Sokol Denis, Vieira Daniel E L, Zarkov Aleksej, Ferreira Mário G S, Beganskiene Aldona, Rubanik Vasili V, Shilin Aleksandr D, Kareiva Aivaras, Salak Andrei N
Institute of Chemistry, Faculty of Chemistry and Geosciences, Vilnius University, Naugarduko 24, LT-03225, Vilnius, Lithuania.
Department of Materials and Ceramics Engineering and CICECO - Aveiro Institute of Materials, University of Aveiro, 3810-193, Aveiro, Portugal.
Sci Rep. 2019 Jul 18;9(1):10419. doi: 10.1038/s41598-019-46910-5.
Single-phase magnesium-aluminium layered double hydroxide (LDH) intercalated with dihydrogen phosphate was successfully produced by hydration of nanopowder of the respective mixed metal oxide (MMO) obtained using sol-gel based method followed by a two-step anion exchange hydroxide-to-chloride and chloride-to-phosphate. The MMO with the metal cation ratio of Mg/Al = 2:1 was prepared using the aqueous sol-gel method. Processes of the parent MgAl-OH LDH formation and the successive anion-exchanges, ОН → Cl and Cl → HPO, were considerably accelerated via the application of high-power (1.5 kW) ultrasound. The crystalline phases formed at all stages of the MgAl-HPO LDH production were characterized using X-ray diffraction, scanning electron microscopy, scanning transmission electron microscopy, inductive coupled plasma optical emission spectroscopy, Fourier transform infrared spectroscopy, and thermogravimetric analysis. Based on the data of chemical analysis and the XRD data, the type of the intercalated phosphate anion was determined and the arrangement of this anion in the interlayer was modelled.
通过基于溶胶 - 凝胶法获得的相应混合金属氧化物(MMO)纳米粉末水合,然后经过两步阴离子交换(氢氧化物到氯化物以及氯化物到磷酸盐),成功制备了插层有磷酸二氢根的单相镁铝层状双氢氧化物(LDH)。采用水相溶胶 - 凝胶法制备了金属阳离子比为Mg/Al = 2:1的MMO。通过应用高功率(1.5 kW)超声,显著加速了母体MgAl - OH LDH的形成过程以及后续的阴离子交换过程,即OH→Cl和Cl→HPO₄²⁻。使用X射线衍射、扫描电子显微镜、扫描透射电子显微镜、电感耦合等离子体发射光谱、傅里叶变换红外光谱和热重分析对MgAl - HPO₄ LDH制备各阶段形成的晶相进行了表征。基于化学分析数据和XRD数据,确定了插层磷酸根阴离子的类型,并对该阴离子在层间的排列进行了建模。