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Accessing photoresponsive copper selenide nanomaterials and thin films through tetranuclear Cu(I) pyridylselenolate cluster
Journal of Materials Science ( IF 4.5 ) Pub Date : 2020-08-10 , DOI: 10.1007/s10853-020-05033-3
Gourab Karmakar , Adish Tyagi , Amey P. Wadawale , Alpa Y. Shah , Gotluru Kedarnath , Amit P. Srivastava , Vishal Singh

The development of single-source molecular precursor for the synthesis of nanomaterials with controlled size and morphology has led to important scientific discoveries in past few decades. Herein, we describe the synthesis of air and moisture stable copper cluster complex with 5-methyl-2-pyridylselenolate, [Cu{2-SeC5H3(Me-5)N}]4 as molecular precursor for copper selenide nanomaterials and thin films. The complex was obtained in good yield, and the purity of the complex was evaluated through multi-nuclear NMR spectroscopy. The complex upon recrystallization in chloroform and toluene produces different polymorphs whose molecular structures were unambiguously established from single-crystal X-ray diffraction technique. Thermolysis of the complex in selected high-boiling solvents afforded phase-pure Cu1.8Se nanostructures. Thin films of phase-pure Cu5Se4 were also deposited by AACVD employing [Cu{2-SeC5H3(Me-5)N}]4 on glass and silicon substrates at different temperatures. The effect of higher temperature is perceived in drastic morphology change from nanosheets to a mixture of nanosheets and nanowires of Cu5Se4 on glass substrate. The nanostructures and thin films were characterized by pXRD, EDS, SEM and TEM techniques. The direct band gaps of the nanomaterials as deduced from diffuse reflectance spectroscopy are in the range 2.74–2.86 eV. The profound effect of solvent on phase purity, morphology and band gap of the nanostructures has also been investigated thoroughly. The nanostructures demonstrated prompt photoresponse which make them suitable candidate for non-toxic and low-cost photon absorber material. A tetranuclear Cu(I) complex with 5-methyl-2-pyridylselenolate ligand has been prepared and crystallized in two polymorphic forms, namely monoclinic [Cu{2-SeC5H3(Me-5)N}]4·C6H5CH3 and triclinic [Cu{2-SeC5H3(Me-5)N}]4. The complex was subjected to undergo thermolysis and AACVD to prepare Cu1.8Se nanomaterials and Cu5Se4 thin films, respectively. The nanomaterials and thin films were characterized using pXRD, SEM and TEM techniques to understand the phase purity and morphology. Fast switching characteristics of the nanomaterials have been established by switching characteristics.

中文翻译:

通过四核 Cu(I) pyridylselenolate 簇获取光响应硒化铜纳米材料和薄膜

在过去的几十年中,用于合成尺寸和形态可控的纳米材料的单源分子前体的开发已经导致了重要的科学发现。在此,我们描述了用 5-methyl-2-pyridylselenolate [Cu{2-SeC5H3(Me-5)N}]4 作为硒化铜纳米材料和薄膜的分子前体合成空气和水分稳定的铜簇复合物。以良好的收率获得了配合物,并通过多核核磁共振光谱评估了配合物的纯度。该复合物在氯仿和甲苯中重结晶后产生不同的多晶型物,其分子结构由单晶 X 射线衍射技术明确确定。复合物在选定的高沸点溶剂中的热解提供相纯的 Cu1.8Se 纳米结构。相纯 Cu5Se4 薄膜也通过 AACVD 在不同温度下使用 [Cu{2-SeC5H3(Me-5)N}]4 沉积在玻璃和硅基板上。在玻璃基板上从纳米片到纳米片和 Cu5Se4 纳米线的混合物的剧烈形态变化中感知到更高温度的影响。通过 pXRD、EDS、SEM 和 TEM 技术对纳米结构和薄膜进行表征。从漫反射光谱推导出纳米材料的直接带隙在 2.74-2.86 eV 范围内。溶剂对纳米结构的相纯度、形态和带隙的深远影响也得到了彻底的研究。纳米结构表现出迅速的光响应,这使其成为无毒和低成本光子吸收材料的合适候选者。制备了具有 5-methyl-2-pyridylselenolate 配体的四核 Cu(I) 配合物,并以两种多晶型形式结晶,即单斜 [Cu{2-SeC5H3(Me-5)N}]4·C6H5CH3 和三斜 [Cu{ 2-SeC5H3(Me-5)N}]4。对该配合物进行热解和 AACVD,分别制备 Cu1.8Se 纳米材料和 Cu5Se4 薄膜。使用 pXRD、SEM 和 TEM 技术对纳米材料和薄膜进行表征,以了解相纯度和形态。纳米材料的快速开关特性已经通过开关特性建立。分别。使用 pXRD、SEM 和 TEM 技术对纳米材料和薄膜进行表征,以了解相纯度和形态。纳米材料的快速开关特性已经通过开关特性建立。分别。使用 pXRD、SEM 和 TEM 技术对纳米材料和薄膜进行表征,以了解相纯度和形态。纳米材料的快速开关特性已经通过开关特性建立。
更新日期:2020-08-10
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