CN111900350A - Porous carbon-graphene composite material and preparation method thereof - Google Patents
Porous carbon-graphene composite material and preparation method thereof Download PDFInfo
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- CN111900350A CN111900350A CN202010676377.4A CN202010676377A CN111900350A CN 111900350 A CN111900350 A CN 111900350A CN 202010676377 A CN202010676377 A CN 202010676377A CN 111900350 A CN111900350 A CN 111900350A
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- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The embodiment of the invention provides a porous carbon-graphene composite material and a preparation method thereof, wherein the preparation method comprises the following steps: adding the super absorbent resin into the graphene oxide solution subjected to ultrasonic treatment, and freezing and molding; freeze-drying in a vacuum environment to obtain a super absorbent resin-graphene oxide composite material; and under a protective atmosphere, sequentially carbonizing, washing and drying the obtained composite material at 500-1000 ℃ to constant weight, and grinding the porous carbon-graphene composite material. According to the embodiment of the invention, the super absorbent resin, water and a small amount of graphene oxide are used as raw materials, the cost is low, the super absorbent resin is filled with the graphene oxide solution, the structure of the porous carbon-graphene composite material obtained after carbonization cannot collapse, the graphene oxide has excellent conductivity after thermal reduction, and the graphene oxide is filled in the porous carbon, so that the conductivity and the specific surface area of the porous carbon are greatly increased, and the reaction activity and the reaction rate are improved. The preparation method has the advantages of simple preparation steps, no toxic or harmful solvent, environmental protection and high efficiency.
Description
Technical Field
The invention relates to the field of new energy, and particularly relates to a porous carbon-graphene composite material and a preparation method thereof.
Background
The positive electrode and the negative electrode of the lithium ion battery are the basis of the battery performance, and directly determine various performance indexes of the battery, such as specific energy, specific power, cycling stability, safety and the like. At present, the negative electrode is generally made of carbon materials, and the porous carbon materials have the advantages of excellent conductivity, low cost, simple preparation process and most extensive application. The super absorbent resin can absorb water which is hundreds of times of the volume of the resin, the volume of the super absorbent resin can be effectively enlarged, a large number of pore channels and pores can be formed in the super absorbent resin after water absorption and drying, and a carbon material with high specific surface area can be formed after carbonization, so that the super absorbent resin has extremely low cost and good conductivity.
In the carbonization process of the super absorbent resin, the volume of the super absorbent resin is increased more, the formed pores are not supported by materials, and the porous structure is easy to collapse, so that the performance of the super absorbent resin is influenced, how to prevent the structure from collapsing in the carbonization process is avoided, and the specific surface area of the super absorbent resin is increased, thereby having important research significance.
Disclosure of Invention
The invention provides a porous carbon-graphene composite material and a preparation method thereof, and aims to solve the technical problems that a structural knot is easy to collapse and is not beneficial to use in the carbonization process of the conventional lithium battery cathode material.
The embodiment of the invention provides a preparation method of a porous carbon-graphene composite material, which comprises the following steps:
s1, adding the super absorbent resin into the graphene oxide solution subjected to ultrasonic treatment, and freezing and forming;
s2, freeze-drying in a vacuum environment to obtain the super absorbent resin-graphene oxide composite material;
and S3, sequentially carbonizing, washing and drying the obtained composite material at 500-1000 ℃ in a protective atmosphere to constant weight, and grinding the porous carbon-graphene composite material.
Further, the super absorbent resin is one or more of starch grafted acrylic acid, grafted acrylamide, high-substitution-degree cross-linked carboxymethyl cellulose, cross-linked carboxymethyl cellulose grafted acrylamide or sodium polyacrylate.
Further, the graphene oxide solution adopts one or more of eigenstate graphene oxide, nitrogen-doped graphene oxide and sulfur-doped graphene oxide.
Furthermore, the size of the graphene oxide is 500-2000 nm, and the number of layers of the graphene oxide is 1-100.
Further, the concentration of the graphene oxide solution is 0.1-2 g/L.
Further, in step S1, the ratio of the mass of the super absorbent resin to the volume of the graphene oxide solution is 1 g: (0.05-1) L.
Further, in step S3, the shielding gas is nitrogen or argon.
Further, in step S3, the drying time is 60-180 min.
Further, in step S3, the heating temperature for carbonization is 500 to 1000 ℃.
On the other hand, the invention also provides a porous carbon-graphene composite material, and the porous carbon-graphene composite material is prepared by the preparation method.
The invention has the beneficial effects that: according to the embodiment of the invention, the super absorbent resin, water and a small amount of graphene oxide are used as raw materials, the cost is low, the super absorbent resin is filled with the graphene oxide solution, the structure of the porous carbon-graphene composite material obtained after carbonization cannot collapse, the graphene oxide has excellent conductivity after thermal reduction, and the graphene oxide is filled in the porous carbon, so that the conductivity and the specific surface area of the porous carbon are greatly increased, and the reaction activity and the reaction rate are improved. In addition, the super absorbent resin is rich in carbon elements and contains other beneficial elements (N, S, P and the like), so that the cycle performance of the lithium ion battery is improved. The preparation method has the advantages of simple preparation steps, no toxic or harmful solvent, environmental protection and high efficiency.
Drawings
Fig. 1 is an SEM image of reduction of the porous carbon-graphene composite material obtained in example 1 of the present invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", and the like, indicate orientations and positional relationships based on those shown in the drawings, and are used only for convenience of description and simplicity of description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be considered as limiting the present invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the present invention, unless otherwise expressly specified or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the present invention, unless otherwise expressly stated or limited, "above" or "below" a first feature means that the first and second features are in direct contact, or that the first and second features are not in direct contact but are in contact with each other via another feature therebetween. Also, the first feature being "on," "above" and "over" the second feature includes the first feature being directly on and obliquely above the second feature, or merely indicating that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature includes the first feature being directly under and obliquely below the second feature, or simply meaning that the first feature is at a lesser elevation than the second feature.
The present invention will be described in further detail with reference to the following detailed description and accompanying drawings.
The embodiment of the invention provides a preparation method of a porous carbon-graphene composite material, which comprises the following steps:
s1, adding the super absorbent resin into the graphene oxide solution subjected to ultrasonic treatment, and freezing and forming;
s2, freeze-drying in a vacuum environment to obtain the super absorbent resin-graphene oxide composite material;
and S3, sequentially carbonizing, washing and drying the obtained composite material at 500-1000 ℃ in a protective atmosphere to constant weight, and grinding the porous carbon-graphene composite material.
According to the embodiment of the invention, the super absorbent resin, water and a small amount of graphene oxide are used as raw materials, the cost is low, the super absorbent resin is filled with the graphene oxide solution, the structure of the porous carbon-graphene composite material obtained after carbonization cannot collapse, the graphene oxide has excellent conductivity after thermal reduction, and the graphene oxide is filled in the porous carbon, so that the conductivity and the specific surface area of the porous carbon are greatly increased, and the reaction activity and the reaction rate are improved. In addition, the super absorbent resin is rich in carbon elements and contains other beneficial elements (N, S, P and the like), so that the cycle performance of the lithium ion battery is improved. The preparation method has the advantages of simple preparation steps, no toxic or harmful solvent, environmental protection and high efficiency.
In an alternative embodiment, the super absorbent resin is one or more of starch grafted acrylic acid, grafted acrylamide, high-substitution crosslinked carboxymethyl cellulose, crosslinked carboxymethyl cellulose grafted acrylamide, or sodium polyacrylate.
In an alternative embodiment, the graphene oxide solution employs one or more of an intrinsic state graphene oxide, a nitrogen-doped graphene oxide, and a sulfur-doped graphene oxide.
In an alternative embodiment, the size of the graphene oxide is 500-2000 nm, and the number of layers of the graphene oxide is in the range of 1-100 layers.
In an optional embodiment, the concentration of the graphene oxide solution is 0.1-2 g/L.
In an alternative embodiment, in step S1, the ratio of the mass of the super absorbent resin to the volume of the graphene oxide solution is 1 g: (0.05-1) L.
In an alternative embodiment, in step S3, the shielding gas is nitrogen or argon. The drying time is 60-180 min. In step S3, the heating temperature for carbonization is 500-1000 ℃.
On the other hand, the invention also provides a porous carbon-graphene composite material, and the porous carbon-graphene composite material is prepared by the preparation method.
According to the embodiment of the invention, the super absorbent resin, water and a small amount of graphene oxide are used as raw materials, the cost is low, the super absorbent resin is filled with the graphene oxide solution, the structure of the porous carbon-graphene composite material obtained after carbonization cannot collapse, the graphene oxide has excellent conductivity after thermal reduction, and the graphene oxide is filled in the porous carbon, so that the conductivity and the specific surface area of the porous carbon are greatly increased, and the reaction activity and the reaction rate are improved. In addition, the super absorbent resin is rich in carbon elements and contains other beneficial elements (N, S, P and the like), so that the cycle performance of the lithium ion battery is improved. The preparation method has the advantages of simple preparation steps, no toxic or harmful solvent, environmental protection and high efficiency.
The specific embodiment is as follows:
example 1
Preparing a graphene oxide solution with the concentration of 0.5g/L, carrying out ultrasonic treatment for 30min, adding 1g of sodium polyacrylate into 100ml of an eigenstate graphene oxide solution, stirring, uniformly distributing the graphene oxide in a single layer, carrying out freeze forming, carrying out vacuum freeze drying to constant weight, heating at 800 ℃ for 120min in a nitrogen atmosphere, washing after carbonization is finished, drying to constant weight, and grinding to obtain the porous carbon-graphene composite material.
And preparing the porous carbon-graphene composite material into the button cell. Through electrochemical performance tests, when the current density is 0.1C, the first discharge specific capacity is 353.81mAh/g, the discharge specific capacity after 100-week circulation is 383.90mAh/g, the capacity retention rate is 108.50%, and the cycle performance is excellent.
Fig. 1 is an SEM image of graphene obtained after reduction of graphene oxide in this example, and as can be seen from fig. 1, graphene oxide has good dispersibility, is a single layer, and can sufficiently exhibit the effects of high conductivity and high specific surface area.
Example 2
Preparing a nitrogen-doped graphene oxide solution with the concentration of 0.5g/L, carrying out ultrasonic treatment for 30min, adding 1g of sodium polyacrylate into 100ml of the graphene oxide solution, stirring to enable the sodium polyacrylate to be uniformly distributed, carrying out freeze drying to constant weight, heating at 500 ℃ for 30min under a nitrogen atmosphere, washing to remove salt ions in the solution after carbonization is completed, drying to constant weight, and grinding to obtain the porous carbon-graphene composite material.
The porous carbon-graphene composite material is used as a lithium ion battery cathode material to prepare the button battery. Through electrochemical performance tests, when the current density is 0.1C, the first discharge specific capacity is 334.29mAh/g, the discharge specific capacity after 100-week circulation is 340.28 mAh/g, the capacity retention rate is 101.79%, and the circulation performance is better.
Example 3
Preparing a nitrogen-doped graphene oxide solution with the concentration of 1g/L, carrying out ultrasonic treatment for 30min, adding 1g of starch grafted acrylic acid into 200ml of the graphene oxide solution, stirring to enable the solution to be uniformly distributed, carrying out freeze drying to constant weight, heating at 900 ℃ for 180min under a nitrogen atmosphere, washing to remove impurities after carbonization is finished, drying to constant weight, and grinding to obtain the porous carbon-graphene composite material.
The porous carbon-graphene composite material is used as a lithium ion battery cathode material to prepare the button battery. Through electrochemical performance tests, when the current density is 0.1C, the first discharge specific capacity is 329.34mAh/g, the discharge specific capacity after 100-week circulation is 322.85 mAh/g, the capacity retention rate is 98.02%, and the circulation performance is good.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples" or the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is a more detailed description of the present invention that is presented in conjunction with specific embodiments, and the practice of the invention is not to be considered limited to those descriptions. It will be apparent to those skilled in the art that a number of simple derivations or substitutions can be made without departing from the inventive concept.
Claims (10)
1. A preparation method of a porous carbon-graphene composite material is characterized by comprising the following steps:
s1, adding the super absorbent resin into the graphene oxide solution subjected to ultrasonic treatment, and freezing and forming;
s2, freeze-drying in a vacuum environment to obtain the super absorbent resin-graphene oxide composite material;
and S3, sequentially carbonizing, washing and drying the obtained composite material at 500-1000 ℃ in a protective atmosphere to constant weight, and grinding the porous carbon-graphene composite material.
2. The method for preparing a porous carbon-graphene composite material according to claim 1, wherein the super absorbent resin is one or more of starch grafted acrylic acid, grafted acrylamide, highly substituted cross-linked carboxymethyl cellulose, cross-linked carboxymethyl cellulose grafted acrylamide, or sodium polyacrylate.
3. The method of preparing a porous carbon-graphene composite material according to claim 1, wherein the graphene oxide solution employs one or more of intrinsic state graphene oxide, nitrogen-doped graphene oxide, and sulfur-doped graphene oxide.
4. The method for preparing a porous carbon-graphene composite material according to claim 1, wherein the size of the graphene oxide is 500-2000 nm, and the number of layers of the graphene oxide is in the range of 1-100 layers.
5. The preparation method of the porous carbon-graphene composite material according to claim 1, wherein the concentration of the graphene oxide solution is 0.1-2 g/L.
6. The method for preparing a porous carbon-graphene composite material according to claim 1, wherein in step S1, the ratio of the mass of the super absorbent resin to the volume of the graphene oxide solution is 1 g: (0.05-1) L.
7. The method for preparing a porous carbon-graphene composite material according to claim 1, wherein in step S3, the shielding gas is nitrogen or argon.
8. The preparation method of the porous carbon-graphene composite material according to claim 1, wherein in the step S3, the drying time is 60-180 min.
9. The method for preparing a porous carbon-graphene composite material according to claim 1, wherein in step S3, the heating temperature for carbonization is 500 to 1000 ℃.
10. A porous carbon-graphene composite material is characterized by being prepared by the preparation method of any one of claims 1-9.
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| CN202010676377.4A CN111900350A (en) | 2020-07-14 | 2020-07-14 | Porous carbon-graphene composite material and preparation method thereof |
| PCT/CN2021/082188 WO2022012075A1 (en) | 2020-07-14 | 2021-03-22 | Porous carbon-graphene composite material and preparation method therefor |
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| CN114590799B (en) * | 2022-03-28 | 2024-05-10 | 南通第六元素材料科技有限公司 | Graphene preparation method, graphene powder and product |
| WO2024033374A1 (en) | 2022-08-11 | 2024-02-15 | Syngenta Crop Protection Ag | Novel arylcarboxamide or arylthioamide compounds |
| GB202214202D0 (en) | 2022-09-28 | 2022-11-09 | Syngenta Crop Protection Ag | Agricultural methods |
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| CN116002660B (en) * | 2022-12-28 | 2023-07-18 | 太原科技大学 | Preparation method of carbon-silicon composite material, carbon-silicon composite material and lithium battery |
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