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.

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的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。