水热微乳液法制备低维硫化镍纳米晶  

Preparation of Low-dimensional Nickel Sulfide Nanocrystals via Microemulsion-assisted Hydrothermal Method

作　　者：陈德良[1] 高濂[1] 

机构地区：[1]中国科学院上海硅酸盐研究所高性能陶瓷与超微结构国家重点实验室,上海200050

出　　处：《高等学校化学学报》2004年第8期1407-1412,M004,共7页Chemical Journal of Chinese Universities

基　　金：国家重点基础研究发展规划项目 (批准号 :G19990 64 5 0 6)资助

摘　　要：以 W/O型微乳液 CTAB/正戊醇 /正己烷 /水为反应介质 ,以 CS2 为硫源 ,在 1 3 0℃水热条件下成功地合成了硫化镍二维纳米薄层片和一维纳米针 (管 ) .TEM结果表明 ,水热初期 ( 5 h)得到的是二维纳米薄层片 ,随着水热时间的延长 ( 1 5 h) ,层片结构消失 ,出现一维的空心纳米针结构 .XRD谱表明 ,纳米薄层片主要为六方相 Ni S1 .0 3,纳米针则为 Ni S1 .0 3与少量针镍矿相 Ni S的混合物 .所得的纳米层片很薄 ,其厚度小于 1 0nm;纳米针的直径为 3 0～ 1 5 0 nm,长度超过 1 0 0 0 nm.空心的纳米针及中间态结构表明 ,一维纳米针是由二维纳米薄层片卷曲而得到的 .二维薄层片结构的形成可归功于微乳液互不相溶的二相环境下低的 S2 -Nickel sulfide nanocrystals with novel morphologies of two-dimensional nanosheets and one-dimensional nanoneedles or nanotubes were successfully prepared in the CTAB/ n -pentanol/ n -hexane/water microemulsion under hydrothermal conditions at 130 ℃. XRD,TEM,SAED and TG-DSC were used to characterize the as-synthesized samples. TEM images show that nickel sulfide nanosheets with a small thickness(less than 10 nm) and nanoneedles with a hollow center(or nanotubes), ca . 50—150 nm in diameter and several microns in length,can be obtained by hydrothermally treating for 5 h and 15 h,respectively. XRD patterns show that the major phase of the nanosheets is hexagonal NiS 1.03 ,and that the nanoneedles are the mixture of hexagonal NiS 1.03 and a small amount of millerite NiS. The sulfuration reaction and the low-dimensional nanocrystal growth mechanism have been discussed in detail. The result reveals that the nanosheets firstly formed under the soft template action of the W/O microemulsion,and then the resulted nanosheets rolled up into one-dimensional nanoneedles or nanotubes.

关 键 词：纳米薄片 纳米针(管) W/O型微乳液 水热合成 硫化镍 

分 类 号：O614[理学—无机化学] TB383[理学—化学]