LaFeAsO纳米晶的中低温合成与表征

doi:10.15541/jim20150218

无机材料学报 ›› 2015, Vol. 30 ›› Issue (12): 1273-1277.DOI: 10.15541/jim20150218 CSTR: 32189.14.10.15541/jim20150218

LaFeAsO纳米晶的中低温合成与表征

张德兴¹, 孙云蕾², 阿布都外力·阿布力米提², 曹光旱²

(1. 安徽师范大学化学与材料科学学院, 芜湖241000; 2. 浙江大学物理系, 杭州 310027)

收稿日期:2015-05-08 修回日期:2015-06-20 出版日期:2015-12-20 网络出版日期:2015-11-24
作者简介:张德兴(1964–), 男, 实验师. E-mail: zdxzwy@mail.ahnu.edu.cn
基金资助:
国家自然科学基金(90922002) National Natural Science Foundation of China (90922002)

Low-temperature Synthesis and Characterizations of LaFeAsO Nanocrystals

ZHANG De-Xing¹, SUN Yun-Lei², ABULIMIT Abuduweli², CAO Guang-Han²

(1. College of Chemistry and Materials Science, Anhui Normal University, Wuhu 241000, China; 2. Department of Physics, Zhejiang University, Hangzhou 310027, China)

Received:2015-05-08 Revised:2015-06-20 Published:2015-12-20 Online:2015-11-24
About author:ZHANG De-Xing. E-mail: zdxzwy@mail.ahnu.edu.cn

摘要/Abstract

摘要：

研究了铁基超导母体化合物LaFeAsO的低温固相反应合成及表征。实验以La₂O₃、LaCl₃以及BaFe₂As₂为原料, 通过球磨混合, 成功地在中低温(~500℃)下实现固相反应, 从而获得LaFeAsO纳米晶。采用X射线衍射Scherrer公式, 估算其平均晶粒尺寸小于100 nm。低温电阻测量表明, LaFeAsO纳米晶的自旋密度波反常变得不显著, 且其转变温度明显下降。采用晶粒尺寸效应和晶胞参数影响对这种现象进行了解释。

关键词: LaFeAsO, 中低温固相反应, 纳米晶, 自旋密度波

Abstract:

LaFeAsO as a parent compound of iron-based superconductor was synthesized at low temperatures. The mixtures of La₂O₃, LaCl₃ and BaFe₂As₂ were ball-milled and the pressed pellets were sintered at 500℃ in vacuum. And nanocrystals of LaFeAsO were formed during the solid-state reaction. The solid-state reaction temperature for preparing LaFeAsO is 200℃ lower than the literature reported. The average crystallite size of the as-prepared LaFeAsO is less than 100 nm, as estimated by the X-ray diffraction Scherrer formula. Meanwhile, the c axis of the unit cell is increased by 0.001 nm, primarily stemming from the nanosize effect. Electrical resistivity measurement shows that the spin-density-wave anomaly becomes unremarkable, accompanied by a significant decrease in the transition temperature. The phenomena are discussed in terms of crystallite-size effect and the influence of lattice parameters.

Key words: LaFeAsO, low-temperature solid-state reaction, nanocrystals, spin-density wave

中图分类号:

O614

张德兴, 孙云蕾, 阿布都外力阿布力米提, 曹光旱. LaFeAsO纳米晶的中低温合成与表征[J]. 无机材料学报, 2015, 30(12): 1273-1277.

ZHANG De-Xing, SUN Yun-Lei, ABULIMIT Abuduweli, CAO Guang-Han. Low-temperature Synthesis and Characterizations of LaFeAsO Nanocrystals[J]. Journal of Inorganic Materials, 2015, 30(12): 1273-1277.

图/表 5

图1 合成LaFeAsO不同阶段下样品的XRD谱图

Fig. 1 XRD patterns of the samples in different stages of the low-temperature solid-state reaction for synthesizing LaFeAsO. From bottom to top: (a) mixtures of La2O3, LaCl3 and BaFe2As2; (b) the mixture after ball milling for 6 h; (c) the pellet sintered at 500℃ for 50 h; (d) the pellet re-sintered at 600℃ for 50 h. As a comparison, the XRD pattern of LaFeAsO polycrystals, prepared by a soild-state reaction at 1100℃, is also presented on the top

表1 室温下LaFeAsO纳米晶和多晶的晶胞参数以及由Scherrer公式估算的晶粒大小

Table 1 Lattice parameters at room temperature and the crystalline-grain sizes for the as-prepared LaFeAsO nanocrystals and polycrystals

图2 在600℃真空烧结LaFeAsO样品的扫描电镜照片(a)以及对小颗粒所采集的典型X射线能谱图(b)

Fig. 2 SEM image (a) of the LaFeAsO sample sintered at 600℃ and typical EDX spectrum (b) for the small particles. The bright large-sized particles are insulating byproduct BaCl2. The dark small-sized particles (~200 nm) are conducting LaFeAsO

图3 在500、600和1100℃烧结而成的LaFeAsO样品的电阻率-温度曲线

Fig. 3 Temperature dependence of resistivity for the LaFeAsO samples sintered at 500℃, 600℃ and 1100℃. The vertical axis of the lower plot adopts the derivative dρ/dT, in which the data are displaced downward for clarity

图4 在500℃和1100℃烧结而成的LaFeAsO的磁化率-温度曲线

Fig. 4 Temperature dependence of magnetic susceptibility for the LaFeAsO samples sintered at 500℃ right axis and 1100℃ leftaxis, respectively. The sample by solid-state reaction at 500℃ basically shows a Curie-Weiss paramagnetic behavior, yet it deviates from the Curie-Weiss fit (represented by the solid line) below 50 K

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LaFeAsO纳米晶的中低温合成与表征

Low-temperature Synthesis and Characterizations of LaFeAsO Nanocrystals

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