Exploration of the Smallest Diameter Tin Nanowires Achievable with Electrodeposition: Sub 7 nm Sn Nanowires Produced by Electrodeposition from a Supercritical Fluid.

Electrodeposition of Sn from supercritical difluoromethane has been performed into anodic alumina templates with pores down to 3 nm in diameter and into mesoporous silica templates with pores of diameter 1.5 nm. Optimized deposits have been characterized using X-ray diffraction, scanning electron microscopy, and scanning transmission electron microscopy (bright field, high-angle annular dark field, and energy-dispersive X-ray elemental mapping). Crystalline 13 nm diameter Sn nanowires have been electrodeposited in symmetric pore anodic alumina. Direct transmission electron microscopy evidence of sub 7 nm Sn nanowires in asymmetric anodic alumina has been obtained. These same measurements present indirect evidence for electrodeposition through 3 nm constrictions in the same templates. A detailed transmission electron microscopy study of mesoporous silica films after Sn deposition is presented. These indicate that it is possible to deposit Sn through the 1.5 nm pores in the mesoporous films, but that the nanowires formed are not stable. Suggestions of why this is the case and how such extreme nanowires could be stabilized are presented.

Electrodeposition of tin nanowires from a dichloromethane based electrolyte.

Tin was electrodeposited from a dichloromethane-based electrolyte at ambient temperature into gold coated anodic alumina membranes with nanoscale pores. The tin nanowires are mainly 〈200〉 aligned, together with some 〈101〉 and 〈301〉 wires. Partial filling of the structure and a distribution of wire lengths was found. Grafting of the pores with hydrophobic surface groups was trialled as a means of modifying the deposition, however, it did not increase the proportion of pores in which wires grew. Under potentiostatic conditions the limited rates of nucleation and diffusion down the 1D pores control the growth of the nanowires.

In situ phase behaviour of a high capacity LiCoPO4 electrode during constant or pulsed charge of a lithium cell.

The phase changes that occur during lithium extraction from LiCoPO4 in lithium half-cells were studied using synchrotron X-ray diffraction. The existence of two two-phase regions with an intermediate phase present was observed. Significant variations in the composition of the phases of nominal stoichiometry LiCoPO4, Li2/3CoPO4 and CoPO4 resulted in unit cell volume variations. On current pulsing, lattice parameter shifts and phase recovery were directly observed.