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Dendritic three-dimensional graphene and its preparation method

A technology of graphene and dendrite, which is applied in the field of dendritic three-dimensional graphene and its preparation, can solve the problem that graphene has no oxygen reduction performance, and achieve good oxygen reduction performance, excellent catalytic performance, and simple preparation method

Active Publication Date: 2017-12-22
SOUTHEAST UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Generally speaking, graphene has no obvious oxygen reduction performance, and only after nitrogen doping has oxygen reduction performance.

Method used

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  • Dendritic three-dimensional graphene and its preparation method

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preparation example Construction

[0021] The preparation method of dendritic three-dimensional graphene comprises the steps:

[0022] 1) In CuSO 4 、NiSO 4 、H 2 SO 4 In the mixed solution with additives, the Cu sheet is used as the working electrode to deposit nano-Cu or CuNi clusters in the mixed solution to obtain a deposited product;

[0023] 2) After washing the deposition product in ultrapure water several times, the product was filtered out and freeze-dried to obtain a freeze-dried sample;

[0024] 3) Place the freeze-dried sample in a vacuum furnace, first perform reduction treatment in a hydrogen atmosphere at 800-1000 degrees Celsius, and then conduct graphene deposition treatment in a mixed atmosphere of 800-1000 degrees Celsius hydrogen and methane, and then use persulfuric acid Ammonium solution or ferric chloride solution removes the alloy substrate to obtain dendritic graphene.

[0025] Step 1), the CuSO 4 The concentration is 0.1-0.3 mol / L, NiSO 4 Concentration 0-2 mol / L, H 2 SO 4 The c...

Embodiment 1

[0029] At 0.1mol / L CuSO 4 + 0.5mol / L H 2 SO 4 In the mixed solution, the Cu sheet was used as the working electrode, the platinum electrode was used as the counter electrode, and the saturated calomel electrode was used as the reference electrode, at 0.25 A / cm 2 Cu nanoclusters were deposited under constant current conditions for 20 s. The deposited product was washed several times in ultrapure water and then freeze-dried. The freeze-dried samples were placed in a vacuum oven under Ar:H 2 (Flow ratio)=6:1, heat at 800 degrees Celsius for 20 minutes for reduction treatment, and then heat at 800 degrees Celsius Ar:H 2 :CH 4 (Flow ratio) = 8:1:1 for graphene deposition. After 20 minutes of deposition, use ammonium persulfate solution or ferric chloride solution to remove the metal substrate to obtain dendritic graphene. The dendritic graphite has a diameter of 200-400 nm and a length of 200-1000 nm primary tubular graphene, on which a large number of secondary tubular graph...

Embodiment 2

[0032] At 0.2 mol / L CuSO 4 + 1.0 mol / L H 2 SO 4 +0.8mol / L NiSO 4 (The addition of Ni ions can change the substrate composition, thermal stability and morphology of metal nanoclusters.) In the mixed solution, the Cu sheet was used as the working electrode, the platinum electrode was used as the counter electrode, and the saturated calomel electrode was used as the reference electrode. At 1.00 A / cm 2 Nano-CuNi clusters were deposited under constant current conditions for 30 s. The deposited product was washed several times in ultrapure water and then freeze-dried. The freeze-dried samples were placed in a vacuum oven under Ar:H 2 (Flow ratio)=6:1, heat at 900 degrees Celsius for 20 minutes for reduction treatment, and then heat at 900 degrees Celsius Ar:H 2 :CH 4Graphene deposition is carried out under the condition of (flow ratio) = 6:1:1, and dendritic graphene can be obtained after 20 minutes of deposition. The dendritic graphite has a diameter of 150-200 nm and a leng...

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Abstract

The invention discloses a preparation method of dendritic three-dimensional graphene and belongs to the technical field of nano material preparation. The preparation method comprises the steps of firstly, depositing nano Cu clusters or CuNi clusters in a mixed solution of CuSO4, NiSO4 and H2SO4 with a Cu sheet serving as a working electrode to obtain a graphene deposition substrate; secondly, putting nano metal clusters into ultra pure water to be cleaned multiple times, and then performing filtering and freeze-drying; thirdly, putting the freeze-dried nano metal clusters into a vacuum furnace, performing reduction treatment in hydrogen atmosphere at the temperature of 800-1000 DEG C, then performing graphene deposition treatment in hydrogen and methane mixed atmosphere at the temperature of 800-1000 DEG C, and removing the alloy substrate through an ammonium persulfate solution or a ferric trichloride solution to obtain dendritic graphene. The invention further discloses a series of dendritic three-dimensional graphene obtained through the method. The dendritic three-dimensional grapheme is characterized in that one end is open, and other ends are closed. The graphene has outstanding oxygen reduction performance.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, and in particular relates to dendritic three-dimensional graphene and a preparation method thereof. Background technique [0002] Graphene materials have excellent electrical and thermal conductivity and ultra-high strength properties. At present, there are two main types of large-scale preparation of graphene materials: one is thin-film two-dimensional graphene prepared by chemical vapor deposition or redox method; the other is three-dimensional graphene prepared by explosion method or template method. Compared with two-dimensional graphene, three-dimensional graphene has a larger specific surface area and is expected to be widely used in sensing, catalysis and other fields. [0003] The current three-dimensional graphene is foamed graphene with a porous structure, and graphene with a dendrite-like structure has not been reported yet. In addition, the microstructure size of th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/186C01B32/194
CPCC01P2004/03C01P2004/30
Inventor 曾宇乔李晨俊葛创何美平项桦张旭海郭新立蒋建清
Owner SOUTHEAST UNIV
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