Max-Planck-Institut für Chemische Physik fester Stoffe, Nöthnitzer Strasse 40, 01187 Dresden, Germany.
J Am Chem Soc. 2011 Jun 15;133(23):9112-8. doi: 10.1021/ja202869d. Epub 2011 May 20.
A two-step synthesis for the preparation of single-phase and nanoparticulate GaPd and GaPd(2) by coreduction of ionic metal-precursors with LiHBEt(3) in THF without additional stabilizers is described. The coreduction leads initially to the formation of Pd nanoparticles followed by a Pd-mediated reduction of Ga(3+) on their surfaces, requiring an additional annealing step. The majority of the intermetallic particles have diameters of 3 and 7 nm for GaPd and GaPd(2), respectively, and unexpected narrow size distributions as determined by disk centrifuge measurements. The nanoparticles have been characterized by XRD, TEM, and chemical analysis to ensure the formation of the intermetallic compounds. Unsupported nanoparticles possess high catalytic activity while maintaining the excellent selectivity of the ground bulk materials in the semihydrogenation of acetylene. The activity could be further increased by depositing the particles on α-Al(2)O(3).
两步合成法用于制备单相和纳米颗粒 GaPd 和 GaPd(2),通过离子金属前驱体与 LiHBEt(3)在 THF 中的共还原,无需添加额外的稳定剂。共还原最初导致 Pd 纳米颗粒的形成,然后通过 Pd 介导在其表面还原 Ga(3+),这需要额外的退火步骤。大多数金属间化合物颗粒的直径分别为 GaPd 和 GaPd(2)的 3nm 和 7nm,并且通过圆盘离心测量确定了意想不到的窄粒径分布。通过 XRD、TEM 和化学分析对纳米颗粒进行了表征,以确保形成金属间化合物。无载体纳米颗粒具有高催化活性,同时保持了在乙炔半氢化中基础块状材料的优异选择性。通过将颗粒沉积在α-Al(2)O(3)上,可以进一步提高活性。