Khabbaz M, Entezari M H
Sonochemical Research Center, Department of Chemistry, Faculty of Science, Ferdowsi University of Mashhad, 91779 Mashhad, Iran; International Campus, Ferdowsi University of Mashhad, Mashhad, Iran.
Sonochemical Research Center, Department of Chemistry, Faculty of Science, Ferdowsi University of Mashhad, 91779 Mashhad, Iran; Environmental Chemistry Research Center, Department of Chemistry, Faculty of Science, Ferdowsi University of Mashhad, 91779 Mashhad, Iran.
J Colloid Interface Sci. 2016 May 15;470:204-210. doi: 10.1016/j.jcis.2016.02.055. Epub 2016 Feb 24.
The synthesis of stable pyrite nanocrystals (NCs) in a simple way is very difficult. A facile and single-stage ultrasonic synthesis route has been successfully developed for the preparation of pyrite (FeS2) NCs in 10min and 70°C. In this study, the influences of reaction time, temperature, and acoustic power on the formation of the target compound were considered. In addition, a comparison was made of the synthesis of pyrite NCs by sonication with 20kHz apparatus and by the classical method (without ultrasound). The as-prepared pyrite was characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), scanning electron microscopy (SEM), Raman spectrophotometry and energy-dispersive X-ray spectroscopy (EDS). The XRD of the sample prepared by classical method indicated a typical cubic FeS2 with space group Pa3 and the average size of 16nm. Sulfur as an impurity in the sample was verified by XRD analysis. The sample prepared by ultrasound showed two phases of pyrite, cubic and marcasite structures. The space groups were pa3 and pnnm, respectively and the average size was 28.8nm. According to the SEM images, the morphology of the synthesized pyrite using the two methods are closely the same. The FT-IR and Raman spectra presented the FeS, FeS and SS functional groups. In addition, the sono-synthesis of pyrite was done under milder conditions and in shorter time with better features than classical method.
以简单的方式合成稳定的黄铁矿纳米晶体(NCs)非常困难。已成功开发出一种简便的单步超声合成路线,可在10分钟和70°C的条件下制备黄铁矿(FeS₂)NCs。在本研究中,考虑了反应时间、温度和声功率对目标化合物形成的影响。此外,还比较了用20kHz仪器超声处理和经典方法(无超声)合成黄铁矿NCs的情况。通过X射线衍射(XRD)、傅里叶变换红外光谱(FT-IR)、扫描电子显微镜(SEM)、拉曼光谱仪和能量色散X射线光谱(EDS)对所制备的黄铁矿进行了表征。经典方法制备的样品的XRD表明其为典型的立方FeS₂,空间群为Pa3,平均尺寸为16nm。通过XRD分析证实了样品中硫作为杂质的存在。超声处理制备的样品显示出黄铁矿的两种相,即立方结构和白铁矿结构。空间群分别为pa3和pnnm,平均尺寸为28.8nm。根据SEM图像,用这两种方法合成的黄铁矿的形态非常相似。FT-IR和拉曼光谱显示了FeS、FeS和SS官能团。此外,与经典方法相比,黄铁矿的超声合成是在更温和的条件下、更短的时间内完成的,且具有更好的特性。