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Title: 以磁控濺鍍Hf–Si–N鍍層之機械性質及抗氧化性研究
Mechanical Properties and Oxidation Resistance of Hf–Si–N Coatings by Magnetron Sputtering
Authors: Liu, Bo-Wei
Contributors: NTOU:Institute of Materials Engineering
Keywords: 磁控濺鍍;Hf–Si–N;機械性質;抗氧化性;熱處理
magnetron sputtering, , , ,;Hf–Si–N;mechanical properties;oxidation resistance;heat treatment
Date: 2018
Issue Date: 2019-05-23T06:19:37Z
Abstract: 本實驗利用反應式直流磁控濺鍍系統沉積Hf–Si–N奈米複合膜。第一部分固定氮氣分壓N2/(Ar+N2)為0.4、工作壓力3 mTorr、Hf靶功率為250 W、改變Si靶功率0–150 W,以沉積不同Si含量之Hf–Si–N硬質鍍層於Si晶片上,目標為製備Si含量從0–20 at. %之間的硬質複合膜;第二部分固定氮氣分壓N2/(Ar+N2)為0.4、工作壓力3 mTorr、Si靶為250 W、改變Hf靶功率150–225 W,目標為製備Hf:Si含量比為1:1的硬質複合膜。利用場發射式電子微探儀(FE-EPMA)對鍍層做定量元素分析,場發射式掃描電子顯微鏡(FE–SEM)、X光繞射儀(XRD),對鍍層之微結構進行分析及確認。並以奈米壓痕儀(Nanoindenter)、原子力顯微鏡(AFM)量測薄膜硬度、楊氏係數及粗糙度。另外以氣氛為1% O2-99%Ar的混合氣於600°C下進行長時間熱處理,並觀察不同退火時間下鍍層之氧化行為及厚度變化,並使用化學分析電子能譜儀(XPS)進行元素鍵結分析。 Hf54N46鍍層為f.c.c.結構,而低Si含量(3 at. %)的鍍層表現出f.c.c.和非晶相的混合物。中Si含量(7 at. %)的鍍層以非晶為主,並摻雜著微量f.c.c.結構。高Si含量(12–27 at. %)鍍層呈現非晶相結構。Hf48Si3N49鍍層的奈米壓痕硬度顯示最大值為22.5 ± 0.8 GPa,隨著Si含量增加至7 at. %硬度值降低至15.3 ± 0.6 GPa,然後保持在15–16 GPa,Si含量持續增加至23–27 GPa時硬度由15.2 GPa持續上升至17.1 GPa。Hf54N46鍍層的殘留應力顯示最大值為–2.4 ± 0.1 GPa,隨著Si含量增加Hf48Si3N49鍍層降至–1.5 ± 0.1 GPa,而Si 7–27 at. %殘留應力則保持在–0.4至–0.7之間。Si含量大於19 at. %以上時,抗氧化能力明顯提升。
In this study, Hf–Si–N nanocomposite coatings were prepared by reactive DC magnetron sputtering system. The first part is to prepare coatings with different Si contents. Therefore, fixed nitrogen partial pressure N2/(Ar+N2) is 0.4, and the working pressure is 3 mTorr. Then fixed Hf target power is 250 W, and the Si target power is changed from 0 to 150 W. The Second part is to prepare a hard composite coating with a Hf:Si content ratio of 1:1. Fixed nitrogen partial pressure N2/(Ar+N2) is 0.4, and the working pressure is 3 mTorr. Then Si target power is fixed at 150 W, and the Hf target power is changed from 150 to 225 W. Chemical composition analysis was carried out with a field-emission electron probe microanalyzer (FE-EPMA, JXA-8500F, JEOL, Japan) on the surface of the samples. The thickness of coatings was evaluated by field emission scanning electron microscopy (FE-SEM, S4800, Hitachi, Japan). A conventional X-ray diffractometer (XRD, X'Pert PRO MPD, PANalytical, Netherlands) with Cu Kα radiation was adopted to identify the phases of the coatings. The surface nanohardness values of various Hf–Si–N coatings were measured with a nanoindentation tester (TI900 Triboindenter, Hysitron, USA). The Hf-Si-N coating is annealed at 600°C in a 1% O2–99% Ar atmosphere.The oxidation behavior and thickness variation of the coating under different annealing times were ecaluated. Elemental bond analysis was performed using a chemical analysis electron spectrometer (ESCA, PHI 5000 Versa Probe II, PHI, Japan). The Hf54N46 coatings exhibited a face-centered cubic (f.c.c.) structure. The low Si content (3 at. %) coating exhibited a mixture of f.c.c. and amorphous phase. High Si content (12–27 at. %) coating exhibited an amorphous phase structure. The nanohardness of the Hf48Si3N49 coating exhibited a maximum of 22.5 ± 0.8 GPa. As Si content increases to 7 at. % hardness value decreases to 15.3 ± 0.6 GPa, then stays at 15–16 GPa. As the Si content continues to increase to 23–27 at. %, the hardness continue to increase from 15.2 GPa to 17.1 GPa. The residual stress of the Hf54N46 coating shows a maximum of –2.4 ± 0.1 GPa. The residual stress of the films with 7–27 at. % remains between –0.4 and –0.7. When the Si content is more than 19 at. %, the antioxidation ability is obviously improved.
Appears in Collections:[Institute of Materials Engineering] Dissertations and Theses

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