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由单源前体制备的热解和水热分解法制备的硫化铋:反应参数对形貌、微观结构和催化活性的影响。

Bismuth sulphides prepared by thermal and hydrothermal decomposition of a single source precursor: the effect of reaction parameters on morphology, microstructure and catalytic activity.

机构信息

Departamento de Química, Universidade Federal de Minas Gerais, Av. Antônio Carlos, 6627, Belo Horizonte, MG CEP 31270-901, Brazil.

出版信息

Phys Chem Chem Phys. 2013 Oct 14;15(38):16236-41. doi: 10.1039/c3cp51609a. Epub 2013 Sep 2.

DOI:10.1039/c3cp51609a
PMID:23994884
Abstract

Bismuth sulphides were prepared by thermal and hydrothermal decomposition of a precursor, bismuth tris-diethyldithiocarbamate, at different temperatures and times. The obtained results showed that the thermal decomposition of the precursor in a tube furnace was not very appropriate to control particle size and morphology. XRD results showed that at 310 °C the precursor was not fully decomposed but at 500 °C besides the orthorhombic bismuth sulphide, the metallic bismuth also started to be formed. At the highest temperature 1D crystals were formed with an apparent mean crystal size of 138 nm. However, hydrothermal decomposition was shown to be a very suitable method to control particle size and morphology just by varying some parameters such as temperature and time. For 6 hours reaction time, as temperature increased, the apparent mean crystal size decreased. The particle morphology was also very affected by this parameter, at 180 °C only 1D particles (nanorods) with lengths varying from 25 to 4700 nm were formed but at 200 °C not only 1D particles but also 2D particles were (nanosheets) obtained. Bismuth sulphide particles obtained at 180 °C and 24 hours reaction time were shown to be formed mostly by 2D particles compared to those obtained at 6 hours. It was clearly seen that the increase in reaction time and temperature led to the formation of bi-dimensional particles. The presence of 1D crystals in the samples obtained by hydrothermal decomposition at 180 °C/6 h and 180 °C/24 h is responsible for their high catalytic efficiency towards methylene blue dye degradation.

摘要

二硫化铋是通过热解和水热分解前驱体三乙基二硫代氨基甲酸铋在不同温度和时间下制备的。所得结果表明,在管式炉中热分解前驱体不太适合控制粒径和形态。XRD 结果表明,在 310°C 时,前驱体未完全分解,但在 500°C 时,除了正交相二硫化铋外,金属铋也开始形成。在最高温度下,形成了一维晶体,平均晶体尺寸为 138nm。然而,水热分解被证明是一种非常合适的方法,可以通过改变温度和时间等参数来控制粒径和形态。对于 6 小时的反应时间,随着温度的升高,平均表观晶体尺寸减小。颗粒形态也受到这个参数的很大影响,在 180°C 时,仅形成 1D 颗粒(纳米棒),长度从 25nm 到 4700nm 不等,但在 200°C 时,不仅形成了 1D 颗粒,还形成了 2D 颗粒(纳米片)。在 180°C 和 24 小时反应时间下获得的二硫化铋颗粒与在 6 小时下获得的相比,主要由二维颗粒组成。很明显,反应时间和温度的增加导致了二维颗粒的形成。在 180°C/6 h 和 180°C/24 h 下通过水热分解获得的样品中存在一维晶体,这是它们对亚甲基蓝染料降解具有高催化效率的原因。

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