Synthesis of mesostructured lamellar lead sulfide in acidic media
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nxiong Ke, Jianmin Li,a) and Shemin Lu Department of Chemical Physics, University of Science and Technology, Hefei, Anhui 230026, People’s Republic of China
Guien Zhou and Shuyuan Zhang Structure Research Laboratory, University of Science and Technology, Hefei, Anhui 230026, People’s Republic of China (Received 2 October 2002; accepted 17 December 2002)
Mesostructured lamellar lead sulfide has been synthesized for the first time at room temperature in acidic media, employing sodium dodecyl sulfonate (SDS) as template and soluble lead salts, and hydrated sodium sulfide as the inorganic sources. The material was chiefly characterized by x-ray powder diffraction, high-resolution transmission electron microscopy, Raman spectroscopy, x-ray photoelectron spectroscopy, and thermogravimetric analysis. In the material, the Pb:S molar ratio for the inorganic phase is about 1:1.2, with a distance of about 2.7 nm between the inorganic layers.
Since the demonstration of the synthesis of multichip module (MCM) mesoporous silicates by the supramolecular templating approach,1,2 numerous other mesoporous silicates and metal oxides have been prepared.3 Although mesoporous silicates and metal oxides could be potentially applied as catalysts and absorbents, they lack unique electronic or photonic properties.4 Bulk materials combining mesoscale structure with semiconducting and optoelectronic features have attracted much interest recently, which could potentially be applied in fields of photocatalysis, nanotechnology, etc.; such characteristics may be expected in mesoporous nonoxidic semiconductor materials such as metal sulfides.4,5 However, the lack of suitable precursors and thermodynamic stability of sulfides in the presence of oxygen hinders the preparation of mesostructured sulfides.6,7 Until now, there have been only a few reports on mesostructured chalcogenides.6–10 Lead sulfide, a narrow direct band gap material with Eg of 0.41 ev at the L point of the Brillouin zone,11 has potential applications in luminescence devices. Here, we report for the first time the synthesis of lamellar mesostructured lead sulfide, using soluble lead salts and
a)
Address all correspondence to this author. e-mail: [email protected] J. Mater. Res., Vol. 18, No. 3, Mar 2003
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hydrated sodium sulfide as the inorganic sources with sodium dodecyl sulfonate as template in acidic media at room temperature. However, our attempts to prepare mesostructured lead sulfide with cationic and neutral surfactants instead of anionic surfactants were unsuccessful. A typical synthesis of the mesostructured material was achieved by the following experiment: 2.0 g C12H25SO3Na (6.4 mol) and 0.95 g Pb(Ac)2 ⭈ 3H2O (2.5 mmol) was dissolved in 30 ml 2.5 M acetate (HAc) solution; 0.72 g Na2S ⭈ 9 H2O (3.0 mmol) in 6 ml of deionized water was added to this solution slowly with stirring. After stirring for 3 h, the mixture (pH ⳱ 2.5) was aged for 100 h at room temperature. The resulting product was filtered, washed with etha
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