纳米材料方面的制备英文文献

Large-scale synthesis of double cauliflower-like Sb 2S 3microcrystallines by hydrothermal

method

Lei Wu a ,Hanyue Xu b ,Qiaofeng Han a ,⇑,Xin Wang a

a Key Laboratory for Soft Chemistry and Functional Materials,Ministry of Education,China

b

School of Electronic and Optical Engineering,Nanjing University of Science and Technology,Nanjing 210094,China

a r t i c l e i n f o Article history:

Received 21December 2012

Received in revised form 20March 2013Accepted 21March 2013

Available online 4April 2013Keywords:

Cauliflower-like Assembled Surfactants

Microcrystallines

a b s t r a c t

The double cauliflower-like Sb 2S 3superstructures assembled by nanorods were prepared using SbCl 3and Na 2S Á9H 2O as raw materials,dodecyltrimethylammonium bromide (DTAB,C 15H 31BrN)as surfactant under acidic condition at 180°C for 30h.The structure,morphology and composition of the product were characterized by X-ray diffraction pattern (XRD),transmission electron microscopy (TEM),scanning elec-tron microscopy (SEM),X-ray photoelectron spectroscopy (XPS)and energy diffraction spectroscopy (EDS).The effect of reaction conditions including temperature,reaction time and surfactants on the sam-ple morphology was discussed and a possible mechanism for the formation of cauliflower-like Sb 2S 3was proposed.The cauliflower-like Sb 2S 3microcrystallines revealed broad spectrum response,which may have a good application prospect in solar energy utilization and photoelectric conversion fields.

Ó2013Elsevier B.V.All rights reserved.

1.Introduction

Antimony trisulfide (stibnite),a kind of layer-structured V–VI semiconductor material with a direct band gap of 1.5–2.2eV,pos-sesses excellent photosensitivity as well as thermoelectricity,which is widely used in microwave devices,electronic equipment,solar,thermoelectric cooling devices [1–5].

Compared with traditional materials,nanomaterials have re-ceived considerable attention due to their unique physical and chemical properties and wide applications in the fabrication of optical and electronic devices.Research on the controllable prepa-ration of nanomaterials with unique structures and morphologies has become an important field for developing nanomaterials.Spe-cially,a variety of self-assembling patterns of inorganic crystals with naturally inspired morphologies have been obtained.For example,Pilapong research group synthesized double-sheaves of Sb 2S 3crystals by using thiourea as sulfur source,antimony acetate as antimony source and copolymer as a crystal splitting agent un-der acidic condition at 200°C [6].Mo and co-workers prepared Sb 2S 3with nanorod,dentrites,straw-tied-like morphology via a precursor–solvothermal–pyrolysis route [7].Our group synthe-sized peanut-shaped Sb 2S 3superstructures by using xanthate as

precursors [8].A variety of novel morphologies of Sb 2S 3such as feather-like,radioactive dendrite-like,prism–sphere-like,prickly sphere-like,flower-like and plate–sphere-like aggregated by one-dimensional (1-D)building blocks were obtained by Hu et al.[9].Surfactants can effectively control morphologies and structures of nanoparticles because they can parcel at the particle surface through coordination or charge effect.Sb 2S 3nanoparticles with various morphologies have been prepared by using polyvinylpyr-rolidone (PVP)[10,11],macrogol 400(PEG-400)and emulsifier OP-10as the surfactants [12].

Herein,we describe the synthesis of cauliflower-like Sb 2S 3microcrystallines via a surfactant (dodecyltrimethylammonium bromide DTAB)assisted hydrothermal route by using SbCl 3and Na 2S as raw materials.As compared to flower-like Sb 2S 3micro-structures obtained by using potassium antimony tartrate as anti-mony source [13]or triethanolamine as solvent [14],raw materials were simpler and the morphology of the products were more reg-ular in our work.The effect of reaction time,reaction temperature,surfactant and the ratio of raw materials on the structures and morphology of the products was carefully investigated.

2.Experimental section 2.1.Synthetic procedure

In a typical experiment, 1.0g (4.4mmol)antimony trichloride (SbCl 3)was added to 20ml distilled water,and concentrated hydrochloric was added into the solution till white precipitate disappeared completely.4.2g (17.5mmol)so-

0925-8388/$-see front matter Ó2013Elsevier B.V.All rights reserved./10.1016/j.jallcom.2013.03.199

Corresponding author.Tel.:+862584315943.

E-mail addresses:hanqiaofeng@ ,hanqiaofeng@ (Q.Han).