Abstract:Nanocrystalline silver sulfide was successfully synthesized at room temperature and ambient pressure via a novel, safe, convenient and inexpensive redox reaction, using silver oxide, sulfur and polyformaldehyde as reactants and ethylenediamine as solvent. The products were characterized with XPS, XRD and TEM. XRD spectrum demonstrates a monoclinic Ag2S; TEM shows the products are rod-like nanoparticles with average diameter of 100 nm, its corresponding SAED reveals clear diffraction spots indexed as (120) and (3-03); XPS confirms the formation of Ag2S and indicates the sample’s surface stoichiometry of Ag∶S=1∶0.453. The control experiments show polyformaldehyde and ethylenediamine are both important in the formation of products. Ethylenediamine accelerates the reactions via dissolving silver oxide and sulfur and neutralizing the by-product formic acid.
叶 寅,邵名望*,吴正翠,倪友保 . 室温合成硫化银纳米粒子及其X射线光电子能谱表征[J]. 光谱学与光谱分析, 2005, 25(04): 553-555.
YE Yin, SHAO Ming-wang*, WU Zheng-cui, NI You-bao . Synthesis of Ag2S Nanoparticles at Room Temperature and Their Characterization with XPS . SPECTROSCOPY AND SPECTRAL ANALYSIS, 2005, 25(04): 553-555.
[1] Xu R, Husmann A, Rosembaum T F, Saboungi M L, Enderby J E, Littlewood P B. Nature, 1997, 57: 390. [2] Boyce J B, Huberman B A. Phys. Rep., 1979, 189: 51. [3] LI Xiao-wei, HAN Li, GENG Ai-cong, YANG Shao-peng, FU Guang-sheng(李晓苇,韩 理,耿爱丛,杨少鹏,傅广生). Spectroscopy and Spectral Analysis(光谱学与光谱分析), 2004,24(7):787. [4] Henshaw G, Parkin I P, Shaw G. Chem. Commun., 1996: 1095. [5] Warren C J, Haushalter R C, Bocarsly A B. J. Alloys Compd., 1995, 175: 229. [6] Henshaw G, Parkin I P, Shaw G. J. Mater. Sci. Lett., 1996, 15: 1742. [7] Henshaw G, Parkin I P, Shaw G. J. Chem. Soc. Dalton. Trans., 1997: 231. [8] Wingrove A S, Caret R L. Organic Chemistry, New York: Haper & Row, 1981. [9] Muilenberg G E, Wager C D, Riggs W M, Davis L E, Moulder J F. (ED). Handbook of X-ray Photoelectron Spectroscopy. New York: Perking-Elmer Corp., 1979. [10] Li B, Xie Y, Liu Y, Huang J X, Qian Y T. J. Solid State Chem., 2001, 158: 260.