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研究生:王麗童
研究生(外文):Li-Tung Wang
論文名稱:含不互溶鈮之銅薄膜濺鍍合成與性質分析研究
論文名稱(外文):Preparation and Characterization of Copper Films With Insoluble Niobium By Sputter Deposition
指導教授:朱 瑾
指導教授(外文):J.P. Chu
學位類別:碩士
校院名稱:國立海洋大學
系所名稱:材料工程研究所
學門:工程學門
學類:材料工程學類
論文種類:學術論文
論文出版年:2002
畢業學年度:90
語文別:英文
中文關鍵詞:銅膜
外文關鍵詞:Cu filmresistivityultra-microhardnessSEMR.F. magnetron sputter depositionNb
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摘要
由於銅和鈮彼此不互溶之特性,因此含不互溶鈮之銅在高溫應用上有很大之潛力。本研究係以射頻磁控濺鍍法製備不互溶之銅鈮合金,在製程參數的控製之下,利用磁控濺鍍法製備之銅鈮合金之含鈮量可達原子百分比24.7%。銅鈮不互溶之結果,使吾人可在濺鍍之銅薄膜觀察到鈮原子置換銅晶格位置所形成之非平衡、過飽和固溶體。X光繞射的結果顯示濺鍍薄膜以及經由退火處理過之試片,其晶格有顯著變化,再次驗證鈮在銅鍍層中行退火處理過之試片,其晶格有顯著變化,再次驗證鈮在銅鍍層中形面析出。熱分析結果顯示退火後濺鍍薄膜有三種狀態。濺鍍薄膜以及經由退火處理過試片之微結構是由SEM來觀察。超微硬度顯示量測結果顯示硬度隨鈮含量增加有上昇之趨勢。低鈮含量薄膜其電阻率呈現下降趨勢,而高鈮含量者則反之,推測可能是由於微結構的改善所造成的。
(關鍵字: 銅薄膜, 鈮, 射頻磁控濺鍍法, DSC, SEM, 超微硬度, 電阻率。)

Abstract
Since copper and niobium are mutually immiscible, copper with insoluble niobium is likely to be a noble material for the high-temperature applications. In this study, Cu-Nb films are prepared by R.F. magnetron sputter deposition technique. With careful control of processing conditions, the niobium concentration in Cu-Nb films can be up to 24.7at% by sputter deposition. Nonequlibrium supersaturated solid solutions of Nb in Cu with nanocrystalline microstructures are observed in as-deposited Cu-Nb films. Variations in lattice parameters for as-deposited and as-annealed Cu-Nb films evidenced by XRD again indicate that solute niobium atoms are in the solid solution with copper. After annealing, the Nb phase separates in Cu matrix and form NbO2 phase in various Cu-Nb films at and above 750°C. Microstructures of both as-deposited and as-annealed Cu-Nb films are examined by SEM. Ultra-microhardness results show an increase in hardness with niobium contents for both as-deposited and as-annealed Cu-Nb films. Electrical resistivity measurements reveal that resistivities of as-deposited Cu-Nb films of low Nb contents (<2.7%Nb) decrease while a different trend is observed in high Nb content films, suggesting the improvement in the microstructure.
(Keywords: Cu film, Nb, R.F. magnetron sputter deposition, SEM, ultra-microhardness, resistivity)

Table of Contents
Ⅰ. Introduction…………………………………………………… 1
A. Material Selection………………………………………….. 1
B. Experimental Objectives…………………………………… 2
Ⅱ. Background……………………………………………..……... 4
A. Properties and Applications Cu and Cu-based Alloys….…. 4
B. Niobium…………………………………………………….. 23
C. Copper With Insoluble niobium…………………………… 25
D. Sputter Deposition…..……………………………………… 25
a. Principles of R.F. Sputter Deposition…………….……... 26
b. Sputtering of Alloys……………………………………... 30
c. Nucleation and Growth of……………………………… 31
c-1. Basic growth modes……………………………….… 31
c-2. Thornton Zone……………………………………….. 33
E. Electrical Properties of Thin Films………………………… 36
F. Hardness Properties of Thin Films……………………….… 39
a. Effects of Film Microstructure on Hardness…………… 39
a-1. Grain Size and Grain Boundary Structure……………. 39
a-2. Metastable Structure………………………………….. 40
a-3. Impurities…..………………………………………… 40
b. Measurements of Hardness…………….………………. 40
Ⅲ. Experimental Procedure……….……………………………... 42
A. Thin Film Deposition……………………………………….. 42
B. Heat Treatment……………………………………………… 48
C. Characterizations………………………………………….… 48
a. Chemistry……………………………………………….. 48
b. Crystal Structure/Microstructure Analyses……………. 50
D. Electrical Resistivity and Ultra-Microhardness Testing…… 50
E. Thermal Analysis……………………………………………. 51
IV. Results and Discussion……………………………………….. 52
A. Chemical Composition……………………………………… 52
B. Crystallography……………………….…………………….. 76
C. Microstructural Observation………………………………... 85
D. Electrical and Mechanical Property Evaluations…………... 113
E. Thermal Analysis……………………………………………. 118
V. Summary……………………………………………………….. 122
Appendix…………………………………………………………... 128

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