Patra Chitta Ranjan, Patra Sujata, Gabashvili Alexandra, Mastai Yitzhak, Koltypin Yuri, Gedanken Aharon, Palchik Valery, Slifkin Michael A
Department of Chemistry, Kanbar Laboratory for Nanomaterials, Bar-Ilan University Center for Advanced Materials and Nanotechnology, Bar-Ilan University, Ramat-Gan 52900, Israel.
J Nanosci Nanotechnol. 2006 Mar;6(3):845-51. doi: 10.1166/jnn.2006.134.
In this article, a simple microwave route was applied for the synthesis of nanoflakes and dendrite-type beta-indium sulfide (In2S3) in high yield (> 97%), using a homogeneous mixture of indium(lll)chloride and thiourea in an ethylene glycol (EG)/polyethylene glycol (PEG400) solvent. The reaction was conducted in a simple domestic microwave oven (DMO). Powder X-ray diffraction (XRD), low resolution and high resolution transmission electron microscopy (LRTEM and HRTEM), selected area electron diffraction (SAED), and energy dispersive X-ray spectroscopy (EDS), were applied to investigate the crystallinity, structure, morphology, and composition of the In2S3 nano-materials. Both the as-synthesized and calcined In2S3 products were a body-centered tetragonal (bct) phase, observed by XRD and HRTEM. The length and width of the resulting nanoflakes were in the range of 70-600 nm and 4-10 nm, respectively. The optical band gap of the powder was determined by diffuse reflectance spectroscopy (DRS) and was found to be 2.44 eV. The electronic properties of the products were studied by measuring the optical absorption spectra using photoacoustic spectroscopy. The band gap calculated by this method was found to be 2.52 eV. A possible mechanism for the formation of nanoflakes/dendrites-type In2S3 was also discussed.
在本文中，采用一种简单的微波路线，以氯化铟（III）和硫脲在乙二醇（EG）/聚乙二醇（PEG400）溶剂中的均匀混合物为原料，高产率（>97%）合成了纳米片和树枝状β-硫化铟（In2S3）。反应在一台简单的家用微波炉（DMO）中进行。采用粉末X射线衍射（XRD）、低分辨率和高分辨率透射电子显微镜（LRTEM和HRTEM）、选区电子衍射（SAED）以及能量色散X射线光谱（EDS）来研究In2S3纳米材料的结晶度、结构、形态和组成。通过XRD和HRTEM观察到，合成态和煅烧后的In2S3产物均为体心四方（bct）相。所得纳米片的长度和宽度分别在70 - 600 nm和4 - 10 nm范围内。通过漫反射光谱（DRS）测定了该粉末的光学带隙，发现其为2.44 eV。通过光声光谱测量光学吸收光谱来研究产物的电子性质。通过该方法计算得到的带隙为2.52 eV。还讨论了形成纳米片/树枝状In2S3的可能机理。
