Sub-nano metal catalyst as well as preparation method and application thereof
A metal catalyst and sub-nanometer technology, applied in the field of sub-nanometer catalysis, can solve the problems of precise control of the content and size of metal active components, harsh preparation conditions, etc.
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[0028] The invention provides a kind of preparation method of subnanometer metal catalyst, comprises the following steps:
[0029] mixing the carrier material and the diluent, coating the resulting mixture on the surface of the substrate, and forming a carrier material layer on the surface of the substrate after drying;
[0030] The surface of the carrier material layer is etched based on the pulse oxidation pretreatment to obtain a defect material rich in epoxy groups, and a defect material layer rich in epoxy groups is formed on the surface of the substrate; the oxidizing agent used in the pulse oxidation pretreatment for ozone;
[0031] Based on the atomic layer deposition method, by sequentially pulsing gaseous metal precursors and gaseous oxidants, metal deposition is performed on the surface of the epoxy-rich defect material layer to obtain subnano metals in the form of atomic dispersion. The sub-nanometer metal catalyst is obtained on the surface of the substrate.
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Embodiment 1
[0061] (1) Prepare graphene carrier material by rapid thermal expansion method (reference: Structural evolutionduring annealing of thermally reduced graphene nanosheets for application insupercapacitors.Carbon 2012,50,3572-3584), denoted as G1600, the epoxy group in the G1600 The content is 0.19at.%; the G1600 is mixed with ethanol, dispersed uniformly to obtain a suspension, the concentration of G1600 in the suspension is 0.01g / mL, and the suspension is coated on a quartz plate (the size is 8cm× 8cm) surface, after natural drying at room temperature (25°C), a G1600 layer (thickness ≤ 0.15cm) is formed on the surface of the quartz plate;
[0062] (2) Place the quartz plate containing the G1600 layer in the atomic layer deposition chamber (the volume of the atomic layer deposition chamber is about 500cm 3 ), the carrier gas is high-purity N 2 (99.999%), utilize atomic layer deposition technology to carry out ozone (O 3 ) etching, the set etching parameters are: chamber temper...
Embodiment 2
[0071] The subnano Pt / graphene catalyst was prepared with reference to the method of Example 1, the only difference from Example 1 was that G1600-O 3 The number of times of deposition treatment of Pt metal on the -60 surface is 1 time, and the subnano Pt / graphene catalyst (referred to as 1Pt / G1600-O 3 -60, the platinum content is 1.06wt.%, where "1" represents the number of depositions).
[0072] According to performance test method in embodiment 1, utilize 1Pt / G1600-O 3 -60 catalyzes the hydrolysis of ammonia borane to produce hydrogen. The test results show that 110 mL of H was produced in 21 minutes. 2 ; After six cycle stability tests according to the method in Example 1, about 80% of the initial reactivity was retained.
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