Growth and Characterisation of Boron Rich Nanomaterials

In this study nanomaterials are grown in a solid state reaction at 1300C of boron, barium oxide and iron(II/III)oxide powders in an argon atmosphere. The nanomaterials are shown to be grown via vapour based method by growing the nanomaterials on a separate silicon wafer that has been sputtered with iron and placed downstream of the powders in the flow of argon. An area of the silicon wafer is kept free of iron by using a mask when sputtering the wafer. When nanomaterials are grown, the masked area remains free of nanomaterials. This shows that the presence of iron is vital for the nucleation of the nanomaterials and also indicates the possibility of growing these nanomaterials on targeted sites. The nanomaterials produced are examined and it is found that we have a presence of amorphous, crystalline and multiple twinned nanowires. The evidence collected suggests that 70% of the nanowires are twinned. The single crystal nanowires can be identified as boron carbide by comparing to diffraction pattern simulations of a boron carbide unit cell. The twinned diffraction pattern is shown to be due to different segments of the nanowire being in different diffraction condition by using Dark Field imaging. The Twinned wires are also shown to have at least four segments in a cyclic [001] twinning orientation in simultaneous diffraction condition by comparing to a twinned structure constructed from simulations. Elemental analysis using Electron Energy Loss Spectroscopy and Energy Dispersive X-ray shows that the composition of the nanomaterials is mainly boron and carbon. The role of the iron layer on the wafer is investigated to see how varying the thickness will affect the nanomaterials grown. It is successfully shown that an increase in the thickness of the iron layer results in a greater density of nanomaterials. However there is no great variation in the average diameter of the nanomaterials produced. The absence of a visible signal for iron in the Elemental analysis of nanostructure covered silicon wafer shows that the amount of iron in the sample has decreased during the reaction. However iron is found in small amounts in droplet structures at the tips of nanomaterials this is different to work done on a similar system at 1100C. This suggests that the role of the iron in the growth of these nanomaterials at this temperature is not yet understood. However this work has confirmed that the iron is essential for the nucleation of the nanomaterials, but post nucleation growth that was previously assumed to be a conventional VLS growth may switch to an oxide assisted growth mode.