超临界流体沉积法对钯铜纳米粒子制备的影响
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The effect of supercritical fluid deposition method on the preparation of palladium-copper nanoparticles
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    摘要:

    以乙酰丙酮钯、乙酰丙酮铜为金属前驱体,以氧化铝球为载体,采用超临界流体沉积法(SCFD)制备氧化铝球负载的平均粒径≤10 nm的钯铜纳米粒子。采用高角度环形暗场-扫描透射电子显微镜(HAADF-STEM)、X射线衍射(XRD)和称重法对钯铜纳米粒子的负载状况、粒径分布进行表征。结果表明,沉积温度与沉积压力对钯铜纳米粒子的粒径有重要影响,在65 ℃、15 MPa时,钯铜纳米粒子的平均粒径可达2.37 nm。在金属前驱体投料量一定时,沉积时间存在最佳值。助溶剂的选择影响钯铜纳米粒子的平均粒径与粒径分布,在65 ℃、15 MPa下,使用8 mL二氯甲烷作为助溶剂,钯铜纳米粒子的平均粒径降至1.81 nm。随着Pd理论负载量的增加,钯铜纳米粒子的平均粒径先降后增,当Pd理论负载量为0.50%时,出现最小值1.81 nm。

    Abstract:

    Palladium-copper nanoparticles which average particle size less than 10 nm were deposited on alumina balls by supercritical fluid deposition (SCFD) method. using alumina balls as carrier and palladium acetylacetonate and copper acetylacetonate as precursors. High-angle annular dark field-scanning transmission election microscope (HAADF-STEM), X-ray diffraction (XRD) and weighing methods were used to characterize the loading status and particle size distribution of palladium-copper nanoparticles. The results showed that the deposition temperature and the deposition pressure had important effects on the particle size of palladium-copper nanoparticles. The average particle size of palladium-copper nanoparticles could reach 2.37 nm at 65 ℃ and 15 MPa. For a fixed amount of metal precursor, the deposition time had an optimal value. The selection of co-solvent affects the particle size distribution and the average particle size of palladium-copper nanoparticles. At 65 ℃ and 15 MPa, when 8 mL of dichloromethane was used as a co-solvent, the average particle size of the palladium-copper nanoparticles was reduced to 1.81 nm. With the increase of Pd theoretical loading, the average particle size of palladium-copper nanoparticles decreased first and then increased. When Pd theoretical loading was 0.50%, the average particle size reached the minimum value 1.81 nm.

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魏炜,王焘,董超,韩宇,刘凤霞,刘志军.超临界流体沉积法对钯铜纳米粒子制备的影响[J].精细化工,2022,39(4):0

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  • 收稿日期:2021-12-13
  • 最后修改日期:2022-01-20
  • 录用日期:2022-01-21
  • 在线发布日期: 2022-01-29
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