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Preparation method of metal mono-atoms

An atom and metal technology, applied in the field of metal single atom preparation, can solve the problems of difficult separation of noble metal catalysts, high catalyst cost, and difficulty in widespread use, and achieve high electrocatalytic activity and stability, high-efficiency application range, and cost reduction. Effect

Active Publication Date: 2017-07-04
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, noble metals are expensive, and noble metal catalysts are not easy to separate, resulting in high cost of noble metal catalysts, which are difficult to be widely used

Method used

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  • Preparation method of metal mono-atoms
  • Preparation method of metal mono-atoms
  • Preparation method of metal mono-atoms

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preparation example Construction

[0018] The preparation method of the metal single atom proposed by the present invention comprises the following steps:

[0019] (1) Use a precursor and a solvent to form a precursor solution with a mass-volume concentration of 0.01-60 mg / ml. The precursor is a compound of a metal single atom, and the metal single atom is Pt, Ag, Au, Any one of Pd, Rh, Ir, Ru, Co, Ni and Cu, and the solvent is any one of water, ethylene glycol, ethanol, tetraethylene glycol, dimethylformamide or formaldehyde kind;

[0020] (2) freezing the precursor solution prepared in step (1) into ice cubes, processing the ice cubes in a set environment, setting the environment as a light field or a thermal field, to obtain metal monoatomic ice cubes;

[0021] (3) placing the metal monoatomic ice cube obtained in the above step (2) in a dark environment to melt naturally to obtain a metal monoatomic solution;

[0022] (4) Mix the metal single atom solution of the above step (3) with the load material to o...

Embodiment 1

[0028] Preparation of Pt single atoms.

[0029] First, configure the precursor solution that needs to be tested, and use chloroplatinic acid and deionized water to make a 3 mg / ml chloroplatinic acid solution. The configuration environment should be a dark environment to prevent other stray light from affecting the chloroplatinic acid. The solution was snap frozen into ice cubes with liquid nitrogen. Put ice cubes in a freeze dryer at -25°C with a light intensity of 0.89mW / cm 2 UV light for one hour. Finally, the ice cubes after ultraviolet irradiation were stored in a dark environment, and the Pt single-atom solution could be obtained after the ice cubes completely melted naturally. The Pt single atom solution was mixed with the mesoporous carbon solution, wherein the mass percentage of Pt single atom was 3%. The mixed solution was filtered, the filtrate was washed with water until all unreacted precursors were removed, and the filtrate was dried at room temperature for 15 ...

Embodiment 2

[0031] Preparation of Pt single atoms.

[0032] First, configure the precursor solution that needs to be tested, and use potassium chloroplatinate and a mixture of ultrapure water and ethanol (volume concentration of ethanol is 8%) to prepare a 0.5 mg / ml potassium chloroplatinate solution. The solution was snap frozen into ice cubes with liquid nitrogen. Put ice cubes in a high and low temperature alternating test box at -5°C with a light intensity of 15mW / cm 2 UV light for 5 minutes. Finally, the ice cubes after ultraviolet irradiation were stored in a dark environment, and the Pt single-atom solution could be obtained after the ice cubes completely melted naturally. The Pt single atom solution is mixed with the ZSM molecular sieve solution, wherein the mass percentage of the Pt single atom is 1%. The mixed solution was filtered, the filtrate was washed with water until all unreacted precursors were removed, and the filtrate was dried at room temperature for 15 hours to ob...

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Abstract

The invention relates to a preparation method of metal mono-atoms and belongs to the technical field of materials science and engineering. The metal mono-atoms prepared through the method may include: Pt, Ag, Au, Pd, Rh, Ir, Ru, Co, Ni and Cu, and metal mono-atoms supported on TiO2, zinc oxide, cerium oxide, aluminum oxide, silicon oxide, ferric oxide, manganese oxide, C3N4, mesoporous carbon, ultrathin carbon films, graphene, carbon nano tubes or molecular sieve materials, etc. The method includes the steps of: preparing a precursor solution in a certain concentration, and freezing the solution; and under an ice phase, processing ice cubes by means of external field or reaction between reactants in the ice cubes, and when the ice cubes are molten, a mono-atom solution is finally produced; mixing the mono-atom solution with different materials, performing ultrasonic treatment, filtration, cleaning and drying to finally obtain the mono-atoms supported on various materials. The preparation method is quick, has high product density, allows mass production, is high in efficiency and has wide application range, and compared with a co-precipitation method and an impregnation method, the method has significant advantages.

Description

technical field [0001] The invention relates to a method for preparing a metal single atom, which belongs to the technical field of material science and engineering. Background technique [0002] When the material is reduced from the macroscopic body to the nanometer scale, the subsequent reduction will eventually realize the single atomic scale material. Due to the sharply increased surface free energy, quantum size effect, unsaturated coordination environment and metal-support interaction, single-atom materials have excellent and unique physical and chemical properties. Single-atom materials, especially those that can be used as catalysts, have been extensively studied due to their complete atom utilization and more active sites. Since the Zhang Tao group first successfully prepared the iron oxide (FeO x ) single-atom Pt / FeO on the support x Catalysts, high catalytic activity and stability in CO oxidation and CO selective oxidation reactions and the concept of single-at...

Claims

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Application Information

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IPC IPC(8): B01J23/42B01J23/44B01J23/46B01J23/50B01J23/52B01J23/63B01J23/656B01J23/66B01J23/72B01J23/75B01J23/755B01J27/24B01J29/00B01J29/04
CPCB01J23/42B01J23/44B01J23/462B01J23/464B01J23/468B01J23/50B01J23/52B01J23/63B01J23/6562B01J23/66B01J23/72B01J23/75B01J23/755B01J27/24B01J29/00B01J29/04B01J35/391B01J35/33
Inventor 伍晖魏呵呵黄凯
Owner TSINGHUA UNIV
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