Phase-pure crystalline zinc phosphide nanoparticles: Synthetic approaches and characterization

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Journal titleChemistry of Materials
Pages19251935; # of pages: 11
SubjectConstituent elements; Core shell structure; Nuclear magnetic resonance(NMR); Photovoltaic applications; Reaction mechanism; Synthetic approach; Synthetic strategies; Tri-n-octylphosphine; Chelation; Crystalline materials; Magic angle spinning; Nanoparticles; Phosphorus; Phosphorus compounds; Photoelectrons; Reaction intermediates; Synthesis (chemical); Transmission electron microscopy; X ray diffraction; X ray photoelectron spectroscopy; Zinc compounds; Zinc
AbstractZinc phosphide may have potential for photovoltaic applications due to its high absorptivity of visible light and the earth abundance of its constituent elements. Two different solution-phase synthetic strategies for phase-pure and crystalline Zn3P2 nanoparticles (∼3-15 nm) are described here using dimethylzinc and vary with phosphorus source. Use of tri-n-octylphosphine (TOP) with ZnMe2 takes place at high temperatures (∼350 C) and appears to proceed via rapid in situ reduction to Zn(0), followed by subsequent reaction with TOP over a period of several hours to produce Zn3P2 nanoparticles. Some degree of control over size was obtained through variance of the TOP concentration in solution; the average size of the particles decreases with increasing TOP concentration. With the more reactive phosphine, P(SiMe3)3, lower temperatures, ∼150 C, and shorter reaction times (1 h) are required. When P(SiMe3)3 is used, the reaction mechanism most likely proceeds via phosphido-bridged dimeric Zn(II) intermediates, and not metallic zinc species, as is the case with TOP. In all cases, the nanoparticles were characterized by a combination of X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and solution and solid-state magic-angle spinning (MAS) nuclear magnetic resonance (NMR) analyses. Surface investigation through a combination of MAS 31P NMR and XPS analyses suggests that the particles synthesized with TOP at 350 C possess a core-shell structure consisting of a crystalline Zn3P 2 core and an amorphous P(0)-rich shell. Conversely, the ligand and phosphorus sources are decoupled in the P(SiMe3)3 synthesis, resulting in significantly reduced P(0) formation. © 2014 American Chemical Society.
Publication date
AffiliationNational Research Council Canada (NRC-CNRC); National Institute for Nanotechnology (NINT-INNT)
Peer reviewedYes
NPARC number21272240
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Record identifierf3c815be-7732-4370-ab5d-a1de98ecfb88
Record created2014-07-23
Record modified2016-05-09
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