Synthesis routes
to forming novel materials are oftentimes complicated
and indirect. For example, Ta2S5 has only been
found as an unwanted byproduct of certain chemical reactions, and
its properties were unknown. However, here we demonstrate the growth
of Ta2S5 wires with steel-like tensile strength,
which are also precursors for the first controlled synthesis of long,
mesoscopic Ta2O5 wires and superconducting Ta2O5–x
S
x
wires. Single-crystal wires of tantalum pentasulfide, Ta2S5, were first grown using vapor transport from
polycrystalline XTa2S5, sulfur, and TeCl4 in fused-quartz tubes, where X = Ba or Sr. Crystals form
as long wires with lengths on the order of a few centimeters and varying
cross sections as small as 25 μm2. They were found
to have steel-like tensile strength, and their crystal structure was
determined using X-ray diffraction to be monoclinic with space group P2/m and with lattice parameters a = 9.91(7) Å, b = 3.82(5) Å,
and c = 20.92(2) Å. Electrical resistivity measurements
reveal Ta2S5 to be a narrow band gap semiconductor
with E
g = 110 meV, while a Debye temperature
ΘD = 97.0(5) K is observed in specific heat. Tantalum
pentasulfide wires were then converted to insulating tantalum pentoxide
(Ta2O5) wires after calcinating them for 30
min in air at 900 °C. Finally, tantalum pentoxide wires were
converted to tantalum oxysulfide (Ta2O5–x
S
x
) wires after annealing
them in CS2 vapor for 30 min at 900 °C. The oxysulfide
crystal structure was determined using X-ray diffraction to be that
of β-Ta2O5. Electrical and magnetic measurements
reveal Ta2O5–x
S
x
to be metallic and superconducting with T
c = 3 K.