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Preparation method of structure-controllable three-dimensional graphene and composite material thereof

A graphene composite, graphene technology, applied in graphene, metal material coating process, liquid chemical plating and other directions, can solve the problem that the pore characteristic graphene sheet orientation cannot be effectively controlled, and the graphene sheet orientation cannot be realized. control, poor surface quality of metal templates, etc., to overcome the uneven distribution of graphene, short preparation cycle, and easy operation.

Active Publication Date: 2017-11-24
HUAZHONG UNIV OF SCI & TECH
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Problems solved by technology

For example, CN102674321A discloses a graphene film deposited on the surface of a three-dimensional foamed nickel template by chemical vapor deposition, and obtains porous foamed graphene after dissolving the porous metal substrate. However, the method uses metal foam as a template, wherein Both the pore characteristics and the orientation of graphene sheets cannot be effectively controlled; CN105776186A discloses a method for preparing a three-dimensional graphene porous material with controllable growth and structure by using SLM forming metal templates. The method is prepared by SLM additive manufacturing technology Metal template growth graphene, the metal template surface quality prepared by SLM is relatively poor, so the prepared graphene quality is relatively poor, is difficult to be applied to the preparation of composite material; CN106349658A, CN105749865A and CN106349658A announced the preparation method of three-dimensional graphene composite material Both use powdered three-dimensional graphene as the composite agent, and the dispersion of graphene has been improved to a certain extent, but agglomeration still occurs, and the orientation of graphene sheets cannot be controlled

Method used

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  • Preparation method of structure-controllable three-dimensional graphene and composite material thereof

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preparation example Construction

[0042] (6) the preparation of three-dimensional graphene composite metal material, the metal structure that the surface that step (4) makes has graphene is long as composite additive material, adopts the method for casting, hot isostatic pressing to make metal fill template space, make Obtain three-dimensional graphene composite metal material;

[0043] The filling metal in step (6) is copper or nickel; the proportion of three-dimensional graphene in the composite material is 0.01-10wt%.

[0044] (7) The three-dimensional graphene with the resin support layer is used for injection molding and solvent evaporation to make the resin material fill the template gap to obtain a three-dimensional graphene composite resin material; the three-dimensional graphene with the resin support layer is filled with ceramic slurry Material, colloidal molding method, so that the ceramic material fills the gap, and then use organic solvent corrosion or heat treatment to remove the resin support la...

Embodiment 1

[0049] (1) Use CAD software to establish a three-dimensional porous unit body with a unit size of 0.1mm. The unit body array is designed as a periodic porous structure with a porosity of 30% and an orderly arrangement. The external size of the model is 50mm×50mm ×10mm.

[0050] (2) The resin structure of the constructed CAD model was prepared by light-curing additive manufacturing technology.

[0051] (3) After cleaning, roughening, neutralizing, sensitizing, and activating the prepared resin structure, adopt an electroless copper plating process to plate a copper metal layer on the surface of the resin structure. The electroless copper plating solution uses copper sulfate as copper salt, and formaldehyde As a reducing agent, the thickness of the plated metal copper layer is 1 μm. Soak the prepared resin structure coated with the metal layer in acetone, take it out after the resin structure is completely dissolved, and then wash and dry it.

[0052] (4) Put the metal templat...

Embodiment 2

[0055] (1) Using CAD software, a three-dimensional porous unit body with a unit size of 10mm is correspondingly established. The unit body array is designed as a periodic porous structure with a porosity of 99% and an orderly arrangement. The external size of the model is 100mm×100mm× 100mm.

[0056] (2) The resin structure of the constructed CAD model was prepared by fused deposition additive manufacturing technology.

[0057] (3) After cleaning, coarsening, neutralizing, sensitizing and activating the prepared resin structure, adopt the electroless nickel plating process to plate a copper metal layer on the surface of the resin structure. The electroless nickel plating solution adopts nickel sulfate as nickel salt, sub Sodium phosphate is used as a reducing agent, and the thickness of the metal nickel layer plated is 50 μm. The prepared resin structure coated with the metal layer was heat-treated at 900° C. for 3 hours under a nitrogen protective atmosphere to decompose and...

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Abstract

The invention belongs to the field of graphene composite material preparation, and discloses a preparation method of structure-controllable three-dimensional graphene and a composite material thereof. The preparation method comprises the following steps: (a) designing and constructing a CAD model, and performing additive manufacturing to obtain a three-dimensional resin structure of a corresponding structure; (b) plating a copper or nickel metal layer on the surface of the three-dimensional resin structure obtained in step (a) by a chemical plating method, and removing a resin material to obtain a three-dimensional structural template of copper or nickel; (c) generating graphene on the three-dimensional structural metal template through a chemical vapor-phase deposition method, thereby preparing the structure-controllable three-dimensional graphene. The obtained graphene is further treated to obtain a graphene composite material. Through the preparation method, control on the structure of three-dimensional graphene can be realized, and a high-quality and multifunctional three-dimensional graphene composite material product under effective and precise control is obtained. The method is simple and convenient to operate, is short in preparation period, and is wide in adaptive range.

Description

technical field [0001] The invention belongs to the field of preparation of graphene composite materials, and more specifically relates to a preparation method of three-dimensional graphene with controllable structure and a composite material thereof. Background technique [0002] Graphene is a two-dimensional (2D) crystal material composed of a single layer of carbon atoms. It has very important application prospects in scientific fields such as storage. Composite materials prepared from graphene have also attracted much attention because of their improvements in the mechanical, thermal and electrical properties of the original materials. [0003] However, there is a strong interaction force between 2D single-layer graphene sheets, and it is easy to aggregate. The graphene materials we usually use are mostly in the form of powder, which leads to its excellent specific surface area and thermal and electrical conductivity. limit. The preparation of existing graphene compos...

Claims

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Application Information

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IPC IPC(8): C01B32/186C04B35/10C04B35/48C04B35/46C04B35/14C04B35/565C04B35/52C04B35/622C22C1/10C23C18/36C23C18/40
CPCC22C1/101C22C1/1036C23C18/36C23C18/405C04B35/10C04B35/14C04B35/46C04B35/48C04B35/522C04B35/565C04B35/622C22C1/1047
Inventor 闫春泽李昭青杨磊史玉升陈鹏
Owner HUAZHONG UNIV OF SCI & TECH
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