Preparation method of porous graphene and applications of finished product thereof

Abstract

The invention relates to a preparation method of porous graphene and applications of finished product thereof. The preparation method comprises following steps: (1) ultrasonically dispersing graphene oxide in deionized water; (2) dissolving a certain amount of water-soluble transition metal salts in deionized water, dropwise adding the solution into the graphene oxide solution, and stirring at the same time; (3) subjecting the mixed solution to treatments of centrifugation and washing to extract products, drying the products for 1 to 20 hours; (4) putting the obtained materials into a tube-type furnace, heating, burning the materials at a constant temperature of 500 to 1050 DEG C for 1 to 20 hours, while controlling the flow speed of inert gas in the range of 10 to 300 mL / min, cooling, and collecting the solid products; (5) processing the solid products with dilute hydrochloric acid to remove the transition metal oxides in the solid products so as to obtain the porous graphene material. The porous graphene material prepared by the method has the advantages of few layers and controllable hole size, and solves the problems of non-conductivity of electrons in the vertical direction to the horizontal surface of the graphite material multi-layer graphene and obstructed route of Li. Furthermore, the construction of nano micro-hole structure is beneficial for storage, diffusion, and transportation of charges.

Description

[0001] Technical field:

[0002] The invention relates to a preparation method of graphene, in particular to a porous graphene, the preparation method and the application of the product. This method can effectively design the three-dimensional structure of graphene to form good electron and ion transport channels, which is the key to constructing high-performance lithium-ion battery anode materials. Background technique:

[0003] Graphene is a new carbonaceous material with a single-layer two-dimensional honeycomb lattice structure in which carbon atoms are tightly packed, and has an ideal two-dimensional crystal structure. The ideal graphene, all of its carbon atoms are exposed on the surface, is a real surface solid with a large specific surface area of ​​2630m 2 / g, with unique carrier characteristics and transport properties, it is a potential energy storage material. In the application of lithium-ion batteries, graphene materials have their unique advantages: 1) G...

Examples

Embodiment 1

[0027] Take 90mg of graphene oxide and add it into 60mL of deionized water for ultrasonic dispersion for 1h; weigh 0.01mol, that is, 2.703g of FeCl 3 ·6H 2 O was dissolved in 10 mL of deionized water to make a 1M solution, and slowly added dropwise to the above 60 mL graphene oxide solution under constant stirring with a magnetic stirrer, and stirred for 2 h. The resulting mixture was centrifuged at 5000-15000 rpm, washed with ethanol, and this process was repeated three times. The resulting precipitate was collected in a petri dish and dried at a temperature of 60° C. for 10 h. After drying, the prepared precursor sample was placed in a quartz boat and placed in a tube furnace, heated at a heating rate of 20°C / min, controlled at a nitrogen flow rate of 300mL / min, and calcined at a constant temperature of 1050°C for 2 hours, and the solid product was collected after cooling . Treat the solid product with dilute hydrochloric acid or dilute sulfuric acid, the volume ratio of w...

Embodiment 2

[0030] Take 90mg graphene oxide and add it into 60mL deionized water for ultrasonic dispersion for 2h; weigh 0.01mol (2.9081g) Ni(NO 3 ) 2 ·6H 2 O was dissolved in 20mL of deionized water to make a 0.5M solution, and slowly added dropwise to the above 60mL graphene oxide solution under constant stirring with a magnetic stirrer, and stirred for 2h. The resulting mixture was centrifuged and washed with deionized water, and this process was repeated three times. The resulting precipitate was collected in a petri dish and dried at a temperature of 110° C. for 2 h. After drying, the prepared precursor samples were placed in a quartz boat and placed in a tube furnace, heated at a heating rate of 10 °C / min, controlled at a nitrogen flow rate of 100 mL / min, calcined at a constant temperature of 700 °C for 20 h, and collected after cooling solid product. The solid product is treated with hot sulfuric acid to remove NiO, filtered and washed with water until neutral, and dried to obta...

Embodiment 3

[0033] Take 90mg graphene oxide and add it into 60mL deionized water for ultrasonic dispersion for 4h; weigh 0.02mol (5.821g) Co(NO 3 ) 2 ·6H 2 O was dissolved in 20 mL of deionized water to make a 1M solution, and slowly added dropwise to the above 60 mL graphene oxide solution under constant stirring with a magnetic stirrer, and stirred for 2 h.

[0034] The resulting mixture was centrifuged and washed with ethanol, and this process was repeated three times. The resulting precipitate was collected in a petri dish and dried at a temperature of 80° C. for 10 h. After the drying is completed, put the prepared precursor sample in a quartz boat and put it into a tube furnace, heat it at a heating rate of 15°C / min, control the nitrogen flow rate at 200mL / min, and calcinate at a constant temperature of 800°C for 20h, and collect the solid product after cooling . Treat the solid product with dilute sulfuric acid, the volume ratio of the two is 1:10, remove cobalt oxide, filter an...

[0001] Technical field:

[0002] The invention relates to a preparation method of graphene, in particular to a porous graphene, the preparation method and the application of the product. This method can effectively design the three-dimensional structure of graphene to form good electron and ion transport channels, which is the key to constructing high-performance lithium-ion battery anode materials. Background technique:

[0003] Graphene is a new carbonaceous material with a single-layer two-dimensional honeycomb lattice structure in which carbon atoms are tightly packed, and has an ideal two-dimensional crystal structure. The ideal graphene, all of its carbon atoms are exposed on the surface, is a real surface solid with a large specific surface area of ​​2630m 2 / g, with unique carrier characteristics and transport properties, it is a potential energy storage material. In the application of lithium-ion batteries, graphene materials have their unique advantages: 1) G...

Examples

Embodiment 1

[0027] Take 90mg of graphene oxide and add it into 60mL of deionized water for ultrasonic dispersion for 1h; weigh 0.01mol, that is, 2.703g of FeCl 3 ·6H 2 O was dissolved in 10 mL of deionized water to make a 1M solution, and slowly added dropwise to the above 60 mL graphene oxide solution under constant stirring with a magnetic stirrer, and stirred for 2 h. The resulting mixture was centrifuged at 5000-15000 rpm, washed with ethanol, and this process was repeated three times. The resulting precipitate was collected in a petri dish and dried at a temperature of 60° C. for 10 h. After drying, the prepared precursor sample was placed in a quartz boat and placed in a tube furnace, heated at a heating rate of 20°C / min, controlled at a nitrogen flow rate of 300mL / min, and calcined at a constant temperature of 1050°C for 2 hours, and the solid product was collected after cooling . Treat the solid product with dilute hydrochloric acid or dilute sulfuric acid, the volume ratio of w...

Embodiment 2

[0030] Take 90mg graphene oxide and add it into 60mL deionized water for ultrasonic dispersion for 2h; weigh 0.01mol (2.9081g) Ni(NO 3 ) 2 ·6H 2 O was dissolved in 20mL of deionized water to make a 0.5M solution, and slowly added dropwise to the above 60mL graphene oxide solution under constant stirring with a magnetic stirrer, and stirred for 2h. The resulting mixture was centrifuged and washed with deionized water, and this process was repeated three times. The resulting precipitate was collected in a petri dish and dried at a temperature of 110° C. for 2 h. After drying, the prepared precursor samples were placed in a quartz boat and placed in a tube furnace, heated at a heating rate of 10 °C / min, controlled at a nitrogen flow rate of 100 mL / min, calcined at a constant temperature of 700 °C for 20 h, and collected after cooling solid product. The solid product is treated with hot sulfuric acid to remove NiO, filtered and washed with water until neutral, and dried to obta...

Embodiment 3

[0033] Take 90mg graphene oxide and add it into 60mL deionized water for ultrasonic dispersion for 4h; weigh 0.02mol (5.821g) Co(NO 3 ) 2 ·6H 2 O was dissolved in 20 mL of deionized water to make a 1M solution, and slowly added dropwise to the above 60 mL graphene oxide solution under constant stirring with a magnetic stirrer, and stirred for 2 h.

[0034] The resulting mixture was centrifuged and washed with ethanol, and this process was repeated three times. The resulting precipitate was collected in a petri dish and dried at a temperature of 80° C. for 10 h. After the drying is completed, put the prepared precursor sample in a quartz boat and put it into a tube furnace, heat it at a heating rate of 15°C / min, control the nitrogen flow rate at 200mL / min, and calcinate at a constant temperature of 800°C for 20h, and collect the solid product after cooling . Treat the solid product with dilute sulfuric acid, the volume ratio of the two is 1:10, remove cobalt oxide, filter an...

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