research papers
The crystalline structures of the superionic high-temperature copper selenides Cu2−xSe (0 < x < 0.25) produced using mechanical alloying were investigated using X-ray diffraction (XRD). The measured XRD patterns showed the presence of peaks corresponding to the crystalline superionic high-temperature α-Cu2Se phase in the as-milled sample, and its structural data were determined by means of a Rietveld refinement procedure. After heat treatment in argon at 473 K for 90 h, this phase transforms to the superionic high-temperature α-Cu1.8Se phase, whose structural data were also determined by Rietveld refinement. In this phase, a very low occupation of the trigonal 32(f) sites (∼ 3%) by Cu ions is found. In order to explain the evolution of the phases in the samples, two possible mechanisms are suggested: (i) the high mobility of Cu ions in superionic phases and (ii) the important diffusive processes in the interfacial component of samples produced by mechanical alloying.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768104007475/av5007sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768104007475/av5007Cu2Se_beforesup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768104007475/av5007Cu2Se_aftersup3.hkl |
Computing details top
(Cu2Se) top
Crystal data top
Cu2Se | Z = ? |
Mr = ? | Cu Kα radiation, λ = 1.5418 Å |
Cubic, F23 | T = 293 K |
a = 5.8164 (3) Å | × × mm |
V = ? Å3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Cu1 | 0.25 | 0.25 | 0.25 | 0.0* | |
Cu2 | 0.5 | 0.5 | 0.5 | 0.0* | .42 |
Cu3 | 0.3333 | 0.3333 | 0.3333 | 0.0* | .08 |
Cu4 | 0.6667 | 0.6667 | 0.6667 | 0.0* | .08 |
Se | 0 | 0 | 0 | 0.0* |
(Cu1.8Se) top
Crystal data top
Cu1.8Se | Z = ? |
Mr = ? | Cu Kα radiation, λ = 1.5418 Å |
Cubic, Fm3m | T = 293 K |
a = 5.7762 (3) Å | × × mm |
V = ? Å3 |
Crystal data top
Cu1.8Se | Z = ? |
Mr = ? | Cu Kα radiation |
Cubic, Fm3m | T = 293 K |
a = 5.7762 (3) Å | × × mm |
V = ? Å3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Cu1 | 0.25 | 0.25 | 0.25 | 5.2* | 0.8 |
Cu2 | 0.3333 | 0.3333 | 0.3333 | 1.7* | .03 |
Se | 0 | 0 | 0 | 3.6* |
Experimental details
(Cu2Se) | (Cu1.8Se) | |
Crystal data | ||
Chemical formula | Cu2Se | Cu1.8Se |
Mr | ? | ? |
Crystal system, space group | Cubic, F23 | Cubic, Fm3m |
Temperature (K) | 293 | 293 |
a (Å) | 5.8164 (3) | 5.7762 (3) |
V (Å3) | ? | ? |
Z | ? | ? |
Radiation type | Cu Kα | Cu Kα |
µ (mm−1) | ? | ? |
Crystal size (mm) | × × | × × |
Data collection | ||
Diffractometer | ? | ? |
Absorption correction | ? | ? |
No. of measured, independent and observed (?) reflections | ?, ?, ? | ?, ?, ? |
Rint | ? | ? |
Refinement | ||
R[F2 > 2σ(F2)], wR(F2), S | ?, ?, ? | ?, ?, ? |
No. of reflections | ? | ? |
No. of parameters | ? | ? |
No. of restraints | ? | ? |
Δρmax, Δρmin (e Å−3) | ?, ? | ?, ? |