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Preparation method of graphene and two-dimensional noble metal cluster composite material

A composite material and precious metal technology, applied in the field of carbon materials, can solve the problem that the performance improvement of composite materials is not as good as that of two-dimensional Pt, and achieve the effect of enhancing synergistic effect, overcoming cumbersome preparation process, and enriching preparation methods.

Active Publication Date: 2016-03-23
浙江荣鑫带钢有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the currently widely used solution chemical reduction method, microwave reduction and other methods can only prepare composite materials of noble metal nanoparticles such as three-dimensional Pt, and the improvement of the performance of the composite material is far less than that of the two-dimensional Pt atomic cluster composite material.

Method used

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  • Preparation method of graphene and two-dimensional noble metal cluster composite material
  • Preparation method of graphene and two-dimensional noble metal cluster composite material

Examples

Experimental program
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Effect test

Embodiment 1

[0024] The first step is the preparation of graphite oxide. Add 10g of natural graphite (with a particle size of 50~80μm) into 230ml of concentrated sulfuric acid containing 5g of sodium nitrate (placed in an ice bath), then add 30g of KMnO4, and control the solution below 20°C, stir well and put React in a water bath at 35°C for 30 minutes, then slowly add 460ml of distilled water to keep the reaction temperature at 98°C, react for another 15 minutes, add 1.4L of distilled water and 10ml of hydrogen peroxide, and centrifuge the yellow suspension in the solution until the filtrate is washed with BaCl 2 No sulfate ion was detected, and the product was dried in air at 60°C for 12 hours, and stored in a desiccator.

[0025]In the second step, add 20mg of graphite oxide to 20ml of distilled water, ultrasonically disperse for 30min, take the dispersed graphite oxide solution and drop it on the glass carbon electrode, let it dry naturally and slowly.

[0026] The third step, insert...

Embodiment 2

[0029] The first and second steps of this implementation are the same as in Embodiment 1.

[0030] The third step, insert the glass electrode into 0.01mMK 2 PtCl 4 , 0.05mM RuCl 3 and 5mM CuSO 4 In the mixed solution of -0.5~1V (the reference electrode is Ag / AgCl, 3MCl － ) potential interval for linear scanning (scan rate 25mV / S).

[0031] The fourth step is to repeatedly perform cyclic scanning in the above potential range, Pt, Ru underpotential deposition, stripping, and cyclic scanning for 300 times, take out the glass carbon electrode and wash it with distilled water to obtain a graphene-two-dimensional PtRu atomic cluster composite material, which The catalytic performance is about 14 times higher than that of commercial E-TEKPtRu / C. (Catalytic activity test conditions: the reference electrode is Ag / AgCl, 3MCl － Electrode, the voltage sweep rate is 25mV / s, the electrolyte solution is 0.5MCH 3 OH+0.1MHClO 4 , at a voltage of ~0.6V, the peak value of the graphene ma...

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Abstract

The invention discloses a preparation method of a graphene and two-dimensional noble metal cluster composite material, comprising following steps: oxidizing graphite in a solution to form graphite oxide, ultrasonically dispersing the graphite oxide in an aqueous solution to form a graphite oxide solution, and dropping the solution to the surface of a glass electrode before natural slow drying; dipping the glass electrode in a mixed solution containing ions of a mediate metal M (Pb or Cu) and noble metal ions, subjecting the glass electrode to underpotential deposition and dissolution and stripping in a certain potential interval, after multiple volt-ampere cycles, depositing a noble metal on the surface of a graphene layer in a two-dimensional cluster form, and forming the graphene and two-dimensional noble metal cluster composite material. The graphene and two-dimensional Pt / Ru cluster composite material prepared by the method has super-high catalytic activity for methanol oxidation reaction. The invention is expected to enrich the preparation methods of graphene composite materials, optimize their structure, improving their performance, and widen their applicable ranges.

Description

technical field [0001] The invention relates to a preparation method for depositing two-dimensional precious metal atomic clusters on the surface of graphene. The graphene-two-dimensional PtRu composite material prepared by the method has super high catalytic activity for methanol oxidation reaction. It belongs to the technical field of carbon materials. Background technique [0002] Graphene-noble metal nanoparticle composites have a wide range of applications in energy storage, fuel cell catalysts, sensors, etc., and have become a research hotspot in materials and related fields in recent years. The noble metal Pt and its alloys have good catalytic activity for the oxidation of methanol, and are the materials with the highest catalytic activity for the direct methanol fuel cell (DMFC) anode catalyst found today. Dispersed on supporting materials such as carbon materials. [0003] Graphene has a unique structure and excellent physical and chemical properties, and is consi...

Claims

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Application Information

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IPC IPC(8): B01J23/42B01J23/46H01M4/90H01M4/92H01M8/10
CPCH01M4/90H01M4/9058H01M4/926H01M8/1011Y02E60/50
Inventor 胡忠良李雪锋席柳江黄志丁燕鸿
Owner 浙江荣鑫带钢有限公司
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