Graphene oxide-perfluorocarboxylic acid composite film and preparation method thereof, liquid lens
By preparing a graphene oxide-perfluorocarboxylic acid composite film, the instability problem of liquid lenses under electric fields or high-temperature environments was solved, thereby improving the stability and reliability of the lenses.
Patent Information
- Application Number
- CN202211631020.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-12-19
- Publication Date
- 2026-01-02
- Estimated Expiration
- 2042-12-19
AI Technical Summary
Liquid lenses are unstable in electric fields or high-temperature environments. The insulating liquid may deform or shift, causing changes in the interface between the two liquid phases and affecting the stability and reliability of the lens.
A graphene oxide-perfluorocarboxylic acid composite membrane was prepared by means of dispersion, pH adjustment, standing and drying operations to prepare a graphene oxide-perfluorocarboxylic acid composite membrane suitable for liquid lenses, which is used to confine two-phase liquids and maintain interface stability.
It significantly improves the stability and reliability of liquid lenses under electric field or high temperature environments, overcoming the defect of unstable performance.
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Figure CN115980895B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the technical field of liquid lens preparation and relates to a graphene oxide-perfluorocarboxylic acid composite film and a preparation method thereof and a liquid lens. BACKGROUND
[0002] The liquid lens based on the electrowetting phenomenon generally comprises two mutually insoluble isodense liquids, namely a conductive liquid and an insulating liquid, the two-phase liquid is kept in contact and forms a meniscus interface, under the action of an external electric field, the surface energy of the insulating layer or the hydrophobic layer changes, the wettability of the conductive liquid and the insulating liquid changes, thereby causing the meniscus to change, and finally realizing the variable focal length effect. Generally, the two-phase liquid interface continuously and stably changes under the action of an electric field, thereby ensuring the reliability of the cyclic use of the liquid lens.
[0003] At present, the liquid lens still has instability factors, especially in an electric field environment or a high-temperature state, due to the violent shaking or thermal motion of the liquid, the insulating liquid may be deformed or displaced, deviating from the set position of the insulating layer or the hydrophobic layer, so that the interface of the two-phase liquid changes, thereby causing the instability of the performance of the liquid lens. Therefore, in order to prevent the large displacement of the insulating liquid from causing the misplacement or separation of the liquid drops, a graphene oxide-perfluorocarboxylic acid composite film is needed to be designed to confine the two-phase liquid and keep the position of the two-phase liquid from changing, thereby further improving the stability and reliability of the liquid lens. SUMMARY
[0004] In view of the deficiencies in the prior art, the purpose of the present application is to provide a graphene oxide-perfluorocarboxylic acid composite film and a preparation method thereof and a liquid lens. In the present application, the preparation method mainly comprises dispersion, pH adjustment, standing and drying operations, the overall operation is simple, the process is short, and the method is especially suitable for the preparation of liquid lens materials. Moreover, the prepared graphene oxide-perfluorocarboxylic acid composite film is applied to the liquid lens, thereby overcoming the instability defect of the performance of the liquid lens in an electric field or a high-temperature environment, and significantly improving the stability and reliability of the liquid lens.
[0005] To achieve the above purpose, the technical scheme adopted by the present application is as follows:
[0006] In a first aspect, the present application provides a preparation method of a graphene oxide-perfluorocarboxylic acid composite film, which comprises the following steps:
[0007] The graphene oxide and the perfluorocarboxylic acid are mixed and then dispersed to obtain a composite suspension, the pH value of the composite suspension is adjusted, and the graphene oxide-perfluorocarboxylic acid composite film is obtained through standing treatment and drying treatment.
[0008] In the present application, the preparation method provided mainly includes dispersing, adjusting pH, standing and drying operations, the overall operation is simple, the process is short, and the method is especially suitable for the preparation of liquid lens materials, and the prepared graphene oxide-perfluorocarboxylic acid composite film is applied to the liquid lens, the performance instability defect of the liquid lens under an electric field or a high temperature environment is overcome, and the stability and reliability of the liquid lens are significantly improved.
[0009] As a preferred technical solution of the present application, the mass ratio of the graphene oxide and the perfluorocarboxylic acid is 1:(1-5), for example, can be 1:1, 1:2, 1:3, 1:4, 1:5, but is not limited to the listed values, and other values not listed in the range are also applicable; preferably 1:(2-4).
[0010] The present application limits the mass ratio of the graphene oxide and the perfluorocarboxylic acid to 1:(1-5), because the quality and functionality of the film layer are considered, too little perfluorocarboxylic acid reduces the affinity to polar liquid, that is, the water drop angle increases and the oil drop angle decreases; too much perfluorocarboxylic acid makes the film layer not easy to form and not uniform.
[0011] Preferably, the standing treatment time is 2-5 min, for example, can be 2 min, 2.5 min, 3 min, 3.5 min, 4 min, 4.5 min, 5 min, but is not limited to the listed values, and other values not listed in the range are also applicable.
[0012] The present application limits the standing treatment time to 2-5 min, because on the one hand it can save time, and on the other hand it can achieve the deposition effect; too long waste time, and too short suspension cannot uniformly complete deposition.
[0013] Preferably, the drying is carried out in an oven.
[0014] Preferably, the drying treatment temperature is 80-100 DEG C, for example, can be 80 DEG C, 82 DEG C, 84 DEG C, 86 DEG C, 88 DEG C, 90 DEG C, 92 DEG C, 94 DEG C, 96 DEG C, 98 DEG C, 100 DEG C, but is not limited to the listed values, and other values not listed in the range are also applicable.
[0015] The present application limits the drying treatment temperature to 80-100 DEG C, because too low temperature prolongs the drying time, and too high temperature may cause film layer cracking and reduce uniformity.
[0016] Preferably, the drying treatment time is 20-40 min, for example, can be 20 min, 22 min, 24 min, 26 min, 28 min, 30 min, 32 min, 34 min, 36 min, 38 min, 40 min, but not limited to the listed values, other values not listed in the range is also applicable.
[0017] The present application limits the drying treatment time to 20-40 min, because too short time cannot be dried, too long waste time.
[0018] As a preferred technical solution of the present application, the perfluorocarboxylic acid is any one or a combination of two or more of perfluorononanoic acid, perfluorooctanoic acid, perfluorooctanoic acid or perfluorodecanoic acid, preferably perfluorooctanoic acid.
[0019] As a preferred technical solution of the present application, the dispersion method is stirring and / or ultrasonic.
[0020] Preferably, a dispersant is added during the dispersion process.
[0021] Preferably, the suspension is prepared as follows:
[0022] The graphene oxide and perfluorocarboxylic acid are mixed and a dispersant is added, and then stirred and / or ultrasonic to obtain the composite suspension.
[0023] As a preferred technical solution of the present application, the dispersant includes water and ethanol.
[0024] Preferably, the volume ratio of the water and ethanol added is 1:(1-4), for example, can be 1:1, 1:2, 1:3, 1:4, but not limited to the listed values, other values not listed in the range is also applicable; wherein, preferably 1:1.
[0025] The present application limits the volume ratio of the water and ethanol added to 1:(1-4), because this volume ratio is the appropriate dispersion solvent ratio, if not in the range, the solution cannot be uniformly dispersed, further leading to poor film uniformity and not dense.
[0026] Preferably, the stirring time is 5-10 min, for example, can be 5 min, 6 min, 7 min, 8 min, 9 min, 10 min, but not limited to the listed values, other values not listed in the range is also applicable.
[0027] Preferably, the ultrasonic uses an ultrasonic cleaner.
[0028] Preferably, the power of the ultrasonic is 200-220w, for example, can be 200w, 202w, 204w, 206w, 208w, 210w, 212w, 214w, 216w, 218w, 220w, but not limited to the listed values, the values within the range of the values not listed are also applicable.
[0029] Preferably, the time of the ultrasonic is 20-40min, for example, can be 20min, 22min, 24min, 26min, 28min, 30min, 32min, 34min, 36min, 38min, 40min, but not limited to the listed values, the values within the range of the values not listed are also applicable.
[0030] As a preferred technical solution of the present application, the pH value of the composite suspension is adjusted according to the following mode:
[0031] An alkali solution is added to the composite suspension to adjust the pH value of the composite suspension.
[0032] As a preferred technical solution of the present application, the alkali solution is any one or a combination of at least two or more of sodium hydroxide solution, calcium hydroxide solution or ammonia water, preferably calcium hydroxide.
[0033] Preferably, the concentration of the alkali solution is 1-2mM, for example, can be 1mM, 1.1mM, 1.2mM, 1.3mM, 1.4mM, 1.5mM, 1.6mM, 1.7mM, 1.8mM, 1.9mM, 2mM, but not limited to the listed values, the values within the range of the values not listed are also applicable.
[0034] The present application limits the concentration of the alkali solution to 1-2mM, because when the concentration is too small, the amount of alkali solution required is large and the operation time is prolonged; when the concentration is too large, it is easy to cause excessive pH adjustment.
[0035] Preferably, the pH value is 9-12, for example, can be 9, 9.5, 10, 10.5, 11, 11.5, 12, but not limited to the listed values, the values within the range of the values not listed are also applicable.
[0036] The present application limits the pH value to 9-12, because in this pH range, the film layer is easy to adhere to the glass to form a firm film layer.
[0037] Exemplarily, the preparation method of the graphene oxide-perfluorocarboxylic acid composite film in the present application specifically comprises:
[0038] The graphene oxide and the perfluorocarboxylic acid are mixed and then dispersed to obtain a composite suspension, the pH value of the composite suspension is adjusted, and the graphene oxide-perfluorocarboxylic acid composite film is obtained through standing treatment and drying treatment.
[0039] The mass ratio of the graphene oxide to the perfluorocarboxylic acid is 1: (1-5), the standing treatment is performed for 2-5 min, the drying is performed in an oven, the drying treatment is performed at a temperature of 80-100°C, and the drying treatment is performed for 20-40 min. The perfluorocarboxylic acid is any one or a combination of two or more of perfluorononanoic acid, perfluorooctanoic acid, perfluorosuberic acid, or perfluorodecanoic acid.
[0040] The dispersion is specifically performed in the following manner: the graphene oxide and the perfluorocarboxylic acid are mixed, a dispersant is added, and the mixture is dispersed through stirring or ultrasonic treatment to obtain a composite suspension; the dispersant includes water and ethanol, the volume ratio of the added amounts of the water and the ethanol is 1: (1-4), the stirring is performed for 5-10 min, the ultrasonic treatment is performed at a power of 200-220 w for 20-40 min.
[0041] The adjustment of the pH value of the composite suspension is specifically performed in the following manner: an alkali solution is added to the composite suspension to adjust the pH value of the composite suspension; the alkali solution is any one or a combination of two or more of a sodium hydroxide solution, a calcium hydroxide solution, or ammonia water, the concentration of the alkali solution is 1-2 mM, and the pH value is 9-12.
[0042] In a second aspect, the present application provides a graphene oxide-perfluorocarboxylic acid composite film, which is prepared by the method of the first aspect.
[0043] Preferably, the water contact angle of the graphene oxide-perfluorocarboxylic acid composite film is less than 40°, for example, 39.8°, 39°, 38°, 37°, 30°, 20°, 10°, 8°, 6°, 4°, etc., but is not limited to the listed values, and other values not listed in the range are also applicable.
[0044] Preferably, the oil contact angle of the graphene oxide-perfluorocarboxylic acid composite film is greater than 110°, for example, 111°, 112°, 113°, 114°, 115°, 116°, 120°, 150°, 160°, etc., but is not limited to the listed values, and other values not listed in the range are also applicable.
[0045] It should be noted that the graphene oxide-perfluorocarboxylic acid composite film in the application has good hydrophilic and oleophobic characteristics, is coated on the inner surface of the upper transparent substrate, and limits the insulation liquid and the conductive liquid, thereby overcoming the performance instability defect of the liquid lens in an electric field or a high temperature environment, and significantly improving the stability and reliability of the liquid lens.
[0046] In a third aspect, the application provides a liquid lens, comprising a first substrate, a second substrate, an upper electrode and a lower electrode, the upper electrode comprises a first upper electrode and a second upper electrode arranged symmetrically, the first upper electrode and the second upper electrode are arranged with the first substrate therebetween, the lower electrode comprises a first lower electrode and a second lower electrode arranged symmetrically, the first lower electrode and the second lower electrode are arranged with the second substrate therebetween, the first substrate, the second substrate, the upper electrode and the lower electrode surround to form a cavity, the cavity is used for injecting liquid, and the first substrate is arranged with the graphene oxide-perfluorocarboxylic acid composite film of the second aspect on the side close to the liquid.
[0047] As a preferred technical solution of the application, the graphene oxide-perfluorocarboxylic acid composite film is arranged on one side surface of the first substrate.
[0048] Preferably, the coating thickness of the graphene oxide-perfluorocarboxylic acid composite film is 50-100 nm, for example, it can be 50 nm, 55 nm, 60 nm, 65 nm, 70 nm, 75 nm, 80 nm, 85 nm, 90 nm, 95 nm or 100 nm, but is not limited to the listed values, and other values not listed in the range are also applicable.
[0049] The application limits the coating thickness of the graphene oxide-perfluorocarboxylic acid composite film to 50-100 nm, because if the coating thickness is too thin, it is difficult to form a complete film layer, and the uniformity of the film layer cannot be guaranteed; and if the coating thickness is too thick, it may affect the light transmittance.
[0050] Compared with the prior art, the application has the following beneficial effects:
[0051] In the application, the preparation method mainly includes dispersion, pH adjustment, standing and drying operations, and the overall operation is simple and the process is short, which is especially suitable for the preparation of liquid lens materials, and the graphene oxide-perfluorocarboxylic acid composite film prepared by the method is applied to a liquid lens, thereby overcoming the performance instability defect of the liquid lens in an electric field or a high temperature environment, and significantly improving the stability and reliability of the liquid lens. BRIEF DESCRIPTION OF DRAWINGS
[0052] Figure 1 The structure schematic diagram of the liquid lens is provided for one specific embodiment of the application;
[0053] Wherein, 1-first substrate; 2-second substrate; 3-upper electrode; 4-lower electrode; 5-graphene oxide-perfluorocarboxylic acid composite film. DETAILED DESCRIPTION
[0054] The technical solutions of the present application are further illustrated below in conjunction with the drawings and through specific embodiments.
[0055] In one specific embodiment, the present application provides a preparation method of a graphene oxide-perfluorocarboxylic acid composite film 5, the preparation method comprising:
[0056] After mixing the graphene oxide and the perfluorocarboxylic acid, dispersion is performed to obtain a composite suspension, the pH value of the composite suspension is adjusted, and the graphene oxide-perfluorocarboxylic acid composite film 5 is obtained through standing treatment and drying treatment.
[0057] In the present application, the preparation method provided mainly comprises dispersion, pH adjustment, standing and drying operations, the overall operation is simple, the process is short, and the preparation method is particularly suitable for the preparation of liquid lens materials, and the graphene oxide-perfluorocarboxylic acid composite film 5 prepared is applied to a liquid lens, overcoming the performance instability defect of the liquid lens under an electric field or a high-temperature environment, and significantly improving the stability and reliability of the liquid lens.
[0058] The mass ratio of the graphene oxide and the perfluorocarboxylic acid is 1:(1-5), which can be 1:1, 1:2, 1:3, 1:4, 1:5, but is not limited to the listed values, and other values not listed in the range are also applicable; further, the mass ratio is 1:(2-4).
[0059] The standing treatment time is 2-5 min, which can be 2 min, 2.5 min, 3 min, 3.5 min, 4 min, 4.5 min, 5 min, but is not limited to the listed values, and other values not listed in the range are also applicable; the drying is performed in an oven, the drying treatment temperature is 80-100℃, which can be 80℃, 82℃, 84℃, 86℃, 88℃, 90℃, 92℃, 94℃, 96℃, 98℃, 100℃, but is not limited to the listed values, and other values not listed in the range are also applicable, and the drying treatment time is 20-40 min, which can be 20 min, 22 min, 24 min, 26 min, 28 min, 30 min, 32 min, 34 min, 36 min, 38 min, 40 min, but is not limited to the listed values, and other values not listed in the range are also applicable.
[0060] The perfluorocarboxylic acid is any one or a combination of two or more of perfluorononanoic acid, perfluorooctanoic acid, perfluorosuberic acid or perfluorodecanoic acid, and is further perfluorooctanoic acid.
[0061] The dispersing is specifically performed in the following manner: the graphene oxide and the perfluorocarboxylic acid are mixed, then a dispersant is added, and the dispersing is performed through stirring or ultrasonic to obtain a composite suspension.
[0062] The dispersant includes water and ethanol, and the volume ratio of the added amount of water to the added amount of ethanol is 1:(1-4), for example, can be 1:1, 1:2, 1:3, 1:4, but is not limited to the listed values, and other values not listed in the range are also applicable; and further, 1:1.
[0063] The stirring time is 5-10 min, for example, can be 5 min, 6 min, 7 min, 8 min, 9 min, 10 min, but is not limited to the listed values, and other values not listed in the range are also applicable; the ultrasonic power is 200-220 w, for example, can be 200 w, 202 w, 204 w, 206 w, 208 w, 210 w, 212 w, 214 w, 216 w, 218 w, 220 w, but is not limited to the listed values, and other values not listed in the range are also applicable; and the ultrasonic time is 20-40 min, for example, can be 20 min, 22 min, 24 min, 26 min, 28 min, 30 min, 32 min, 34 min, 36 min, 38 min, 40 min, but is not limited to the listed values, and other values not listed in the range are also applicable.
[0064] The pH value of the composite suspension is adjusted specifically in the following manner: an alkali solution is added to the composite suspension to adjust the pH value of the composite suspension.
[0065] The alkali solution is any one or a combination of at least two or more of a sodium hydroxide solution, a calcium hydroxide solution, or ammonia water, and further, the calcium hydroxide; the concentration of the alkali solution is 1-2 mM, for example, can be 1 mM, 1.1 mM, 1.2 mM, 1.3 mM, 1.4 mM, 1.5 mM, 1.6 mM, 1.7 mM, 1.8 mM, 1.9 mM, 2 mM, but is not limited to the listed values, and other values not listed in the range are also applicable; and the pH value is 9-12, for example, can be 9, 9.5, 10, 10.5, 11, 11.5, 12, but is not limited to the listed values, and other values not listed in the range are also applicable.
[0066] In another specific embodiment, the application provides a graphene oxide-perfluorocarboxylic acid composite film 5 prepared by the above preparation method.
[0067] The water contact angle of the graphene oxide-perfluorocarboxylic acid composite film 5 is less than 40°, for example, can be 39.8°, 39°, 38°, 37°, 30°, 20°, 10°, 8°, 6°, 4°, etc., but not limited to the listed values, and other values not listed in the value range are also applicable; the oil contact angle of the graphene oxide-perfluorocarboxylic acid composite film 5 is greater than 110°, for example, can be 111°, 112°, 113°, 114°, 115°, 116°, 120°, 150°, 160°, etc., but not limited to the listed values, and other values not listed in the value range are also applicable.
[0068] It should be noted that the graphene oxide-perfluorocarboxylic acid composite film 5 in the present application has good hydrophilic and oleophobic characteristics, which is coated on the inner surface of the upper transparent substrate to confine the insulating liquid and the conductive liquid, overcoming the performance instability of the liquid lens in an electric field or high temperature environment, and significantly improving the stability and reliability of the liquid lens.
[0069] In another specific embodiment, the present application provides a liquid lens, as shown in Figure 1 The liquid lens includes a first substrate 1, a second substrate 2, an upper electrode 3 and a lower electrode 4, the upper electrode 3 includes a first upper electrode and a second upper electrode arranged symmetrically, the first upper electrode and the second upper electrode are arranged with the first substrate 1 therebetween, the lower electrode 4 includes a first lower electrode and a second lower electrode arranged symmetrically, the first lower electrode and the second lower electrode are arranged with the second substrate 2 therebetween, the first substrate 1, the second substrate 2, the upper electrode and the lower electrode form a cavity therebetween, the cavity is used for injecting liquid, and the first substrate 1 is provided with the graphene oxide-perfluorocarboxylic acid composite film 5 on the side close to the liquid.
[0070] The graphene oxide-perfluorocarboxylic acid composite film 5 is arranged on one side surface of the first substrate 1, and the coating thickness of the graphene oxide-perfluorocarboxylic acid composite film 5 is 50-100 nm, for example, can be 50 nm, 55 nm, 60 nm, 65 nm, 70 nm, 75 nm, 80 nm, 85 nm, 90 nm, 95 nm, 100 nm, but not limited to the listed values, and other values not listed in the value range are also applicable.
[0071] Example 1
[0072] The present embodiment provides a preparation method of a graphene oxide-perfluorocarboxylic acid composite film 5, which specifically includes:
[0073] The graphene oxide and the perfluorocarboxylic acid are mixed and dispersed to obtain a composite suspension, the pH value of the composite suspension is adjusted, and the graphene oxide-perfluorocarboxylic acid composite film 5 is obtained through standing treatment and drying treatment.
[0074] The mass ratio of graphene oxide and perfluorocarboxylic acid is 1:1, the standing treatment time is 2 min, the drying is performed in an oven, the drying treatment temperature is 80°C, and the drying treatment time is 20 min. The perfluorocarboxylic acid is perfluorooctanoic acid.
[0075] The dispersion is specifically performed in the following manner: after the graphene oxide and the perfluorocarboxylic acid are mixed, a dispersant is added, and dispersion is performed through ultrasonic to obtain a composite suspension; the dispersant comprises water and ethanol, the volume ratio of the added amounts of water and ethanol is 1:1, the ultrasonic power is 200 w, and the ultrasonic time is 20 min.
[0076] The adjustment of the pH value of the composite suspension is specifically performed in the following manner: an alkali solution is added to the composite suspension to adjust the pH value of the composite suspension; the alkali solution is a calcium hydroxide solution, the concentration of the alkali solution is 1 mM, and the pH value is 9.
[0077] Example 2
[0078] The embodiment provides a preparation method of a graphene oxide-perfluorocarboxylic acid composite film 5, and specifically comprises the following steps:
[0079] The graphene oxide and the perfluorocarboxylic acid are mixed and then dispersed to obtain a composite suspension, the pH value of the composite suspension is adjusted, and the graphene oxide-perfluorocarboxylic acid composite film 5 is obtained through standing treatment and drying treatment.
[0080] The mass ratio of graphene oxide and perfluorocarboxylic acid is 1:2, the standing treatment time is 3 min, the drying is performed in an oven, the drying treatment temperature is 90°C, and the drying treatment time is 30 min. The perfluorocarboxylic acid is perfluorononanoic acid.
[0081] The dispersion is specifically performed in the following manner: after the graphene oxide and the perfluorocarboxylic acid are mixed, a dispersant is added, and dispersion is performed through ultrasonic to obtain a composite suspension; the dispersant comprises water and ethanol, the volume ratio of the added amounts of water and ethanol is 1:2, the ultrasonic power is 210 w, and the ultrasonic time is 30 min.
[0082] The adjustment of the pH value of the composite suspension is specifically performed in the following manner: an alkali solution is added to the composite suspension to adjust the pH value of the composite suspension; the alkali solution is a sodium hydroxide solution, the concentration of the alkali solution is 1.5 mM, and the pH value is 10.
[0083] Example 3
[0084] The embodiment provides a preparation method of a graphene oxide-perfluorocarboxylic acid composite film 5, and specifically comprises the following steps:
[0085] The graphene oxide and the perfluorocarboxylic acid are mixed and then dispersed to obtain a composite suspension, the pH value of the composite suspension is adjusted, and the graphene oxide-perfluorocarboxylic acid composite film 5 is obtained through standing treatment and drying treatment.
[0086] The mass ratio of graphene oxide and perfluorocarboxylic acid is 1:4, the standing treatment time is 5 min, the drying is performed in an oven, the drying treatment temperature is 100℃, and the drying treatment time is 40 min. The perfluorocarboxylic acid is perfluorooctanoic acid.
[0087] The dispersion is specifically performed in the following manner: after the graphene oxide and the perfluorocarboxylic acid are mixed, a dispersant is added, and dispersion is performed through ultrasonic, to obtain a composite suspension; the dispersant comprises water and ethanol, the volume ratio of the added amounts of water and ethanol is 1:4, the ultrasonic power is 220w, and the ultrasonic time is 40 min.
[0088] The adjustment of the pH value of the composite suspension is specifically performed in the following manner: an alkali solution is added to the composite suspension to adjust the pH value of the composite suspension; the alkali solution is ammonia water, the concentration of the alkali solution is 2mM, and the pH value is 11.
[0089] Example 4
[0090] The embodiment provides a preparation method of a graphene oxide-perfluorocarboxylic acid composite film 5, and specifically comprises the following steps.
[0091] The graphene oxide and the perfluorocarboxylic acid are mixed and then dispersed to obtain a composite suspension, the pH value of the composite suspension is adjusted, and the graphene oxide-perfluorocarboxylic acid composite film 5 is obtained through standing treatment and drying treatment.
[0092] The mass ratio of graphene oxide and perfluorocarboxylic acid is 1:5, the standing treatment time is 5 min, the drying is performed in an oven, the drying treatment temperature is 95℃, and the drying treatment time is 35 min. The perfluorocarboxylic acid is perfluorooctanoic acid.
[0093] The dispersion is specifically performed in the following manner: after the graphene oxide and the perfluorocarboxylic acid are mixed, a dispersant is added, and dispersion is performed through stirring, to obtain a flocculent composite suspension; the dispersant comprises water and ethanol, the volume ratio of the added amounts of water and ethanol is 1:2, and the stirring time is 8 min.
[0094] The adjustment of the pH value of the composite suspension is specifically performed in the following manner: an alkali solution is added to the composite suspension to adjust the pH value of the composite suspension; the alkali solution is a calcium hydroxide solution, the concentration of the alkali solution is 1.3mM, and the pH value is 12.
[0095] Example 5
[0096] The embodiment provides a preparation method of a graphene oxide-perfluorocarboxylic acid composite film 5, and different from example 1, the mass ratio of graphene oxide and perfluorocarboxylic acid is 1:0.8, and other parameters and test conditions are the same as those of example 1.
[0097] Example 6
[0098] The embodiment provides a preparation method of a graphene oxide-perfluorocarboxylic acid composite film 5, and different from example 1, a mass ratio of graphene oxide and perfluorocarboxylic acid is 1:6, and other parameters and test conditions are the same as those in example 1.
[0099] Example 7
[0100] The embodiment provides a preparation method of a graphene oxide-perfluorocarboxylic acid composite film 5, and different from example 1, a mass ratio of graphene oxide and perfluorocarboxylic acid is 1:6, and other parameters and test conditions are the same as those in example 1.
[0101] Example 8
[0102] The embodiment provides a preparation method of a graphene oxide-perfluorocarboxylic acid composite film 5, and different from example 1, a mass ratio of graphene oxide and perfluorocarboxylic acid is 1:6, and other parameters and test conditions are the same as those in example 1.
[0103] Comparative Example 1
[0104] The comparative example provides a preparation method of a graphene oxide-perfluorocarboxylic acid composite film 5, and different from example 1, no perfluorocarboxylic acid is used, and other parameters and test conditions are the same as those in example 1.
[0105] Comparative Example 2
[0106] The comparative example provides a preparation method of a graphene oxide-perfluorocarboxylic acid composite film 5, and different from example 1, no graphene oxide is used, and other parameters and test conditions are the same as those in example 1.
[0107] The first substrate 1 coated with the graphene oxide-perfluorocarboxylic acid composite film is subjected to water contact angle testing and oil contact angle testing by using a contact angle instrument, and test results are as shown in the following table 1.
[0108] Table 1
[0109]
[0110]
[0111] It is known from the above table 1 that:
[0112] Through comparison of example 1 and examples 5 and 6, it is known that the water contact angle in example 1 is smaller than that in examples 5 and 6, and the oil contact angle in example 1 is greater than that in examples 5 and 6, because the mass ratio of the graphene oxide and the perfluorocarboxylic acid is limited to 1:(1-5) in the application, so that the film layer is hydrophilic and oleophobic, and excellent performance is achieved.
[0113] By comparing example 1 and examples 7 and 8, it is found that the water contact angle in example 1 is smaller than that in examples 7 and 8, and the oil contact angle in example 1 is larger than that in examples 7 and 8, because the volume ratio of the water and the ethanol is limited to 1:(1-4) in the application, so that the dispersion liquid is uniformly dispersed and well deposited, and the hydrophilic and oleophobic effect is achieved.
[0114] By comparing example 1 and comparative examples 1 and 2, it is found that the water contact angle in example 1 is smaller than that in comparative examples 1 and 2, and the oil contact angle in example 1 is larger than that in comparative examples 1 and 2, because the film layer prepared by the perfluorocarboxylic acid and the graphene oxide together achieves the hydrophilic and oleophobic effect.
[0115] The above merely describes the specific embodiments of the present application, but the protection scope of the present application is not limited thereto, and those skilled in the art should understand that any changes or replacements within the technical scope disclosed by the present application can be easily thought of by those skilled in the art, and all fall within the protection scope and disclosure scope of the present application.
Claims
1. A method for preparing a graphene oxide-perfluorocarboxylic acid composite film, characterized by, The preparation method includes: Graphene oxide and perfluorocarboxylic acid are mixed and dispersed to obtain a composite suspension. The pH value of the composite suspension is adjusted, and the mixture is subjected to static treatment and drying treatment to obtain the graphene oxide-perfluorocarboxylic acid composite membrane. The mass ratio of graphene oxide to perfluorocarboxylic acid is 1:(1~5). A dispersant is also added during the dispersion process; the dispersant includes water and ethanol; the volume ratio of the added water and ethanol is 1:(1~4); The drying temperature is 80~100℃; The pH value of the composite suspension is adjusted in the following manner: An alkaline solution is added to the composite suspension to adjust the pH value of the composite suspension; The pH value is 9-12; The graphene oxide-perfluorocarboxylic acid composite membrane prepared by the method has a water contact angle of less than 40° and an oil contact angle of greater than 110°.
2. The production method according to claim 1, characterized by, The mass ratio of graphene oxide to perfluorocarboxylic acid is 1:(2~4).
3. The production method according to claim 1, characterized by, The settling time is 2-5 minutes.
4. The method of claim 1, wherein, The drying process is carried out in an oven.
5. The preparation method according to claim 1, characterized in that, The drying process takes 20 to 40 minutes.
6. The method of claim 1, wherein, The perfluorocarboxylic acid is any one or a combination of two or more of perfluorononanoic acid, perfluorooctanoic acid, perfluorooctanoic acid, or perfluorodecanoic acid.
7. The preparation method according to claim 6, characterized in that, The perfluorocarboxylic acid is perfluorooctanoic acid.
8. The method of claim 1, wherein, The dispersion method is stirring and / or ultrasonication.
9. The method of claim 1, wherein, The composite suspension is prepared in the following manner: The composite suspension is obtained by mixing graphene oxide and perfluorocarboxylic acid, adding a dispersant, and then stirring and / or sonicating.
10. The method of claim 1, wherein, The volume ratio of water to ethanol added is 1:
1.
11. The preparation method according to claim 8, characterized in that, The stirring time is 5-10 minutes.
12. The preparation method according to claim 8, characterized in that, The power of the ultrasound is 200~220w.
13. The preparation method according to claim 8, characterized in that, The ultrasound session lasted 20-40 minutes.
14. The method of claim 1, wherein, The alkaline solution is any one or a combination of at least two or more of sodium hydroxide solution, calcium hydroxide solution, or ammonia water.
15. The preparation method according to claim 14, characterized in that, The alkaline solution is calcium hydroxide.
16. The method of claim 1, wherein, The concentration of the alkaline solution is 1~2mM.
17. A graphene oxide-perfluorocarboxylic acid composite film, characterized by, The graphene oxide-perfluorocarboxylic acid composite membrane was prepared using the preparation method described in any one of claims 1-16.
18. The graphene oxide-perfluorocarboxylic acid composite film according to claim 17, wherein, The water contact angle of the graphene oxide-perfluorocarboxylic acid composite membrane is less than 40°.
19. The graphene oxide-perfluorocarboxylic acid composite film according to claim 17, wherein, The oil contact angle of the graphene oxide-perfluorocarboxylic acid composite film is greater than 110°.
20. A liquid lens characterized by The liquid lens includes a first substrate, a second substrate, an upper electrode, and a lower electrode. The upper electrode includes a first upper electrode and a second upper electrode arranged symmetrically, with a first substrate disposed between the first upper electrode and the second upper electrode. The lower electrode includes a first lower electrode and a second lower electrode arranged symmetrically, with a second substrate disposed between the first lower electrode and the second lower electrode. The first substrate, the second substrate, the upper electrode, and the lower electrode form a cavity for injecting liquid. The side of the first substrate closest to the liquid is provided with a graphene oxide-perfluorocarboxylic acid composite film as described in any one of claims 17-19.
21. The liquid lens of claim 20, wherein, The graphene oxide-perfluorocarboxylic acid composite film is coated on one side surface of the first substrate.
22. The liquid lens of claim 21, wherein, The coating thickness of the graphene oxide-perfluorocarboxylic acid composite film is 50~100nm.
Citation Information
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