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高多孔 Co(II)-水杨酸金属有机骨架:合成、表征和磁性。

Highly porous Co(II)-salicylate metal-organic framework: synthesis, characterization and magnetic properties.

机构信息

Department of Materials Science, Indian Association for the Cultivation of Science, Jadavpur, Kolkata, 700 032, India.

出版信息

Dalton Trans. 2011 Mar 28;40(12):2932-9. doi: 10.1039/c0dt01483d. Epub 2011 Feb 14.

Abstract

A new porous Co(II)-salicylate metal-organic framework material has been synthesized hydrothermally through the reaction of Co(II) chloride with sodium salicylate under mild alkaline pH conditions. To get an idea about the structural aspect of the material from the powder X-ray diffraction (PXRD) pattern, MAUD program has been successfully utilized and the assigned peaks match very well with a new tetragonal phase (space group, P4mm) having the unit cell parameters: a = b = 12.957 (0.042) Å; c = 12.738 (0.019) Å; α = β = γ = 90°, V = 2138.73 Å(3). N(2) adsorption/desorption analyses suggested the material is highly porous in nature having high BET surface area and pore dimensions of 2.0-3.0 nm, which is within the range of small mesopores. Thermogravimetric analysis (TGA) revealed that the H(2)O molecules may be removed from the framework without collapsing the structure and the material is stable up to ca. 573 K. The material is characterized thoroughly by using different characterization tools such as TEM, SEM, UV-visible reflectance spectroscopy, FT IR spectroscopy and photoluminescence spectroscopy. X-Ray photoelectron spectroscopic (XPS) analysis was employed to understand the oxidation state of the cobalt atom and presence of other elements within the framework. The material shows interesting magnetic properties, where the magnetic moments monotonically increase with the decrease in temperature down to 9 K. Below 9 K there is a steep increase in magnetization on further lowering the temperature, thereby suggesting the onset of a long range ferromagnetic transition with ferromagnetic Curie temperature, T(C) = 8.5 K. Furthermore, the M-H curve at 2 K shows a clear hysteresis loop with a coercive field 150 Oe and remnant magnetization 0.8 μ(B)/f.u.

摘要

一种新的多孔 Co(II)-水杨酸金属有机骨架材料已经通过 Co(II) 氯化物与水杨酸钠在温和碱性 pH 条件下的水热反应合成。为了从粉末 X 射线衍射(PXRD)图谱中了解材料的结构方面,成功地利用了 MAUD 程序,并且指定的峰与一个新的四方相(空间群,P4mm)非常匹配,具有单元细胞参数:a = b = 12.957(0.042)Å;c = 12.738(0.019)Å;α = β = γ = 90°,V = 2138.73 Å(3)。N(2)吸附/解吸分析表明,该材料本质上是高度多孔的,具有高 BET 表面积和 2.0-3.0nm 的孔径,这在小介孔范围内。热重分析(TGA)表明,H(2)O 分子可以从骨架中去除而不会使结构坍塌,并且该材料在约 573K 下稳定。该材料通过使用不同的表征工具如 TEM、SEM、UV-可见反射光谱、FTIR 光谱和光致发光光谱进行了彻底的表征。X 射线光电子能谱(XPS)分析用于了解钴原子的氧化态和骨架中其他元素的存在。该材料表现出有趣的磁性,其中磁矩随着温度的降低单调增加,直至 9K。在 9K 以下,随着温度的进一步降低,磁化强度急剧增加,从而表明长程铁磁转变的开始,铁磁居里温度 T(C) = 8.5K。此外,在 2K 下的 M-H 曲线显示出明显的滞后环,矫顽场为 150Oe,剩余磁化强度为 0.8μ(B)/f.u.

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