A method and device for reducing graphene oxide

Reduced graphene oxide films were prepared by vacuum ball milling and porous silica reduction method, which solved the problems of low graphene production efficiency and poor retention capacity in the existing technology, and realized efficient preparation and large-scale production, making them suitable for heat dissipation materials for electronic devices.

CN118744986BActive Publication Date: 2025-01-24HUBEI HUAEN NEW MATERIAL CO LTD
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Patent Information

Application Number
CN202410742121.7
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-06-11
Publication Date
2025-01-24
Estimated Expiration
2044-06-11

AI Technical Summary

Technical Problem

Existing technologies are difficult to prepare graphene efficiently, especially reduced graphene oxide, resulting in low production efficiency, low yield and poor retention capacity, which limits the large-scale production and application of graphene.

Method used

Graphene oxidation was carried out by ball milling under vacuum conditions, combined with the reduction process of porous silica and acetone oxime. Reduced graphene oxide films were prepared by vacuum filtration and drying, which simplified the process and improved production efficiency and retention capacity.

Benefits of technology

Large-scale production and efficient preparation of graphene have been achieved, and the retention capacity of reduced graphene oxide has been significantly improved, making it suitable for heat dissipation materials and meeting the high thermal conductivity requirements of electronic devices.

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Abstract

The present invention relates to the field of graphene processing, and discloses a method and equipment for reducing graphene oxide, wherein a method for reducing graphene oxide comprises the following steps: S1: performing a first-stage ball milling of graphene under vacuum conditions to obtain graphene powder; S2: introducing an oxygen-containing atmosphere under vacuum conditions to perform a second-stage ball milling to obtain graphene oxide powder; S3: adding porous silica to the graphene oxide powder, stirring to form a mixture, and then adding deionized water to the mixture to obtain a mixed solution; S4: adding acetone oxime to the mixed solution, stirring to obtain a reduced graphene oxide solution; S5: taking the reduced graphene oxide solution, using a porous membrane as a support membrane, and forming a composite membrane on the support membrane by vacuum filtration. The present invention has the following advantages and effects: the preparation method is simple, the production efficiency is high, it is conducive to the large-scale production of graphene, and the prepared reduced graphene oxide has a good interception capacity.
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Description

Technical Field

[0001] The present invention relates to the technical field of graphene processing, and in particular to a method and equipment for reducing graphene oxide. Background Art

[0002] With the increasing requirements for the integration and miniaturization of electronic devices, the problem of heat accumulation has become increasingly prominent, seriously affecting the operating efficiency and service life of electronic equipment. Therefore, heat dissipation has become an important aspect for the further development of integrated circuits. In order to improve the heat dissipation performance of the device, the heat dissipation material should have the following properties: light, thin, high thermal conductivity, and low thermal resistance at the interface. Traditional heat dissipation materials for electronic devices, such as aluminum and copper, have high thermal conductivity. However, they are often required in large quantities, which makes the equipment bulky. Two-dimensional materials are generally considered to be ideal heat dissipation materials for miniaturized and integrated nanoelectronic devices due to their high inherent thermal conductivity.

[0003] In terms of heat dissipation applications, graphene is the most suitable two-dimensional material because of its ultra-high thermal conductivity and the ability of single / multilayer graphene to be directly used as a heat dissipation material. In particular, low-cost mass production of chemically oxidized graphene (GO) and reduced graphene oxide (RGO) flakes has been achieved; and both GO and RGO have many active oxygen groups, which are conducive to functionalization and adjustment of their properties. Although the thermal conductivity of RGO is lower than that of graphene prepared by mechanical exfoliation, its thermal conductivity can be adjusted. Theoretical analysis shows that the in-plane thermal conductivity of RGO can be further improved by adjusting the defect density of RGO at high temperature, which provides an opportunity to adjust the thermal conductivity of two-dimensional materials.

[0004] At present, the preparation methods of graphene include chemical vapor deposition, epitaxial growth, mechanical exfoliation and redox method. The graphene yield obtained by the first two methods is low, the process is complex, and the equipment is expensive, which is not conducive to the large-scale production of graphene. The production efficiency and output of the mechanical exfoliation method are low, which limit the production of graphene to a certain extent. In addition, the prepared reduced graphene oxide has poor interception capacity. Therefore, it is necessary to design a method and equipment for reducing graphene oxide to solve the above problems.

[0005] The information disclosed in this background technology section is only intended to enhance the understanding of the overall background of the invention and should not be regarded as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to a person skilled in the art. Summary of the invention

[0006] The object of the present invention is to provide a method and device for reducing graphene oxide to solve the above problems.

[0007] The above technical purpose of the present invention is achieved by the following technical solution: A method for reducing graphene oxide, comprising the following steps:

[0008] S1: ball milling the graphene in the first stage under vacuum conditions to obtain graphene powder;

[0009] S2: introducing an oxygen-containing atmosphere under vacuum conditions to perform a second stage of ball milling to obtain graphene oxide powder;

[0010] S3: adding porous silica to the graphene oxide powder, stirring to form a mixture, and then adding deionized water to the mixture to obtain a mixed solution;

[0011] S4: adding acetone oxime to the mixed solution, stirring and obtaining a reduced graphene oxide solution;

[0012] S5: taking a reduced graphene oxide solution, using a porous membrane as a support membrane, and forming a composite membrane on the support membrane by vacuum filtration;

[0013] S6: After the composite film is vacuum dried, the support film is removed to obtain a reduced graphene oxide film.

[0014] The present invention is further configured as follows: in the step S1, a ball mill is used to perform the first stage of ball milling, the ball milling time is set to 15-20 minutes, and after the graphene powder is obtained, the graphene powder is sieved.

[0015] The present invention is further configured as follows: in the step S2, a ball mill is used for the second stage of ball milling, the ball milling time is set to 30-40 minutes, and after the graphene oxide powder is obtained, the graphene oxide powder is sieved.

[0016] The present invention is further configured as follows: in the step S3, a stirrer is used to stir the porous silica and graphene oxide powders, the stirrer speed is 200-300 r / min, deionized water is added after stirring for 8-10 minutes, and after the deionized water is added, the stirrer speed is set to 800-900 r / min, and the stirring time is set to 12-15 minutes.

[0017] The present invention is further configured as follows: in step S4, a stirrer is used to stir the mixed solution and acetone oxime, the stirring temperature is set to 50-60° C., the stirring speed is set to 150-180 r / min, and the stirring time is set to 60-80 min.

[0018] The present invention is further configured as follows: in step S5, the reduced graphene oxide solution is poured into the porous membrane, and the vacuum degree in the vacuum container is controlled to be 30-100 kPa and maintained for 5-60 minutes.

[0019] The present invention is further configured as follows: in step S6, the drying temperature of the vacuum drying is set to 80-120° C., the drying time of the vacuum drying is set to 10-24 hours, and after the vacuum drying is completed, the support film is removed.

[0020] A device for reducing graphene oxide, comprising:

[0021] The first-stage ball milling unit is used to perform the first-stage ball milling of graphene under vacuum conditions to obtain graphene powder;

[0022] The second-stage ball milling unit is used to introduce an oxygen-containing atmosphere under vacuum conditions to perform the second-stage ball milling to obtain graphene oxide powder;

[0023] A first mixing unit is used to add porous silicon dioxide to graphene oxide powder, stir to form a mixture, and then add deionized water to the mixture to obtain a mixed solution;

[0024] A second mixing unit is used to add acetone oxime to the mixed solution, and obtain a reduced graphene oxide solution after stirring;

[0025] The composite membrane preparation unit is used to take a reduced graphene oxide solution, use a porous membrane as a support membrane, and form a composite membrane on the support membrane through vacuum filtration;

[0026] The reduced graphene oxide film preparation unit is used to vacuum dry the composite film and then remove the support film to obtain the reduced graphene oxide film.

[0027] The beneficial effects of the present invention are:

[0028] 1. The present invention ball-mills graphene under vacuum conditions, and then introduces an oxygen-containing atmosphere under vacuum conditions. During the ball-milling process, graphene can be fully contacted with oxygen, and an oxidation reaction is automatically performed on graphene. No oxidant needs to be added, so the preparation is relatively convenient, and the oxidation effect is relatively good. After oxidation, reduced graphene oxide can be prepared after reduction. The preparation method is simple, the production efficiency is high, and it is conducive to the large-scale production of graphene.

[0029] 2. The present invention prepares the prepared reduced graphene oxide into a film, and then detects the retention rate of the film, and it is concluded that the prepared reduced graphene oxide has good retention capacity. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the following briefly introduces the drawings required for use in the description of the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.

[0031] Figure 1 It is a schematic diagram of the structure of a device for reducing graphene oxide proposed in the present invention. DETAILED DESCRIPTION

[0032] The technical solution of the present invention will be clearly and completely described below in conjunction with specific embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0033] Example 1

[0034] The present invention provides a method for reducing graphene oxide, comprising the following steps:

[0035] S1: ball milling the graphene in the first stage under vacuum conditions to obtain graphene powder;

[0036] S2: introducing an oxygen-containing atmosphere under vacuum conditions to perform a second stage of ball milling to obtain graphene oxide powder;

[0037] S3: adding porous silica to the graphene oxide powder, stirring to form a mixture, and then adding deionized water to the mixture to obtain a mixed solution;

[0038] S4: adding acetone oxime to the mixed solution, stirring and obtaining a reduced graphene oxide solution;

[0039] S5: taking a reduced graphene oxide solution, using a porous membrane as a support membrane, and forming a composite membrane on the support membrane by vacuum filtration;

[0040] S6: After the composite film is vacuum dried, the support film is removed to obtain a reduced graphene oxide film.

[0041] Specifically, in step S1, a ball mill is used for the first stage of ball milling, and the ball milling time is set to 15 min. After obtaining the graphene powder, the graphene powder is sieved. In step S2, a ball mill is used for the second stage of ball milling, and the ball milling time is set to 30 min. After obtaining the graphene oxide powder, the graphene oxide powder is sieved. In step S3, a stirrer is used to stir the porous silica and graphene oxide powders, and the stirrer speed is 200 r / min. After stirring for 8 min, deionized water is added. After adding the deionized water, the stirrer speed is set to In step S4, the mixed solution and acetone oxime are stirred by a stirrer, the stirring temperature is set to 50°C, the stirrer speed is set to 150r / min, and the stirring time is set to 60min. In step S5, the reduced graphene oxide solution is poured into the porous membrane, and the vacuum degree in the vacuum container is controlled to be 30kPa and maintained for 5min. In step S6, the drying temperature of vacuum drying is set to 80°C, and the drying time of vacuum drying is set to 10h. After the vacuum drying is completed, the support membrane is removed.

[0042] See also Figure 1 The present invention also provides a device for reducing graphene oxide, comprising:

[0043] The first-stage ball milling unit is used to perform the first-stage ball milling of graphene under vacuum conditions to obtain graphene powder;

[0044] The second-stage ball milling unit is used to introduce an oxygen-containing atmosphere under vacuum conditions to perform the second-stage ball milling to obtain graphene oxide powder;

[0045] A first mixing unit is used to add porous silicon dioxide to graphene oxide powder, stir to form a mixture, and then add deionized water to the mixture to obtain a mixed solution;

[0046] A second mixing unit is used to add acetone oxime to the mixed solution, and obtain a reduced graphene oxide solution after stirring;

[0047] The composite membrane preparation unit is used to take a reduced graphene oxide solution, use a porous membrane as a support membrane, and form a composite membrane on the support membrane through vacuum filtration;

[0048] The reduced graphene oxide film preparation unit is used to vacuum dry the composite film and then remove the support film to obtain the reduced graphene oxide film.

[0049] Example 2

[0050] The present invention provides a method for reducing graphene oxide, comprising the following steps:

[0051] S1: ball milling the graphene in the first stage under vacuum conditions to obtain graphene powder;

[0052] S2: introducing an oxygen-containing atmosphere under vacuum conditions to perform a second stage of ball milling to obtain graphene oxide powder;

[0053] S3: adding porous silica to the graphene oxide powder, stirring to form a mixture, and then adding deionized water to the mixture to obtain a mixed solution;

[0054] S4: adding acetone oxime to the mixed solution, stirring and obtaining a reduced graphene oxide solution;

[0055] S5: taking a reduced graphene oxide solution, using a porous membrane as a support membrane, and forming a composite membrane on the support membrane by vacuum filtration;

[0056] S6: After the composite film is vacuum dried, the support film is removed to obtain a reduced graphene oxide film.

[0057] Specifically, in step S1, a ball mill is used for the first stage of ball milling, and the ball milling time is set to 16 min. After obtaining the graphene powder, the graphene powder is sieved. In step S2, a ball mill is used for the second stage of ball milling, and the ball milling time is set to 32 min. After obtaining the graphene oxide powder, the graphene oxide powder is sieved. In step S3, a stirrer is used to stir the porous silica and graphene oxide powders, and the stirrer speed is 220 r / min. After stirring for 8 min, deionized water is added. After adding the deionized water, the stirrer speed is set to In step S4, the mixed solution and acetone oxime are stirred by a stirrer, the stirring temperature is set to 52°C, the stirrer speed is set to 155r / min, and the stirring time is set to 65min. In step S5, the reduced graphene oxide solution is poured into the porous membrane, and the vacuum degree in the vacuum container is controlled to be 45kPa and maintained for 20min. In step S6, the drying temperature of vacuum drying is set to 90°C, and the drying time of vacuum drying is set to 12h. After the vacuum drying is completed, the support membrane is removed.

[0058] See also Figure 1 The present invention also provides a device for reducing graphene oxide, comprising:

[0059] The first-stage ball milling unit is used to perform the first-stage ball milling of graphene under vacuum conditions to obtain graphene powder;

[0060] The second-stage ball milling unit is used to introduce an oxygen-containing atmosphere under vacuum conditions to perform the second-stage ball milling to obtain graphene oxide powder;

[0061] A first mixing unit is used to add porous silicon dioxide to graphene oxide powder, stir to form a mixture, and then add deionized water to the mixture to obtain a mixed solution;

[0062] A second mixing unit is used to add acetone oxime to the mixed solution, and obtain a reduced graphene oxide solution after stirring;

[0063] The composite membrane preparation unit is used to take a reduced graphene oxide solution, use a porous membrane as a support membrane, and form a composite membrane on the support membrane through vacuum filtration;

[0064] The reduced graphene oxide film preparation unit is used to vacuum dry the composite film and then remove the support film to obtain the reduced graphene oxide film.

[0065] Example 3

[0066] The present invention provides a method for reducing graphene oxide, comprising the following steps:

[0067] S1: ball milling the graphene in the first stage under vacuum conditions to obtain graphene powder;

[0068] S2: introducing an oxygen-containing atmosphere under vacuum conditions to perform a second stage of ball milling to obtain graphene oxide powder;

[0069] S3: adding porous silica to the graphene oxide powder, stirring to form a mixture, and then adding deionized water to the mixture to obtain a mixed solution;

[0070] S4: adding acetone oxime to the mixed solution, stirring and obtaining a reduced graphene oxide solution;

[0071] S5: taking a reduced graphene oxide solution, using a porous membrane as a support membrane, and forming a composite membrane on the support membrane by vacuum filtration;

[0072] S6: After the composite film is vacuum dried, the support film is removed to obtain a reduced graphene oxide film.

[0073] Specifically, in step S1, a ball mill is used for the first stage of ball milling, and the ball milling time is set to 18 minutes. After obtaining the graphene powder, the graphene powder is sieved. In step S2, a ball mill is used for the second stage of ball milling, and the ball milling time is set to 36 minutes. After obtaining the graphene oxide powder, the graphene oxide powder is sieved. In step S3, a stirrer is used to stir the porous silica and the graphene oxide powder, and the stirrer speed is 260r / min. After stirring for 9 minutes, deionized water is added. After adding the deionized water, the stirrer speed is set to 860r / min, the stirring time is set to 13min, in step S4, the mixed solution and acetone oxime are stirred by a stirrer, the stirring temperature is set to 56°C, the stirrer speed is set to 170r / min, and the stirring time is set to 66min, in step S5, the reduced graphene oxide solution is poured into the porous membrane, the vacuum degree in the vacuum container is controlled to be 70kPa and maintained for 40min, in step S6, the drying temperature of vacuum drying is set to 100°C, the drying time of vacuum drying is set to 16h, and after the vacuum drying is completed, the support membrane is removed.

[0074] See also Figure 1 The present invention also provides a device for reducing graphene oxide, comprising:

[0075] The first-stage ball milling unit is used to perform the first-stage ball milling of graphene under vacuum conditions to obtain graphene powder;

[0076] The second-stage ball milling unit is used to introduce an oxygen-containing atmosphere under vacuum conditions to perform the second-stage ball milling to obtain graphene oxide powder;

[0077] A first mixing unit is used to add porous silicon dioxide to graphene oxide powder, stir to form a mixture, and then add deionized water to the mixture to obtain a mixed solution;

[0078] A second mixing unit is used to add acetone oxime to the mixed solution, and obtain a reduced graphene oxide solution after stirring;

[0079] The composite membrane preparation unit is used to take a reduced graphene oxide solution, use a porous membrane as a support membrane, and form a composite membrane on the support membrane through vacuum filtration;

[0080] The reduced graphene oxide film preparation unit is used to vacuum dry the composite film and then remove the support film to obtain the reduced graphene oxide film.

[0081] Example 4

[0082] The present invention provides a method for reducing graphene oxide, comprising the following steps:

[0083] S1: ball milling the graphene in the first stage under vacuum conditions to obtain graphene powder;

[0084] S2: introducing an oxygen-containing atmosphere under vacuum conditions to perform a second stage of ball milling to obtain graphene oxide powder;

[0085] S3: adding porous silica to the graphene oxide powder, stirring to form a mixture, and then adding deionized water to the mixture to obtain a mixed solution;

[0086] S4: adding acetone oxime to the mixed solution, stirring and obtaining a reduced graphene oxide solution;

[0087] S5: taking a reduced graphene oxide solution, using a porous membrane as a support membrane, and forming a composite membrane on the support membrane by vacuum filtration;

[0088] S6: After the composite film is vacuum dried, the support film is removed to obtain a reduced graphene oxide film.

[0089] Specifically, in step S1, a ball mill is used for the first stage of ball milling, and the ball milling time is set to 19 minutes. After obtaining the graphene powder, the graphene powder is sieved. In step S2, a ball mill is used for the second stage of ball milling, and the ball milling time is set to 38 minutes. After obtaining the graphene oxide powder, the graphene oxide powder is sieved. In step S3, a stirrer is used to stir the porous silica and the graphene oxide powder, and the stirrer speed is 280r / min. After stirring for 9 minutes, deionized water is added. After adding the deionized water, the stirrer speed is set to 880r / min, the stirring time is set to 14min, in step S4, the mixed solution and acetone oxime are stirred by a stirrer, the stirring temperature is set to 58°C, the stirrer speed is set to 175r / min, and the stirring time is set to 75min, in step S5, the reduced graphene oxide solution is poured into the porous membrane, the vacuum degree in the vacuum container is controlled to be 90kPa and maintained for 50min, in step S6, the drying temperature of vacuum drying is set to 110°C, the drying time of vacuum drying is set to 20h, and after the vacuum drying is completed, the support membrane is removed.

[0090] See also Figure 1 The present invention also provides a device for reducing graphene oxide, comprising:

[0091] The first-stage ball milling unit is used to perform the first-stage ball milling of graphene under vacuum conditions to obtain graphene powder;

[0092] The second-stage ball milling unit is used to introduce an oxygen-containing atmosphere under vacuum conditions to perform the second-stage ball milling to obtain graphene oxide powder;

[0093] A first mixing unit is used to add porous silicon dioxide to graphene oxide powder, stir to form a mixture, and then add deionized water to the mixture to obtain a mixed solution;

[0094] A second mixing unit is used to add acetone oxime to the mixed solution, and obtain a reduced graphene oxide solution after stirring;

[0095] The composite membrane preparation unit is used to take a reduced graphene oxide solution, use a porous membrane as a support membrane, and form a composite membrane on the support membrane through vacuum filtration;

[0096] The reduced graphene oxide film preparation unit is used to vacuum dry the composite film and then remove the support film to obtain the reduced graphene oxide film.

[0097] Example 5

[0098] The present invention provides a method for reducing graphene oxide, comprising the following steps:

[0099] S1: ball milling the graphene in the first stage under vacuum conditions to obtain graphene powder;

[0100] S2: introducing an oxygen-containing atmosphere under vacuum conditions to perform a second stage of ball milling to obtain graphene oxide powder;

[0101] S3: adding porous silica to the graphene oxide powder, stirring to form a mixture, and then adding deionized water to the mixture to obtain a mixed solution;

[0102] S4: adding acetone oxime to the mixed solution, stirring and obtaining a reduced graphene oxide solution;

[0103] S5: taking a reduced graphene oxide solution, using a porous membrane as a support membrane, and forming a composite membrane on the support membrane by vacuum filtration;

[0104] S6: After the composite film is vacuum dried, the support film is removed to obtain a reduced graphene oxide film.

[0105] Specifically, in step S1, a ball mill is used for the first stage of ball milling, and the ball milling time is set to 20 min. After obtaining the graphene powder, the graphene powder is sieved. In step S2, a ball mill is used for the second stage of ball milling, and the ball milling time is set to 40 min. After obtaining the graphene oxide powder, the graphene oxide powder is sieved. In step S3, a stirrer is used to stir the porous silica and graphene oxide powders, and the stirrer speed is 300 r / min. After stirring for 10 min, deionized water is added. After adding the deionized water, the stirrer speed is set to 900r / min, the stirring time is set to 15min. In step S4, the mixed solution and acetone oxime are stirred by a stirrer, the stirring temperature is set to 60°C, the stirrer speed is set to 180r / min, and the stirring time is set to 80min. In step S5, the reduced graphene oxide solution is poured into the porous membrane, and the vacuum degree in the vacuum container is controlled to be 100kPa and maintained for 60min. In step S6, the drying temperature of vacuum drying is set to 120°C, and the drying time of vacuum drying is set to 24h. After the vacuum drying is completed, the support membrane is removed.

[0106] See also Figure 1 The present invention also provides a device for reducing graphene oxide, comprising:

[0107] The first-stage ball milling unit is used to perform the first-stage ball milling of graphene under vacuum conditions to obtain graphene powder;

[0108] The second-stage ball milling unit is used to introduce an oxygen-containing atmosphere under vacuum conditions to perform the second-stage ball milling to obtain graphene oxide powder;

[0109] A first mixing unit is used to add porous silicon dioxide to graphene oxide powder, stir to form a mixture, and then add deionized water to the mixture to obtain a mixed solution;

[0110] A second mixing unit is used to add acetone oxime to the mixed solution, and obtain a reduced graphene oxide solution after stirring;

[0111] The composite membrane preparation unit is used to take a reduced graphene oxide solution, use a porous membrane as a support membrane, and form a composite membrane on the support membrane through vacuum filtration;

[0112] The reduced graphene oxide film preparation unit is used to vacuum dry the composite film and then remove the support film to obtain the reduced graphene oxide film.

[0113] The interception capacity of the prepared reduced graphene oxide film was tested, and the results are as follows:

[0114] Retention rate Example 1 99.2% Example 2 99.6% Example 3 99.4% Example 4 99.3% Example 5 99.2%

[0115] It can be seen from the above content that the prepared reduced graphene oxide has good interception ability, and Example 2 is the best example.

[0116] The above is a detailed introduction to a method and device for reducing graphene oxide provided by the present invention. Specific embodiments are used herein to illustrate the principles and implementation methods of the present invention. The description of the above embodiments is only used to help understand the method of the present invention and its core idea. It should be pointed out that for ordinary technicians in this technical field, without departing from the principle of the present invention, several improvements and modifications can be made to the present invention, and these improvements and modifications also fall within the scope of protection of the claims of the present invention.

Claims

1. A method for preparing a reduced graphene oxide film, characterized in that: The following steps are involved: S1: ball milling the graphene in the first stage under vacuum conditions to obtain graphene powder; S2: introducing an oxygen-containing atmosphere under vacuum conditions to perform a second stage of ball milling to obtain graphene oxide powder; S3: adding porous silica to the graphene oxide powder, stirring to form a mixture, and then adding deionized water to the mixture to obtain a mixed solution; S4: adding acetone oxime to the mixed solution, stirring to obtain a reduced graphene oxide solution; S5: taking the reduced graphene oxide solution, using the porous membrane as a support membrane, and forming a composite membrane on the support membrane by vacuum filtration; S6: After the composite film is vacuum dried, the support film is removed to obtain a reduced graphene oxide film; In the step S1, a ball mill is used to perform the first stage of ball milling, and the ball milling time is set to 15-20 minutes. After the graphene powder is obtained, the graphene powder is sieved; In the step S2, a ball mill is used for the second stage of ball milling, and the ball milling time is set to 30-40 minutes. After the graphene oxide powder is obtained, the graphene oxide powder is sieved; In the step S3, the porous silica and graphene oxide powders are stirred by a stirrer at a speed of 200-300 r / min. After stirring for 8-10 min, deionized water is added. After adding the deionized water, the stirrer speed is set to 800-900 r / min, and the stirring time is set to 12-15 min. In the step S4, a stirrer is used to stir the mixed solution and acetone oxime, the stirring temperature is set to 50-60° C., the stirring speed is set to 150-180 r / min, and the stirring time is set to 60-80 min.

2. The method for preparing a reduced graphene oxide film according to claim 1, characterized in that: In the step S5, the reduced graphene oxide solution is poured into the porous membrane, and the vacuum degree in the vacuum container is controlled to be 30-100 kPa and maintained for 5-60 minutes.

3. The method for preparing a reduced graphene oxide film according to claim 1, characterized in that: In the step S6, the drying temperature of the vacuum drying is set to 80-120° C., the drying time of the vacuum drying is set to 10-24 hours, and after the vacuum drying is completed, the support film is removed.

Citation Information

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