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1.
Nanoscale ; 13(25): 11289-11297, 2021 Jul 07.
Artigo em Inglês | MEDLINE | ID: mdl-34156049

RESUMO

Understanding of cobalt nanorods' (Co NRs) formation still remains challenging when it comes to enhancing their anisotropic properties applicable in magnetic or catalytic areas. Herein, we propose a mechanism for the morphological transition from spherical cobalt nanoparticles (NPs) to Co NRs over time (9 h) in a mixture of [CoCl(PPh3)3] and oleylamine (OAm). In the literature, we described how spherical Co NPs are synthesized via a disproportionation process. Based on in situ and pseudo in situ observations, two steps of this unique mechanism are characterized first by the dissolution of the spheres and then the regrowth in rods' shape in the presence of an OAm template. Furthermore, ex situ experiments show that these steps are the result of interdependent reactions occurring between Co NPs, cobalt(ii) and OAm. The latter plays numerous roles in this synthesis: as a surfactant, a disproportionation promoter, and a hydrogen source allowing the reduction of cobalt(ii) complexes; its ammonium salt derivative is involved in oxidative etching of Co NPs and it promotes the anisotropic growth in NRs. These coupling actions of reduction and etching generate two cobalt reservoirs of nuclei under thermodynamic conditions.

2.
Chem Commun (Camb) ; 55(64): 9539-9542, 2019 Aug 07.
Artigo em Inglês | MEDLINE | ID: mdl-31334515

RESUMO

We report herein the synthesis of symmetric and non-symmetric bis-amidinato-germylene Fe(CO)3 complexes, as well as the preparation of the corresponding disymmetric germylene-stannylene and germylene-silylene complexes by selective displacement of a carbonyl ligand under UV-a light irradiation. The symmetric bis-germylene Fe(CO)3 complex has been applied in the synthesis of iron germanide nanocrystals.

3.
Dalton Trans ; 47(42): 15114-15120, 2018 Oct 30.
Artigo em Inglês | MEDLINE | ID: mdl-30306994

RESUMO

The synthesis of iron germanide nanoparticles at the nanoscale is a challenging task. Here, we describe the preparation of nanocrystals of the hexagonal Fe1.67Ge phase via the thermolysis of single source precursors [{iPrNC(tBu)NiPr}RGe]Fe(CO)4 (where R = Cl, N(SiMe3)2) under mild conditions (200 °C). These bimetallic precursors and the corresponding germylenes [{iPrNC(tBu)NiPr}RGe] were fully characterized by spectroscopic techniques as well as single crystal X-ray diffraction. While the structural features of the molecular species were shown to be almost identical, the results of the thermolysis were highly dependent on the nature of R. When R = Cl, multimodal size distributions and non-controlled phases were obtained. In contrast, the thermolysis of [{iPrNC(tBu)NiPr}{N(SiMe3)2}Ge]Fe(CO)4 yielded pure ferromagnetic Fe1.67Ge nanoparticles with a mean diameter close to 6 nm and a narrow size distribution (<12%). These results were rationalized in terms of Ge-substituent bond energy thanks to a computational study.

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