CN113903888B - Cross-linked reduced graphene oxide-based flexible self-supporting membrane electrode and rapid preparation method thereof - Google Patents

Cross-linked reduced graphene oxide-based flexible self-supporting membrane electrode and rapid preparation method thereof Download PDF

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CN113903888B
CN113903888B CN202111024316.0A CN202111024316A CN113903888B CN 113903888 B CN113903888 B CN 113903888B CN 202111024316 A CN202111024316 A CN 202111024316A CN 113903888 B CN113903888 B CN 113903888B
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graphene oxide
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reduced graphene
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CN113903888A (en
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刘治明
何燕
魏晴
王晓君
由杰
李慧芳
李海昌
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Qingdao University of Science and Technology
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Abstract

The invention belongs to the technical field of electrode material preparation, and particularly relates to a cross-linked reduced graphene oxide-based flexible self-supporting membrane electrode and a rapid preparation method thereof, wherein a high theoretical capacity material is uniformly mixed with a graphene oxide dispersion liquid, the mixed liquid is subjected to freeze drying to obtain a graphene oxide-based composite material, then the graphene oxide-based composite material is subjected to rapid cross-linking reduction treatment by using a hot ammonium sulfide solution at room temperature, and the cross-linked reduced graphene oxide-based flexible self-supporting membrane composite electrode is obtained after freeze drying again; the composite structure fully exerts the characteristics of high specific capacity among different components and excellent mechanical property and high conductivity of the reduced graphene oxide, and the prepared composite material can effectively buffer the volume expansion effect in the circulation process and has obvious advantages.

Description

Cross-linked reduced graphene oxide-based flexible self-supporting membrane electrode and rapid preparation method thereof
The technical field is as follows:
the invention belongs to the technical field of electrode material preparation, and particularly relates to a cross-linked reduced graphene oxide-based flexible self-supporting membrane electrode and a rapid preparation method thereof.
The background art comprises the following steps:
the information in this background section is disclosed only to enhance an understanding of the general background of the disclosure and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
In recent years, carbon-based composite materials have been widely studied and applied in electrode materials of energy storage devices due to advantages such as large specific surface area and good buffer characteristics. The graphene is used as an excellent self-buffering framework material, the three-dimensional self-buffering network constructed by the graphene can enable the material to have more active sites, high conductivity and high mechanical strength, and the graphene-based hybrid structure often shows the characteristics of capacity increase, speed improvement, stability improvement and the like in a lithium ion battery. The graphene oxide is subjected to reduction treatment, so that the graphene oxide has more excellent toughness and enhanced mechanical strength.
However, this build strategy is still in the infancy and still presents some challenges, limiting the practical application of graphene-based nanocomposites. The introduction of the carbon material increases the specific surface area, and at the same time, the side reaction between the electrolyte and the active material is increased, and the coulombic efficiency and the actual specific capacity of the first circle are reduced. Moreover, most of the composite materials are only limited to attaching the nano materials on the surface of the carbon-based material, and the volume expansion effect in the charge and discharge process cannot be effectively relieved.
In addition, the conventional methods for preparing the rGO-based composite material, such as a hydrothermal method, generally require complex high-temperature heating (generally 120-180 ℃ and 1-12 hours) and other processes, so that much time and energy consumption are required. The graphene-based composite membrane material obtained by the suction filtration method usually takes a long time, and graphene sheets are stacked seriously, so that the graphene-based composite membrane material has a poor three-dimensional network structure, and the ion diffusivity perpendicular to the membrane direction is poor, so that the rate performance in a battery test is greatly reduced. In addition, the conventional slurry coating method requires the addition of a conductive agent and a binder when preparing an electrode, which undoubtedly lowers the energy density of a battery, and thus a new electrode form is required to solve the above problems.
The invention content is as follows:
the invention aims to solve the technical problems that in the carbon-based composite material, the graphene oxide is subjected to reduction treatment so as to have better toughness and enhanced mechanical strength; however, the construction strategy is still in the initial stage, and some challenges still exist, which limit the practical application of the graphene-based nanocomposite.
In order to solve the problems, the invention well solves the problems by utilizing a self-supporting flexible electrode through a crosslinked reduced graphene oxide-based flexible self-supporting membrane composite electrode and a rapid preparation method thereof. The composite structure fully exerts the characteristics of high specific capacity among different components and excellent mechanical property and high conductivity of the reduced graphene oxide, and the prepared composite material can effectively buffer the volume expansion effect in the circulation process and has obvious advantages.
In order to achieve the purpose, the invention is realized by the following technical scheme that a high theoretical capacity material and a graphene oxide dispersion liquid are uniformly mixed to form a uniform mixed liquid; freeze-drying the mixed solution to obtain a graphene oxide-based composite material; the theoretical capacity of the high theoretical capacity material is more than 400mAh g -1 (ii) a Carrying out rapid crosslinking reduction treatment on the graphene oxide-based composite material by using a hot ammonium sulfide solution at room temperature, and freeze-drying again to obtain a crosslinked reduced graphene oxide-based flexible self-supporting membrane composite electrode;
preferably, the high theoretical capacity material is a zero-dimensional ferric oxide nanocube and one-dimensional Bi 2 S 3 Nanorod and two-dimensional SnS 2 One or more than two of the nano sheets.
Preferably, the high theoretical capacity material is Fe 2 O 3 A nanocube.
Preferably, the high theoretical capacity material is Fe 2 O 3 The preparation method comprises the following steps:
s1: pre-prepared Fe 2 O 3 Adding into graphene oxide dispersion liquid, stirring at a ratio of 0.2-5 to obtain Fe 2 O 3 A mixed solution with graphene oxide;
s2: transferring the uniformly stirred mixed solution into a culture dish, and freeze-drying;
s3: pouring ammonium sulfide solution heated to 50-90 ℃ in advance into the graphene oxide-based membrane material obtained after freeze drying for rapid reduction crosslinking treatment, washing off residual ammonium sulfide by using DIW, and freeze drying again to obtain reduced graphene oxide and Fe 2 O 3 A composite flexible self-supporting membrane electrode material.
Preferably, the concentration of the ammonium sulfide solution is 10-30%.
A high-theoretical-capacity material and reduced graphene oxide are compounded together, the reduced graphene oxide is of a cross-linked structure, and the high-theoretical-capacity material is wrapped in the cross-linked structure to form a stable structure, so that the cycling stability of the electrode can be effectively improved.
The invention has the beneficial effects that: the greatest innovation point of the composite structure is that the flexible self-supporting membrane electrode can be rapidly prepared at room temperature by a freeze-drying membrane forming method and an ammonium sulfide cross-linking reduction method, and the flexible self-supporting membrane electrode is easy to prepare on a large scale;
(1) The preparation method disclosed by the invention is quick and simple in preparation process and low in cost, and can be used for quickly crosslinking and reducing the graphene oxide at room temperature without a complicated heating process to obtain the rGO-based flexible self-supporting membrane electrode. The method directly forms a film, can ensure the loose and porous structural characteristics of the prepared electrode material, has good flexibility, avoids the use of a conductive agent and a binder in a slurry method, and can improve the energy density of the material.
(2) The composite electrode prepared by the invention takes the reduced graphene oxide as a conductive substrate, and combines the characteristics of high specific capacity among different components, excellent mechanical buffering performance and high conductivity of the reduced graphene oxide, so that the specific surface area of the composite material is effectively improved, the conductivity is improved, the problem of volume expansion in the circulation process is effectively relieved, and the circulation stability is enhanced, thereby greatly improving the electrochemical performance.
(3) The membrane electrode is prepared by a freeze drying method, and the membrane electrode is directly formed, so that the loose and porous structural characteristic of the prepared electrode material can be ensured, the membrane electrode has good flexibility, the use of a conductive agent and a binder in a slurry method is avoided, the energy density of the material can be improved, and the reduced graphene oxide-based membrane electrode material synthesized by the method is easy to regulate and control in parameters such as structure, components, morphology, thickness, loading capacity and the like, and is easy to prepare on a large scale.
(4) The ammonium sulfide has strong reducibility, the ammonium sulfide used in the preparation process of the rGO-based flexible self-supporting membrane electrode can rapidly reduce and crosslink graphene oxide in a very short time, and meanwhile, the obtained rGO-based flexible self-supporting membrane electrode can show electrochemical performance equivalent to or even better than that of the previous method, and can reduce stacking of the graphene oxide in the reduction process, so that the loose and porous structural characteristics of the material are better maintained.
(5) According to the method, various high-capacity materials can be compounded with graphene oxide to prepare the rGO-based flexible self-supporting membrane electrodes with different architectures. In addition, the flexible self-supporting membrane electrode with different surface loading amounts is obtained by regulating and controlling the amount of high-capacity materials in the preparation process, and has certain practical application significance.
Drawings
FIG. 1 is a graph relating to one-dimensional Bi 2 S 3 SEM pictures of nanorod-composited rGO-based flexible self-supporting membrane electrode materials;
FIG. 2 is a diagram of a two-dimensional SnS 2 SEM pictures of the nano-sheet compounded rGO-based flexible self-supporting membrane electrode material;
FIG. 3 is a schematic representation of the relationship with zero-dimensional Fe 2 O 3 SEM pictures of the composite rGO-based flexible self-supporting membrane electrode material;
FIG. 4 shows the zero-dimensional Fe 2 O 3 And (3) processing the composite rGO-based flexible self-supporting membrane electrode material by ammonium sulfide.
The specific implementation mode is as follows:
in order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
Fe 2 O 3 a rapid preparation method of a @ rGO flexible self-supporting membrane composite electrode comprises the following steps:
s1: a certain amount of Fe prepared in advance 2 O 3 Adding into GO dispersion containing a certain amount of GO, stirring for 5-10min with 3:1, and debubbling to obtain Fe 2 O 3 Mixed with GO.
S2: and transferring the uniformly stirred mixed solution to a culture dish with a certain size, and freeze-drying to obtain the graphene oxide-based membrane material.
S3: and (2) pouring a preheated ammonium sulfide solution (wt 20%,50-90 ℃) into the graphene oxide base membrane obtained after freeze drying for rapid reduction crosslinking treatment, then washing away residual ammonium sulfide by using DIW, and freeze drying again to obtain the reduced graphene oxide-based flexible self-supporting membrane electrode material.
S4: by changing the amount of the mixed liquid in the step S1, flexible self-supporting membrane electrodes with different surface loading amounts can be obtained.
Example 2
The preparation process is identical to example 1, with the difference that Fe is added 2 O 3 Conversion to one-dimensional Bi 2 S 3 Nanorod and two-dimensional SnS 2 Nanosheets.
As can be seen from fig. 1-3, after the ammonium sulfide is rapidly cross-linked and reduced, the high-capacity active material is well wrapped by rGO to form a good composite structure, which will effectively increase the specific surface area of the composite material, enhance the conductivity, and effectively alleviate the problem of volume expansion during the circulation process.
As can be seen from FIG. 4, the composite material is directly filmed after being treated by ammonium sulfide, so that the loose and porous structural characteristic of the material is ensured, and the material has good flexibility.
In conclusion, the graphene oxide can be rapidly crosslinked and reduced at room temperature without a complicated heating process to obtain the rGO-based flexible self-supporting membrane electrode, the membrane is directly formed by freeze drying, the loose and porous structural characteristics of the prepared electrode material can be ensured, the flexibility is good, the use of a conductive agent and a binder in a slurry method is avoided, and the energy density of the material can be improved.
The above embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above embodiments, and it should be understood by those skilled in the art that various modifications or changes can be made by those skilled in the art without inventive efforts based on the technical solutions of the present invention.

Claims (4)

1. A method for rapidly preparing a cross-linked reduced graphene oxide-based flexible self-supporting membrane electrode is characterized by comprising the following steps: uniformly mixing a high theoretical capacity material and the graphene oxide dispersion liquid to form a uniform mixed liquid; the theoretical capacity of the high theoretical capacity material is more than 400mAh g -1 (ii) a Freeze-drying the mixed solution to obtain a graphene oxide-based composite material; carrying out rapid crosslinking reduction treatment on the graphene oxide-based composite material by using a hot ammonium sulfide solution at room temperature, and freeze-drying again to obtain a crosslinked reduced graphene oxide-based flexible self-supporting membrane composite electrode; the high theoretical capacity material is one or more than two of a zero-dimensional ferric oxide nanocube, a one-dimensional Bi2S3 nanorod and a two-dimensional SnS2 nanosheet; the concentration of the ammonium sulfide solution is wt 10-30%; the prepared cross-linked reduced graphene oxide-based flexible self-supporting membrane electrode is formed by compounding a high theoretical capacity material and reduced graphene oxide together, wherein the reduced graphene oxide is in a cross-linked structure, and the high theoretical capacity material is wrapped in the cross-linked structure to form a stable structure.
2. The method of claim 1, wherein: the high theoretical capacity material is Fe 2 O 3 A nanocube.
3. The method of claim 2, wherein: the method comprises the following steps:
s1: pre-prepared Fe 2 O 3 Adding the mixture into graphene oxide dispersion liquid, and stirring to obtain Fe 2 O 3 A mixed solution with graphene oxide;
s2: transferring the uniformly stirred mixed solution into a culture dish, and freeze-drying;
s3: pouring ammonium sulfide solution heated to 50-90 ℃ in advance into the graphene oxide-based membrane material obtained after freeze drying for rapid reduction crosslinking treatment, washing off residual ammonium sulfide by using DIW, and freeze drying again to obtain reduced graphene oxide and Fe 2 O 3 A composite flexible self-supporting membrane electrode material.
4. The method of claim 3, wherein: fe in step S1 2 O 3 The molar ratio of the graphene oxide to the graphene oxide is 0.2-5.
CN202111024316.0A 2021-09-02 2021-09-02 Cross-linked reduced graphene oxide-based flexible self-supporting membrane electrode and rapid preparation method thereof Active CN113903888B (en)

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