Department of Nanotechnology Engineering, Mineral Industries Research Center, Shahid Bahonar University of Kerman, Kerman, Iran; Young Researchers Society, Shahid Bahonar University of Kerman, Kerman, Iran.
Department of Nanotechnology, Graduate University of Advanced Technology, Kerman, Iran.
Ultrason Sonochem. 2018 Mar;41:234-251. doi: 10.1016/j.ultsonch.2017.09.046. Epub 2017 Sep 28.
Reverse micelle (RM) and ultrasound assisted reverse micelle (UARM) were applied to the synthesis of novel thorium nanostructures as metal organic frameworks (MOFs). Characterization with different techniques showed that the Th-MOF sample synthesized by UARM method had higher thermal stability (354°C), smaller mean particle size (27nm), and larger surface area (2.02×10m/g). Besides, in this novel approach, the nucleation of crystals was found to carry out in a shorter time. The synthesis parameters of UARM method were designed by 2 factorial and the process control was systematically studied using analysis of variance (ANOVA) and response surface methodology (RSM). ANOVA showed that various factors, including surfactant content, ultrasound duration, temperature, ultrasound power, and interaction between these factors, considerably affected different properties of the Th-MOF samples. According to the 2 factorial design, the determination coefficient (R) of the model is 0.999, with no significant lack of fit. The F of 5432, implied that the model was highly significant and adequate to represent the relationship between the responses and the independent variables, also the large R-adjusted value indicates a good relationship between the experimental data and the fitted model. RSM predicted that it would be possible to produce Th-MOF samples with the thermal stability of 407°C, mean particle size of 13nm, and surface area of 2.20×10m/g. The mechanism controlling the Th-MOF properties was considerably different from the conventional mechanisms. Moreover, the MOF sample synthesized using UARM exhibited higher capacity for nitrogen adsorption as a result of larger pore sizes. It is believed that the UARM method and systematic studies developed in the present work can be considered as a new strategy for their application in other nanoscale MOF samples.
反胶束(RM)和超声辅助反胶束(UARM)被应用于新型钍纳米结构作为金属有机骨架(MOF)的合成。不同技术的表征表明,通过 UARM 方法合成的 Th-MOF 样品具有更高的热稳定性(354°C)、更小的平均粒径(27nm)和更大的比表面积(2.02×10m/g)。此外,在这种新方法中,发现晶体的成核时间更短。通过 2 因子设计 UARM 方法的合成参数,并使用方差分析(ANOVA)和响应面法(RSM)系统地研究过程控制。ANOVA 表明,各种因素,包括表面活性剂含量、超声持续时间、温度、超声功率以及这些因素之间的相互作用,对 Th-MOF 样品的不同性质有很大影响。根据 2 因子设计,模型的确定系数(R)为 0.999,不存在显著的拟合不足。F 值为 5432,表明模型高度显著,足以表示响应与独立变量之间的关系,较大的 R-调整值表明实验数据与拟合模型之间存在良好的关系。RSM 预测,有可能生产出热稳定性为 407°C、平均粒径为 13nm、比表面积为 2.20×10m/g 的 Th-MOF 样品。控制 Th-MOF 性质的机制与传统机制有很大的不同。此外,由于较大的孔径,使用 UARM 合成的 MOF 样品对氮气吸附的容量更高。相信 UARM 方法和本工作中开发的系统研究可以被认为是在其他纳米级 MOF 样品中的应用的一种新策略。