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標題: 氮化鈦薄膜鍍著銅材在高溫控制氣氛下之劣化研究
The Degradation of TiN-Coated Copper at High Temperature under
作者: 李基魁
Lee, Ji-Kwei
關鍵字: TiN

出版社: 材料工程學研究所
摘要: 本研究是以陰極電弧電漿沉積法,將氮化鈦薄膜鍍於銅材上,而後以 空氣、氮氣、氬氣及成份N2:H2:CO2=81:9:10之混合氣等四種氣氛,在溫 度300~1000C之間,熱處理約3~12小時後,研究經過不同條件下熱處理後 ,氮化鈦薄膜劣化的情形。 在本實驗的結果中,銅片電解拋光的最佳 條件是:磷酸與水的體積比為7:3,操作電壓2V,操作時間5分鐘,陰極是 環形銅片。而鍍著氮化鈦薄膜後,在膜厚量測方面,由於二次鍍著時間不 同,膜厚亦有異,一批膜厚約1.2~1.5um,另一批膜厚約0.6~0.8um。 由熱力學的分析,氮化鈦薄膜在本研究所選擇的氣氛下,會氧化成鈦的氧 化物TiOx,再由鈦的與氧分壓的平衡相圖中知,鈦若發生氧化,在本實驗 條件下是生成TiO2。 鍍著完之試片,以XPS做表面分析,可發現除了 TiN外,還有TiO2。而以AES做縱深分析,可發現表面有一層C及O存在。在 各種氣氛中熱處理後,空氣中300C熱處理4小時後,外觀上開始有顏色變 化,這可能是氮化鈦薄膜氧化成TiOx的原因。在氮氣中以505C熱處理6小 時後,氮化鈦表面上會變成紫色,600C熱處理6小時後,由XRD可以分析得 TiO2。氬氣下以450C熱處理12小時後,氮化鈦表面上亦變成紫色,而 在600C熱處理6小時後,由XRD和GIXD亦可以分析得TiO2。在成份N2:H2: CO2=81:9:10之混合氣下以600C熱處理6小時後,氮化鈦表面上會變成紫色 ,700C熱處理6小時後,由XRD可以得TiO2。
In this research, TiN films were deposited on copper substrates byusing the Cathodic Arc Deposition technique.The degradation of TiN filmsat high temperature (300~1000C) and different annealing time (3~12 hrs)under controlled atmospheres (air, N2, Ar, N2:H2:CO2=81:9:10) was investigated. The best condition of electrolytic polish in this experiment is :electrolyte:HNO3:H2O=7:3 ; volt :2V ; time :5 min ; cathode : copper.After the deposition of TiN films , and the morphology of the TiN films were investigates by using the optical microscopy and the scanning electionmicroscope. From thermodynamic analysis, TiN films will be oxidized to TiOx under our experiment condition. As predicted from the Ti-O phase diagram, TiOx would be TiO2 under these condition at equilibrium. We used XPS to analyze the chemical state and the composition of TiN is found to be mainly TiO2. The depth of the films was also analyzed by using AES. The result of TiN films after annealing at different atmosphere were discussed. The color of the films has started to change after annealingin air at 300 C for 4 hrs. It is possible that TiN films were oxidized to be TiOx. After annealing in N2 at 500 C for 600 hrs, the color of the TiN films turns to purple. XRD result indicate that TiN transforms to TiO2 after annealing in N2 at 600 C for 6 hrs. The color of TiN films also turns to purple after annealing in Ar at 450 C for 12 hrs. XRD and GIXD results indicate that TiN transforms to TiO2 after annealing in Ar at 600 C for 6hrs. For the atmosphere of mixing gas(N2:H2:CO2=81:9:10), the color of TiN surface turns to purple after annealing at 600 C for 6 hrs. XRD result indicate that TiN transforms to TiO2 annealing at 700 C for 6 hrs.
Appears in Collections:材料科學與工程學系



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