本研究主要利用物理氣相沉積法成長奈米複合薄膜微結構特性與機械性質之研究，相關文獻指出由於單純類鑽碳膜可能會有熱穩定性及附著力不佳或內部高應力等問題，因此希望藉由添加矽及鈦元素以改善一般傳統類鑽碳膜之性質。其中利用超高真空離子束濺鍍系統成長單層碳(C)、雙層碳/矽(C/Si)及堆疊式三層矽/碳/矽(Si/C/Si)奈米複合薄膜。藉由封閉式非平衡磁控濺鍍系統成長含鈦類鑽碳(Ti-DLC)薄膜及其它奈米複合薄膜之研究上則利用反應式磁控共濺鍍法沉積鉭-矽-氮(Ta-Si-N)薄膜。探討奈米複合薄膜的製程参數、成分比例、溫度、微奈米結構與機械性質的關係。最後並進行脈波電化學在304不銹鋼棒成形具次微米特徵刀具之披覆含鈦類鑽碳薄膜與單晶鑽石刀具劃切實驗比較。上述相關奈米複合薄膜預期可在表層改質披覆、光電元件、微機電系統元件及工程材料等之應用。
本論文首先提出非晶矽(a-Si)層對於堆疊式碳/矽複合薄膜之影響的章節中，相關非晶矽層之位置對於複合薄膜結構藉由後處理高真空退火機制下沉積於基材為單晶矽之三種單、雙層及堆疊式矽/碳/矽三明治複合薄膜結構，研究其非晶矽層對於碳、矽間的反應影響。其中當單層碳於退火溫度達900℃，時間為1.5小時，無互相擴散反應。但當退火在相同條件下卻有部份擴散發生於雙層之碳/矽結構，同時檢測到非晶矽轉換成多晶矽結構。然而在三層矽/碳/矽複合薄膜三明治結構中，觀察到非晶矽轉換成多晶矽結構之退火溫度降為700℃，而且內部互相擴散反應明顯發生於900℃同時有結晶之碳化矽(SiC)形成。藉由堆疊式之碳/矽結構中轉換成之多晶矽晶界，其可能之擴散及反應機制在內文中有完整之探討。
相關碳化矽奈米晶粒形成探討上，利用超高真空離子束濺鍍系統成長於基材為單晶矽(100)晶圓之堆疊式矽/碳/矽結構中，藉由高真空熱退火機制轉換形成碳化矽奈米晶粒。當退火溫度500℃而退火時間為1小時條件下，並無任何碳化矽奈米晶粒檢測出，當退火溫度增加至700℃時開始部分碳化矽奈米晶粒形成，而當退火溫度達900℃時，次微米大之晶粒週遭觀察到有著數十奈米之碳化矽奈米晶粒產生。由於較高之原子遷移率及成長率所產生，由於退火溫度達900℃時，降低了較小晶粒的總表面能而使得晶粒成長。
奈米機械性質與薄膜之微結構特性息息相關。在各奈米複合薄膜機械性質探討之章節中，將分別針對高溫退火下非晶矽對於單、雙層及堆疊式三層矽/碳/矽之三種結構的機械性質行為影響，以及含鈦類鑽碳薄膜奈米機械性質探討。另外將針對氮氣流量比對於鉭-矽-氮奈米複合薄膜之微結構與奈米硬度關係之研究。
硬質薄膜層披覆應用探討上，將利用脈波電化學加工具次微米特徵之刀具進行含鈦類鑽碳薄膜披覆之特性探討，實驗結果發現隨著鈦成份含量增加而隨之sp2鍵結增加，導致降低薄膜材料之楊氏係數。因此相關奈米壓痕之硬度(H)與楊氏係數(E)之機械性質檢測上，當組別Ti-DLC-2鈦成份含量為7.2 %時有較高的H/E比值，亦即將有較佳之切削磨耗應用。最後，對於覆膜刀具與單晶鑽石在劃切實驗來觀察刀具幾何及材料性質對切削之影響，其中切削力之差異探討比較上，經切削實驗證明，覆膜刀具之比切削能於平均切削厚度約在20 μm時與單晶鑚石刀具之值大小相近，即切削性質與單晶鑚石刀具切削性接近；但是覆膜刀具在加工時的摩擦係數仍大於單晶鑚石刀具，即相關鍍膜條件參數及刀具材料尚有改善空間。而在電化學參數影響方面，也證明了調降脈衝寬度能降低表面粗度與刀刃圓角。

In this study, we utilized the method of physical vapor deposition (PVD) to form the single-layer C, two-layer C/a-Si and three-layer a-Si/C/a-Si nanocomposite films using ultra high vacuum ion beam sputtering (UHV IBS) system, Ti-containing diamond-like hydrocarbon (Ti-DLC) coatings in closed field unbalanced magnetron sputtering (CFUBMS) deposition system, and the Ta-Si-N nanocomposite films by magnetron co-sputtering reaction system. The relations between deposition parameters, composition, temperature, microstructure and nanomechanical properties are discussed and established by means of characterization and material analysis in this dissertation. They are potentially used for the application of surface modification, optoelectronic devices, microelectromechanical system and engineering tribology.
In the section of the reaction between C and Si, the amorphous silicon (a-Si) layer positioned under or sandwiching the C layer will affect reaction temperature between the a-Si and C layers at constant annealing time. The post vacuum annealing was performed in order to study the effect of a-Si layer during the reaction between C and Si in three specific kinds of structures i.e. C, C/a-Si and a-Si/C/a-Si deposited on crystalline silicon (c-Si) substrates. There was no interdiffusion between the single-layer C and c-Si substrate when annealed up to 900 ºC for 1.5 hours. But some interdiffusion occurred between C and a-Si of the two-layer C/a-Si structure when annealed at 900 ºC for 1.5 hours. Simultaneously, transformation of a-Si to polycrystalline Si was detected. In the a-Si/C/a-Si structure, the transformation of a-Si to polycrystalline Si was observed at 700 ºC along with significant interdiffusion at 900 ºC as well as crystalline SiC formation in the multilayer.
In the section of the formation of SiC nanoparticles, deposition of Si/C/Si multilayers on Si(100) wafers by UHV IBS was followed by thermal annealing in vacuum for the conversion into SiC nanoparticles. No nanoparticles were formed for multilayers which were annealed at 500 ºC, while a few particles started to appear when the annealing temperature increased to 700 ºC. At an annealing temperature of 900 ºC, many small SiC nanoparticles, of several tens of nanometers, surrounding larger submicron ones appeared with a particle density approximately 16 times higher than that observed at 700 ºC. The higher the annealing temperature, the larger the nanoparticle size along with a higher density. These particles grew larger at 900 ºC to reduce the total surface energy of smaller particles due to their higher atomic mobility and growth rate.
The nanomechanical properties are related to the microstructure of thin films. In the section of nanomechanical properties of C, C/Si, Si/C/Si and other nanocomposite films i.e. Ti-DLC and Ta-Si-N films are individual discussions about the effect of a-Si addition on the nanomechanical behavior of the C, C/Si and Si/C/Si films at high temperatures, nanomechanical properties of Ti-DLC, and nanohardness of Ta-Si-N thin films at different nitrogen flow ratios. In addition, in the section of hard coating for the application of wedge-shape tool, the Ti-DLC coatings on the electrochemical fabricated stainless steel tools have been synthesized by CFUBMS process. The microstructures of Ti-DLC coating are characterized by Raman spectroscopy. The results show that the sp2 bonding increases with decreasing Ti composition. Therefore, as Ti composition decreases, the hardness of Ti-DLC coatings increases. The high ratio of hardness to elastic modulus (H/E) in Ti-DLC-2 with low Ti content of 7.2% is good for the cutting and wearing tool applications. The fabricated tool is tested successfully in a scribing experiment and compared with a single crystal diamond cutter.

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