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標題: 氮化鋯鍍膜在高溫控制氣氛下劣化之研究
Degradation of ZrN Films at High Temperature under Controlled Atmosphere
作者: Lo, Wen-Zheng
關鍵字: 氮化鋯
zirconium nitride
residual stress
出版社: 材料工程學研究所
摘要: 本研究主要是探討氮化鋯薄膜於不同氣氛(空氣、氮氣及N2/H2=9混合氣包含真空)高溫熱處理後劣化現象,熱處理溫度範圍為300∼1200℃,持溫時間為0.5~12小時,劣化現象包含了鍍膜顏色變化及形成巨觀缺陷等。 氮化鋯薄膜在上述氣氛400℃以上,表面皆會出現直徑大小約5-10 mm圓形凸狀物(A型)之巨觀缺陷,凸狀物部分已有破裂現象,此時薄膜外觀顏色與剛鍍著之氮化鋯薄膜相同,呈現金黃色澤。到達700-800℃時,薄膜表面除了A型圓形凸狀物外,另出現B型緻密不規則凸狀物之缺陷,此時薄膜顏色皆呈現粉紅色,但在真空處理未發現此缺陷,由於真空下薄膜並不會產生氧化反應,因此確定B型不規則凸狀物缺陷與氧化有密切地關係。 另外,以X光繞射儀及拉曼光譜儀分析氮化鋯薄膜於三種氣氛(空氣、氮氣及N2/H2=9混合氣)退火後之晶體結構變化,在空氣及氮氣中600℃以上開始出現單斜晶系氧化鋯,而在N2/H2=9混合氣中700℃以上才開始出現,並觀察鍍膜橫截面變化,利用熱力學分析薄膜氧化變化。 使用掃描式雷射曲率法量測薄膜退火後之應力變化,剛鍍著時應力為-4.5 GPa,在本研究選用N2/H2=9混合氣及真空氣氛下皆在400℃應力增大(-7.2 GPa),因此研判A型較大圓形凸狀物之巨觀缺陷為薄膜之殘留應力所致。並利用XRD測量薄膜退火後之應變與殘留應力關係,可求得氮化鋯薄膜之楊氏係數為250± 80 GPa,與文獻報導相符。
The objective of this research is to investigate degradation of ZrN films annealed in the controlled atmosphere. The ZrN films were deposited onto (100) Si substrates by unbalanced magnetron sputtering. The films were then annealed in air, N2, N2/H2=9, and vacuum which possess dramatically different pN2/pO2 ratios. Annealing was conducted over temperatures of 300-1200°C for 0.5-12 h. Large blisters denoted as A-type defects appeared on the film surface above 400°C in all the atmosphere. The top of many blisters has broken surface. Small blisters denoted as B-type defects showed up above 700℃ in all atmosphere except vacuum. Such blisters resulted from oxidation of the films. X-ray diffraction and Raman spectroscopy results showed that monoclinic ZrO2 existed above 600°C both in air and N2 while appeared above 700°C in N2/H2=9. Oxidation kinetics was discussed. Residual stresses were measured by a scanning laser curvature technique. Residual stress of the as-deposited ZrN films was —4.5 GPa and was decreased to -7.2 GPa at 400℃. Such pronounced residual stress change was responsible for the formation of A-type large blisters. The Young's modulus of ZrN films could be deduced from the stress-strain relation. The obtained value was 250±80 GPa, which is compatible with the data available in the literature.
Appears in Collections:材料科學與工程學系



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