金属Pd薄膜的超临界流体沉积制备及其结构表征

王燕磊; 张占文; 李波; 江波

doi:10.7498/aps.60.088103

摘要

用超临界流体化学沉积法以有机金属化合物为前驱物制备金属单质薄膜.超临界CO2为溶剂,六氟乙酰丙酮钯(Pd(Ⅱ)(hfac)2)为前驱物,在温度为100 ℃、压力为1218 MPa、反应时间为1020 h的条件下,经过H2气催化还原在单晶Si片上制备金属Pd薄膜,薄膜均匀且连续,厚度为0.31.5 m.经X射线光电子能谱和X射线衍射谱分析可知,沉积的薄膜为金属Pd单质晶体结构.扫描电子显微镜研究结果表明,沉积压力对薄膜的晶粒尺寸有很大

关键词:

Abstract

Pd films are deposited on the Si wafers by the reduction of palladium(Ⅱ) hexafluoroacetylacetonate, which is used as the precursor, in the supercritical CO2 solution at temperature 100 ℃ and pressures between 12 and 18 MPa, and with reaction for 1020 h. The films are continuous, uniform and 0.31.5 m thick. The analyses of the Pd films by X-ray photoelectron spectroscopy and X-ray diffraction indicate that the structures of the deposited films are of single matter and nanocrystalline. The scanning electron microscope images show that pressure is a factor of affecting the size of the grain of the deposited film. At a pressure of 12 MPa, the size of grain is between 30 and 60 nm, at a pressure of 15 MPa, it is between 90 and 120 nm. Moreover, at a pressure of 18 MPa, it is between 150 and 180 nm. At the same temperature, with higher pressures, the size of the grain is bigger. On the same conditions, Pd thin films are deposited on the inner and the outer surfaces of cylindrical cavity.

Keywords:

作者及机构信息

1.
四川大学化学学院,成都 610064;

2.
中国工程物理研究院激光聚变研究中心,高温高密度等离子体物理国防科技重点实验室,绵阳 621900

基金项目: 高温高密度等离子体物理国防科技重点实验室基金(批准号:9140C680803080C68)资助的课题.

Authors and contacts

1.
College of Chemistry, Sichuan University, Chengdu 610064, China;

2.
Key Laboratory of National Defense Science and Technology for High-Temperature and High-Density Plasma Physics, Reserch Center of Laser Fusion, China Academy of Engineering Physics, Mianyang 621900, China

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施引文献

[1]	James J W, Jason M B, Thomas J M 1999 Chem. Mater. 11 213
[2]	Ephrem T H, James J W 2004 Chem. Mater. 16 498
[3]
[4]
[5]	Neil E F, Scott M F, Joseph C P 2001 Chem. Mater. 13 2023
[6]	Albertina C, Jason M B, James J W 2002 Microelectron. Eng. 64 53
[7]
[8]
[9]	Jason M B, David P L, Albertina C, James J W 2001 Science 294 141
[10]
[11]	Xu Q Q, Yin J Z, Xiao M, Wang A Q 2007 Chem. Bull. 70 188 (in Chinese) [徐琴琴、银建中、肖敏、王爱琴 2007 化学通报 70 188]
[12]
[13]	Han B X 2005 Supercritical Fluid Science and Technology (Beijing: Sinopec Press) p17 (in Chinese)[韩布兴 2005超临界流体科学与技术 (北京:石化出版社) 第17页]
[14]
[15]	Liu J G, Wan X B, Fu Q, Zhou L, Xiao J 2005 At. Ener. Sci. Techn. 39 77 (in Chinese) [刘继光、万小波、付渠、周兰、肖江 2005 原子能科学技术 39 77]
[16]
[17]	Jay J S, Fu T, Diana R 2003 Chem. Vap. Depos. 9 258
[18]
[19]	Zeng C L, Tang D S, Liu X H, Hai K, Yang Y, Yuan H J, Xie S S 2007 Acta Phys. Sin. 56 6531 (in Chinese) [曾春来、唐东升、刘星辉、海阔、羊亿、袁华军、解思深 2007 物理学报 56 6531]
[20]	Yin J Z, Zhang C J, Xu Q Q, Wang A Q 2009 J. Inorg. Mater. 24 129 (in Chinese) [银建中、张传杰、徐琴琴、王爱琴 2009 无机材料学报 24 129]
[21]
[22]	Liu W 2008 M. S. Dissertation (Tianjin: Tianjin University) (in Chinese) [刘伟 2008 硕士学位论文 (天津:天津大学)]
[23]
[24]	Jason M B, David P L, James J W 2000 Chem. Mater. 12 2625
[25]
[26]
[27]	David P L, Jason M B, James J W 2000 Adv. Mater. 12 913
[28]
[29]	Kondoh E, Kato H 2002 Microelectron. Eng. 64 495
[30]
[31]	Wu Z Q, Wang B 2001 The Growth of Thin Films (Beijing: Science Press) p170 (in Chinese) [吴自勤、王兵 2001 薄膜生长 (北京:科学出版社) 第170页]
[32]	Zong Y F, James J W 2004 Mat. Res. Soc. Symp. Proc. 812 F8.6.1
[33]
[34]	Wu F M, Shi J Q, Wu Z Q 2001 Acta Phys. Sin. 50 1555 (in Chinese)[吴锋民、施建青、吴自勤 2001 物理学报 50 1555]
[35]
[36]
[37]	Cai X, Gu J F, Zhou P N, Yang X Y 1997 Trans. Metal Heat Treatm. 18 30 (in Chinese) [蔡勋、顾剑锋、周平南、杨晓豫 1997 金属热处理学报 18 30]

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