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Synthesis and characterization of layered double hydroxides containing Nickel in unstable oxidation state + 3 in cationic sites
Journal of Solid State Chemistry ( IF 3.2 ) Pub Date : 2018-06-14 , DOI: 10.1016/j.jssc.2018.06.001
I.G. Ryltsova , O.V. Nestroinaya , O.E. Lebedeva , F. Schroeter , F. Roessner

A series of layered double hydroxides (LDH) with molar ratio M2⁺/M³ ⁺ = 3:1 and different degrees of aluminum substitution in the cationic sites by Ni3+ were prepared by precipitation from solution in the presence of sodium hypochlorite as an oxidizing agent. The synthesized samples were characterized by various techniques including powder X-ray Diffraction (XRD), Thermogravimetric and Differential Thermal Analysis (TG-DTA), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), Diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy and inverse Temperature-programmed Reduction (iTPR). The results indicate that single-phase LDHs were formed during synthesis and they were of a high degree of crystallinity. The thermal stability of LDHs did not decrease essentially with increasing Ni3+ content. The calcination at 600 °C led to the complete destruction of the layered structure and formation of mixed oxide phases. In iTPR experiments for as-synthesized LDHs the reduction of Ni3+ to Ni2+ took place above 400 °C, and the reduction of Ni2+ to Ni° occurred above 600 °C.



中文翻译:

阳离子位点含不稳定氧化态+ 3的层状双氢氧化物的合成与表征

一系列层状双氢氧化物(LDH)以摩尔比M的2 ⁺/立方米⁺= 3:1和不同程度的阳离子位置由镍铝取代3+通过沉淀在次氯酸钠的存在下制备从溶液作为氧化剂。合成的样品通过各种技术进行表征,包括粉末X射线衍射(XRD),热重和差热分析(TG-DTA),扫描电子显微镜(SEM),透射电子显微镜(TEM),漫反射红外傅里叶变换(DRIFT)光谱和反向程序升温还原(iTPR)。结果表明,在合成过程中形成了单相LDH,并且它们具有很高的结晶度。LDHs热稳定性基本上不会随着Ni3+含量的增加而降低600°C下的煅烧导致层状结构的完全破坏和混合氧化物相的形成。在用于合成的LDH的iTPR实验中,Ni3+还原为Ni2+发生在400°C以上,Ni2+还原为Ni°发生在600°C以上。

更新日期:2018-07-12
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