent may be polyethylene glycol dimethyl ether. In other examples, the crosslinking agent may be dihydrazine adipic acid. Furthermore, in still other examples, the crosslinking agent may be polyethylene glycol.
[0097] Furthermore, in this embodiment, in step S30, the amount of crosslinking agent added to the lifting liquid can be from 1 mg / ml to 25 mg / ml. This improves both the tensile strength and water resistance of the film while also creating a lifting liquid with a suitable viscosity. For example, in some examples, the amount of crosslinking agent added can be 6 mg / ml. In other examples, the amount of crosslinking agent added can be 25 mg / ml. In still other examples, the amount of crosslinking agent added can be 1 mg / ml, 2 mg / ml, 5 mg / ml, 7 mg / ml, 10 mg / ml, 12 mg / ml, 15 mg / ml, 20 mg / ml, or 22 mg / ml.
[0098] Additionally, in some examples, the crosslinking agent can be a solid. In other examples, the crosslinking agent can be a crosslinking agent solution. In some examples, the solvent of the crosslinking agent solution can be the same as the solvent of the membrane solution.
[0099] In some examples, in step S40, the microelectrode can be immersed and pulled under a protective atmosphere. In other examples, in step S40, the microelectrode can be immersed and pulled out of the pulling liquid according to a predetermined procedure under a protective atmosphere.
[0100] Additionally, in some examples, step S40 may include a lifting step in which the microelectrode is immersed in the lifting liquid at an immersion rate of 2 mm / s to 8 mm / s for an immersion time of 1 s to 60 s, followed by a lifting step in which the microelectrode is removed from the lifting liquid at a lifting rate of 2 mm / s to 8 mm / s. This allows a thin film of a certain thickness to be formed on the surface of the microelectrode.
[0101] In some examples, the immersion rate, pull-up rate, and immersion time can affect the film thickness. In other examples, appropriate immersion rates, pull-up rates, and immersion times can be selected based on actual needs.
[0102] In some examples, the predetermined procedure may include immersing the microelectrode in the lifting solution at an immersion rate of 6 mm / s for 5 s, and then withdrawing it from the lifting solution at a lifting rate of 6 mm / s.
[0103] In some examples, the parameters for the lifting step can be: descent rate 4 mm / s, lifting rate 4 mm / s, and immersion time 8 s. In other examples, the parameters can be: descent rate 5 mm / s, lifting rate 5 mm / s, and immersion time 12 s. In still other examples, the parameters can be: descent rate 7 mm / s, lifting rate 7 mm / s, and immersion time 15 s.
[0104] In some examples, step S40 may further include repeating the lifting step at least once. This allows for the formation of a multilayer film, resulting in a smoother microelectrode surface and more stable performance. Additionally, in some examples, when the number of repetitions exceeds five, the lifting rate in the lifting step can be reduced from the sixth repetition onwards. In this case, since the uniformity of the coating decreases with increasing lifting rate, reducing the lifting rate on top of the multilayer film allows for a more uniform film formation on the microelectrode surface, thus improving the consistency of the film on the microelectrode.
[0105] In some examples, the predetermined procedure may include repeating the lifting step 1 to 30 times. For example, the lifting step may be repeated 1 time, 5 times, 6 times, 8 times, 10 times, 12 times, 15 times, 20 times, 25 times, or 30 times. In some examples, the number of repetitions may be selected based on the required thickness of the microelectrode surface.
[0106] In some examples, when repeating the first to fifth lifting steps, the microelectrode can be immersed in the lifting solution at an immersion rate of 6 mm / s for 5 seconds, and then pulled out of the lifting solution at a lifting rate of 6 mm / s; when repeating the sixth to tenth lifting steps, the microelectrode can be immersed in the lifting solution at an immersion rate of 6 mm / s for 5 seconds, and then pulled out of the lifting solution at a lifting rate of 3 mm / s.
[0107] In some examples, when repeating the first to fifth lifting steps, the microelectrode can be immersed in the lifting liquid at an immersion rate of 8 mm / s for 4 seconds, and then pulled out of the lifting liquid at a lifting rate of 6 mm / s; when repeating the sixth to fifteenth lifting steps, the microelectrode can be immersed in the lifting liquid at an immersion rate of 6 mm / s for 4 seconds, and then pulled out of the lifting liquid at a lifting rate of 2 mm / s.
[0108] In some examples, when the number of repetitions exceeds 5, the parameters of the lifting step can be adjusted from the 6th repetition onwards, depending on actual needs. For example, the immersion rate can be increased, or the immersion time can be extended.
[0109] Additionally, in some examples, the predetermined procedure in step S40 can be performed by the dip-coating machine 2. This allows for efficient dip-coating. Furthermore, in some examples, the dip-coating machine 2 can have a device for forming a protective atmosphere. This allows step S40 to be performed under a protected atmosphere. For example, in some examples, the dip-coating machine 2 can have a sealed cavity for dip-coating.
[0110] Additionally, in some examples, step S40 may include fixing the film to be coated in the dip-coating machine 2. In this case, it is possible to better dip-coat a batch of microelectrodes.
[0111] Additionally, in some examples, step S40 may include placing the lifting solution prepared in step S30 into a sealable cavity for immersion lifting in the immersion lifting coating machine 2. In other examples, the lifting solution may be placed in a single container within the immersion lifting coating machine 2, in which case all microelectrodes fixed in the fixture 1 can be immersed and lifted in the lifting solution within one container. In still other examples, the lifting solution may be placed in multiple containers within the immersion lifting coating machine 2, in which case each row (column) of microelectrodes fixed in the fixture 1 can be immersed and lifted in the lifting solution within one container, or each microelectrode fixed in the fixture 1 can be immersed and lifted in the lifting solution within its corresponding container.
[0112] Additionally, in some examples, in step S40, the composition of the gas in the protective atmosphere can be the same as the solvent of the membrane solution. In this case, it is possible to suppress the increase in the concentration of the membrane solution due to solvent evaporation, i.e., to reduce the concentration change of the lifting liquid during the immersion lifting process. For example, in some examples, the solvent can be ethanol, and the composition of the atmosphere can be ethanol.
[0113] Furthermore, in this embodiment, the gas saturation in step S40 can be 90% to 100%. In this case, the gas can effectively suppress the evaporation of the solution, thereby maintaining the concentration of the lifting liquid during the immersion lifting process.
[0114] In addition, in some examples, preferably, the atmosphere saturation can be 90%; more preferably, the atmosphere saturation can be 95%; more preferably, the atmosphere saturation can be 96%; more preferably, the atmosphere saturation can be 97%; more preferably, the atmosphere saturation can be 98%; more preferably, the atmosphere saturation can be 99%; more preferably, the atmosphere saturation can be 99.5%; more preferably, the atmosphere saturation can be 99.8%; more preferably, the atmosphere saturation can be 99.9%; and most preferably, the atmosphere saturation can be 100%.
[0115] In this embodiment, the microelectrode can be cured in a vacuum environment during step S50. This makes the film less susceptible to contamination. Additionally, in some examples, the microelectrode can be cured in a vacuum environment for 20 to 30 hours during step S50. This allows for better film deposition on the microelectrode surface.
[0116] In some examples, the microelectrodes can be cured in a vacuum environment for 24 hours. In other examples, the microelectrodes can be cured in a vacuum environment for 22 hours. Furthermore, in still other examples, the microelectrodes can be cured in a vacuum environment for 26 hours. Additionally, in some examples, the vacuum environment can be a vacuum chamber, vacuum room, etc.
[0117] Furthermore, in this embodiment, the thickness of the thin film after coating the microelectrode surface can be from 50 nm to 50 μm. For example, in some examples, the thickness of the thin film after coating the microelectrode surface can be 50 μm. In other examples, the thickness of the thin film after coating the microelectrode surface can be 50 nm. In still other examples, the thickness of the thin film after coating the microelectrode surface can be 100 nm, 500 nm, 800 nm, 1 μm, 2 μm, 5 μm, 10 μm, 20 μm, 30 μm, 40 μm, or 45 μm.
[0118] According to this disclosure, a method for coating a microelectrode surface can be provided that can improve film consistency, make the film thickness uniform and the appearance smooth.
[0119] While the present disclosure has been specifically described above in conjunction with the accompanying drawings and embodiments, it is to 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 its essential spirit and scope, and all such modifications and variations fall within the scope of the present disclosure.
Claims
1. A method for depositing a film on the surface of a batch of microelectrodes, characterized in that: It consists of the following steps: (a) Prepare multiple microelectrodes to be coated; (b) Fixing a plurality of the microelectrodes to a coating fixture to obtain a coating assembly, wherein the fixture includes a loading portion, a cover plate, and a connecting portion; the loading portion has a first loading surface and a bottom surface intersecting the first loading surface; a plurality of positioning grooves for placing the microelectrodes are arranged side by side on the first loading surface, the positioning grooves ensuring that the microelectrodes are consistently positioned on the fixture; the positioning grooves penetrate the bottom surface in a direction parallel to the first loading surface; the cover plate engages with the first loading surface of the loading portion to fix the microelectrodes located in the positioning grooves; the cover plate has protrusions that engage with the positioning grooves for fixing the microelectrodes; the connecting portion engages with one end of the loading portion away from the positioning grooves and is used to fix the loading portion and connect to a coating machine; the connecting portion has a plurality of grooves that engage with the loading portion; (c) Prepare a membrane solution and a crosslinking agent, mix them to obtain a lifting liquid, and place the lifting liquid in a sealable cavity for immersion lifting of an immersion lifting coating machine. The viscosity of the lifting liquid is 0.1 to 20 cP. (d) The assembly to be coated is fixed in the dip-coating machine, and under a protective atmosphere, the dip-coating machine dips and pulls multiple microelectrodes in the assembly from the lifting liquid according to a predetermined program. The composition of the gas in the protective atmosphere is the same as the solvent of the film solution. The predetermined program includes: immersing the microelectrodes into the lifting liquid at an immersion rate of 2 mm / s to 8 mm / s for an immersion time of 1 s to 60 s, followed by a pulling step of removing the microelectrodes from the lifting liquid at a pulling rate of 2 mm / s to 8 mm / s, and repeating the pulling step at least once. When the number of repetitions is greater than 5, the pulling rate in the pulling step is reduced from the 6th time onwards; and (e) The plurality of said microelectrodes are cured in a vacuum environment.
2. The method as described in claim 1, characterized in that: In step (d), the gas saturation is 90% to 100%.
3. The method as described in claim 1, characterized in that: The solute of the membrane solution is selected from at least one of poly(4-vinylpyridine), polyvinylpyrrolidone, polyurethane, polypropylene, polyethylene oxide, polyvinyl alcohol, polyacrylate, and polyacrylic acid, and the solvent is selected from at least one of ethanol, water, tetrahydrofuran, acetone, ethyl acetate, diethyl ether, and turpentine.
4. The method as described in claim 1, characterized in that: The crosslinking agent is selected from at least one of polyethylene glycol dimethyl ether, polyethylene glycol, boric acid, dihydrazine adipic acid, polyacrylamide, and polyisocyanate.
5. The method as described in claim 1, characterized in that: The concentration of the membrane solution is from 1 mg / ml to 150 mg / ml.
6. The method as described in claim 1, characterized in that: In the lifting liquid, the amount of crosslinking agent added is from 1 mg / ml to 25 mg / ml.
7. The method as described in claim 1, characterized in that: In step (a), the microelectrode is cleaned with ethanol for 1 to 10 minutes and then with deionized water for 1 to 10 minutes.
8. The method as described in claim 1, characterized in that: In step (e), the microelectrode is placed in a vacuum environment for curing for 20 to 30 hours.