Rozmanowski Tomasz, Krawczyk Piotr
Poznań University of Technology, Institute of Chemistry and Technical Electrochemistry Ul. Berdychowo 4 60-965 Poznań Poland
RSC Adv. 2024 Mar 28;14(15):10263-10269. doi: 10.1039/d3ra08536h. eCollection 2024 Mar 26.
The present work describes preparation of a graphite lead composite, its modification and the examination of basic physicochemical and electrochemical properties. Graphite lead composites are the products of reaction of lead chloride with flaky graphite performed in a molten salt system. The process was carried out at 450 °C for 96 hours. In the second stage, the obtained composites were subjected to thermal or chemical treatment in order to modify their physicochemical properties. The structure of the as prepared material has been examined by X-ray diffraction analysis. Transmission electron microscopy analysis (TEM) along with energy dispersive spectroscopy (EDS) have been used to determine the size as well as the distribution of Pb particles. To study the electrochemical properties of graphite-based lead composites, cyclic voltammetry and galvanostatic methods have been used. It has been proved that the thermally modified compound at 600 °C contains on its surface spherical particles of lead chloride and/or oxide with diameters varying from hundreds of nanometers to several micrometers. The acquired electrochemical results revealed that graphite/Pb composites exhibit good electrochemical activity towards the reversible reaction of Pb → Pb oxidation. Charge associated with the reversible transformation of Pb to Pb amounts to 15.72 C g and 14.62 C g for the original compound and the compound heated at 600 °C, respectively. It has been also proved that the highest level of structure modification of the composite is reached by its chemical treatment with hydrogen peroxide. However, the mentioned modification leads to the removal of the entire lead from the structure of the graphite matrix.
本工作描述了石墨铅复合材料的制备、改性以及基本物理化学和电化学性质的研究。石墨铅复合材料是在熔盐体系中氯化铅与片状石墨反应的产物。该过程在450℃下进行96小时。在第二阶段,对所得复合材料进行热处理或化学处理,以改变其物理化学性质。通过X射线衍射分析对制备态材料的结构进行了研究。利用透射电子显微镜分析(TEM)和能谱分析(EDS)来确定铅颗粒的尺寸和分布。为了研究石墨基铅复合材料的电化学性质,采用了循环伏安法和恒电流法。已证明在600℃下热改性的化合物在其表面含有直径从几百纳米到几微米不等的球形氯化铅和/或氧化物颗粒。所获得的电化学结果表明,石墨/Pb复合材料对Pb→Pb氧化的可逆反应表现出良好的电化学活性。原始化合物和在600℃下加热的化合物中与Pb向Pb的可逆转变相关的电荷量分别为15.72 C/g和14.62 C/g。还证明了用过氧化氢对复合材料进行化学处理可达到最高程度的结构改性。然而,上述改性导致石墨基体结构中的所有铅被去除。