水热微乳液法制备低维硫化镍纳米晶

高等学校化学学报 ›› 2004, Vol. 25 ›› Issue (8): 1407.

水热微乳液法制备低维硫化镍纳米晶

陈德良, 高濂

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

收稿日期:2003-08-18 出版日期:2004-08-24 发布日期:2004-08-24
基金资助:
国家重点基础研究发展规划项目(批准号:G1999064506)资助

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

CHEN De-Liang, GAO Lian

State Key Lab of High Performance Ceramics and Superfine Microstructure, Shanghai Insititute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China

Received:2003-08-18 Online:2004-08-24 Published:2004-08-24

摘要/Abstract

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130℃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(5h)得到的是二维纳米薄层片,随着水热时间的延长(15h),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NiS_1.03,纳米针则为NiS_1.03与少量针镍矿相NiS的混合物.所得的纳米层片很薄,其厚度小于10nm;纳米针的直径为30～150nm,长度超过1000nm.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-释放速率以及较高温度和压强下球形微乳液向层状相结构转变而得的二维软模板的导向作用.

关键词: 纳米薄片, 纳米针(管), W/O型微乳液, 水热合成, 硫化镍

Abstract: 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.

Key words: Nanosheet, Nanoneedle, W/O microemulsion, Hydrothermal synthesis, Nickel sulfide

中图分类号:

O614
TB383

TrendMD:

陈德良, 高濂. 水热微乳液法制备低维硫化镍纳米晶. 高等学校化学学报, 2004, 25(8): 1407.

CHEN De-Liang, GAO Lian . Preparation of Low-dimensional Nickel Sulfide Nanocrystals via Microemulsion-assisted Hydrothermal Method. Chem. J. Chinese Universities, 2004, 25(8): 1407.

参考文献

[1] 　X ia Y.,Yang P.,Sun Y.et al..A dv.M ater.[J],2003,15(5):353—389 [2] 　YAN G Q ing-L in(杨青林),SON G Yan-L in(宋延林),W AN M ei-X iang(万梅香)et al..Chem.J.Ch inese U n iversities(高等学校化学学报)[J],2002,23(6):1 105—1 109 [3] 　W ang Z.L..A dv.M ater.[J],1998,10(1):13—30 [4] 　HON G X ia(洪霞),W E I L i(魏莉),A I X in(艾欣)et al..Chem.J.Ch inese U n iversities(高等学校化学学报)[J],2002,23(2):255—258 [5] 　Chen X.,Xu H.,Xu N.et al..Ino rg.Chem.[J],2003,42(9):3 100—3 106 [6] 　R em skar M.,M rzel A.,Sk raba Z.et al..Science[J],2001,292:479—481 [7] 　Ye C.,M eng G.,J iang Z.et al..J.Am.Chem.Soc.[J],2002,124(51):15 180—15 181 [8] 　R em skar M.,M rzel A.,J esih A.et al..A dv.M ater.[J],2002,14(9):680—684 [9] 　L i Y.D.,L i X.L.,H e R.R.et al..J.Am.Chem.Soc.[J],2002,124(7):1 411—1 416 [10] 　B ro rson M.,H an sen T.W.,J acob sen J.H..J.Am.Chem.Soc.[J],2002,124(39):11 582—11 583 [11] 　Yu S.H.,Yo sh im u ra M..A dv.Funct.M ater.[J],2002,12(4):277—285 [12] 　J iang X.,X ie Y.,L u J.et al..A dv.M ater.[J],2001,13(16):1 278—1 281 [13] 　Zhang P.,Gao L..L angm u ir[J],2003,19:208—210 [14] 　Kh iew P.S.,R ad im an S.,H uang N.M.et al..J.C ryst.Grow th[J],2003,254:235—243 [15] 　M o M.,Zeng J.,L iu X.et al..A dv.M ater.[J],2002,14(22):1 658—1 662 [16] 　B ishop D.W.,T hom as P.S.,R ay A.S..J.T herm.A nal.Calo rim.[J],1999,56:429—435 [17] 　Yokoyam a M.,Im am o to T..Syn thesis[J],1998,10:797—799 [18] 　Grau J.,A k inc M..J.Am.Ceram.Soc.[J],1997,80(4):941—951 [19] 　M eng Z.,Peng Y.,Yu W.et al..M ater.Chem.Phys.[J],2002,74:230—233 [20] 　R em skar M.,M rzel A.,San jines R.et al..A dv.M ater.[J],2003,15(3):237—240 [21] 　Hopw ood L.D.,M ann S..Chem.M ater.[J],1997,9(8):1 819—1 826 [22] 　Chen S.H.,Rouch J.,Scio rtino F.et al..J.Phys.:Conden s.M atter[J],1994,6:10 855—10 883 [23] 　Eastoe J.,Rob in son B.H.,Steytler D.C..J.Chem.Soc.,Faraday T ran s.[J],1990,86:511—514 [24] 　Seto H.,Kaw abata D.,Kaw abata Y.et al..J.Chem.Phys.[J],2000,112(23):10 608—10 614 [25] 　Schm id t O.G.,Eberl K..N atu re[J],2001,410:168