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用机械合金化方法快速合成了Fe Se1-x(0.04≤x≤0.12)样品,在氩气保护下进行退火处理,研究了样品在不同退火状态下的物相、电性能和磁性能。结果表明:样品中的主相为β-Fe Se超导相;在673 K退火30 min后,在温度7 K附近样品的磁化强度和电阻率明显降低,但是没有观察到零电阻和完全抗磁性;在673 K进行第二次退火20 h后,观察到了零电阻现象,x=0.04、0.08和0.12样品的零电阻转变温度分别为6.0、6.4和6.6 K;样品内存在强磁性的铁磁性/亚铁磁性杂相,掩盖了样品中超导相的完全抗磁性;样品的上临界磁场可达230 k Oe。
The samples of Fe Se1-x (0.04≤x≤0.12) were synthesized rapidly by mechanical alloying and annealed under argon. The phase, electrical and magnetic properties of the samples were investigated under different annealing conditions. The results show that the main phase in the sample is β-Fe Se superconducting phase. After annealed at 673 K for 30 min, the magnetization and resistivity of the sample at 7 K are obviously decreased, but zero resistance and complete diamagnetism are not observed ; Zero-resistance was observed after a second anneal at 673 K for 20 h. The zero-resistance transition temperatures were 6.0, 6.4 and 6.6 K for samples x = 0.04, 0.08 and 0.12, respectively. Ferromagnetic / Ferrimagnetic heterophase masks the complete diamagnetic properties of the superconducting phase in the sample; the upper critical magnetic field of the sample can reach 230 k Oe.