17-4PH鋼表面沉積Ti-DLC梯度功能膜及其組織性能研究
發(fā)布時間:2018-07-01 08:38
本文選題:類金剛石薄膜 + 微觀組織結(jié)構(gòu); 參考:《哈爾濱工業(yè)大學》2017年碩士論文
【摘要】:類金剛石(Diamond-like carbon,DLC)薄膜具有優(yōu)異的力學(高的硬度和彈性模量、低摩擦系數(shù))、電磁學、光學性能(增透減反)、生物相容性和化學穩(wěn)定性等,已成為一種重要的新型功能膜。但是研究發(fā)現(xiàn)其主要存在內(nèi)應力較大和熱穩(wěn)定性較差這兩大問題。本文將采用閉合場非平衡磁控濺射離子鍍(UBMS)技術制備不同鈦含量摻雜的DLC梯度功能膜以期解決這兩大問題,并探究鈦含量對類金剛石薄膜微觀組織結(jié)構(gòu)和性能影響規(guī)律和機理。研究結(jié)果表明:所制備的Ti-DLC薄膜表面光滑平坦、膜層致密和顆粒均勻細小,其粗糙度Rq在8.45nm~21.6nm范圍內(nèi)。且鈦靶電流從0.4A增大到0.8A,表面粗糙度升高。GXRD分析可知,Ti-DLC薄膜均在44.5°附近均出現(xiàn)了碳衍射峰,且都生成TiO和TiO_2納米晶,此外鈦靶電流為0.4A試樣還形成了TiN_(0.3)納米晶。XPS分析可知Ti-DLC薄膜表層元素主要以Ti-O和Ti-N鍵合形式存在,分別對應化合物是TiO、TiO_2和TiN_(0.3)。此外,C 1s XPS譜峰可分為sp~3 C峰、sp~2 C峰和C-O峰,通過對各鍵合面積積分求出不同鈦靶電流的Ti-DLC薄膜sp~3C含量在49.03%~53.31%。研究發(fā)現(xiàn)較高的鈦靶電流有利于sp~3 C成鍵,且隨著鈦靶電流從0.3A增加到1.0A,鈦含量從0.82at.%增加到1.97at.%。較高的鈦靶電流促使sp~3 C峰位向高位偏移和半高寬減小。Raman光譜分析可知除了鈦靶電流為1.0A的Ti-DLC薄膜,其它薄膜D峰和G峰位置偏移很小,并求出ID/IG(RI)在1.1~1.7。納米壓痕分析可知,鈦靶電流為0.4A的Ti-DLC薄膜具有最大的硬度(50.697GPa)和彈性模量(368.185GPa)。鈦含量從0.82at.%增大到1.1at.%,其納米硬度與彈性模量均增加;隨后則出現(xiàn)相反的趨勢。摩擦磨損性能分析可知,未處理基體發(fā)生了嚴重氧化磨損和黏著磨損,其磨痕寬度和深度分別約為700μm和100μm;而Ti-DLC薄膜只發(fā)生輕微的磨粒磨損,其磨痕寬度和深度分別約為80μm和0.1μm。與未處理基體相比,其摩擦系數(shù)最大降低了96.15%,磨損率最大降低了99.10%。綜合考慮,鈦靶電流為0.3A的Ti-DLC薄膜耐摩擦磨損性能最好。腐蝕性能分析可知,未處理基體表面腐蝕坑大而密(直徑約為440μm),其微區(qū)元素主要為Cu、Fe和Cr,而Ti-DLC薄膜表面腐蝕坑小而疏(直徑約為1μm),其微區(qū)元素仍以C和Ti元素為主。與未處理基體相比,鍍膜試樣具有更寬鈍化區(qū)。其中鈦靶電流為0.3A試樣具有最低自腐蝕電流,0.4A試樣具有最高點蝕電位和最寬鈍化區(qū),0.6A試樣具有最高自腐蝕電位。綜上所述,最佳的工藝為鈦靶電流0.3A到0.5A。
[Abstract]:Diamond-like carbon (DLC) thin films with excellent mechanical properties (high hardness and elastic modulus, low friction coefficient), electromagnetics, optical properties (antireflection), biocompatibility and chemical stability have become an important new functional film. However, it is found that there are two main problems: high internal stress and poor thermal stability. In this paper, DLC gradient functional films doped with different titanium content will be prepared by closed field unbalanced magnetron sputtering ion plating (UBMS) in order to solve these two problems, and the effect of titanium content on microstructure and properties of diamond-like carbon films is investigated. The results show that the surface of Ti-DLC thin film is smooth and flat, the film is compact and fine, and its roughness RQ is in the range of 8.45nm~21.6nm. When the current of Ti target increases from 0.4A to 0.8A, the surface roughness increases. GXRD analysis shows that all Ti-DLC films have carbon diffraction peaks near 44.5 擄, and both TIO and TiO-2 nanocrystals are formed. In addition, TiN0.3 nanocrystalline. XPS analysis shows that the surface elements of Ti-DLC films mainly exist in the form of Ti-O and Ti-N bonding, and the corresponding compounds are TiOO _ 2O _ 2 and TiN _ (0.3) respectively. In addition, the peaks of C 1s XPS spectra can be divided into sp~3 C peaks and C O peaks. Through the integration of each bonding area, the content of SSP 3C of Ti-DLC thin films with different Ti target currents is 49.03 and 53.31. It is found that the higher titanium target current is beneficial to the bonding of sp~3 C, and the titanium content increases from 0.82at.% to 1.97at.with the titanium target current increasing from 0.3A to 1.0 A. The high Ti target current causes the sp~3 C peak to shift to a high position and the half-maximum width to decrease. Raman spectra show that, except for Ti-DLC thin films with 1.0 A Ti target current, the shift of D and G peaks in other films is very small, and the IDR / IG (RI) is found to be 1.1 ~ 1.7. Nano indentation analysis shows that Ti-DLC film with 0.4A target current has the highest hardness (50.697GPa) and elastic modulus (368.185GPa). When the titanium content increased from 0.82at.% to 1.1at.its nanohardness and elastic modulus increased, and then the reverse trend was observed. According to the analysis of friction and wear properties, serious oxidation wear and adhesion wear occurred in untreated substrate, the width and depth of wear mark were about 700 渭 m and 100 渭 m, respectively, while that of Ti-DLC film was only slightly abrasive wear, the width and depth of wear trace were about 80 渭 m and 0.1 渭 m, respectively. Compared with the untreated matrix, the maximum friction coefficient and wear rate are reduced 96.15 and 99.10% respectively. Considering the friction and wear resistance of Ti-DLC thin films with target current of 0.3A, the friction and wear resistance of Ti-DLC thin films is the best. The corrosion performance analysis shows that the corrosion pits on the surface of untreated substrates are large and dense (about 440 渭 m), in diameter), and the microelements are mainly Cu Fe and Cr, while the corrosion pits on the surface of Ti-DLC films are small and sparse (about 1 渭 m), in diameter). Compared with the untreated substrate, the coated sample has a wider passivation zone. The titanium target current of 0.3A has the lowest self-corrosion current of 0.4A and the highest pitting potential of 0.4A and the highest self-corrosion potential of 0.6A with the widest passivation region. To sum up, the best process is titanium target current 0.3A to 0.5A.
【學位授予單位】:哈爾濱工業(yè)大學
【學位級別】:碩士
【學位授予年份】:2017
【分類號】:TG174.45
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本文編號:2087197
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