近年來由於高熵合金具有高硬度與良好的熱穩定性等各種優異性能，因此引起了學術研究界和工業界的廣泛關注，其中ZrTiNbSiFe 高熵合金薄膜更是擁有良好熱穩定性。本研究使用高功率脈衝磁控濺射 (HiPIMS) 系統，改變不同的氮氣流量比例，在矽晶片與304不銹鋼表面鍍製六種不同氮含量的 ZrTiNbSiFeNx 高熵合金薄膜。本研究以場發射電子探針顯微儀檢定各薄膜的化學成分。以X光繞射儀與TEM穿透式電子顯微鏡分析各薄膜的晶體結構，由場發射掃描式電子顯微鏡觀察各薄膜的橫截面形貌，採用納米壓痕儀、刮痕測試儀和膜耗儀分別研究各 HEAN 薄膜的硬度、附著力和摩擦學性能並將鍍製於Si基板之ZrTiNbSiFeNx高熵合金薄膜進行在空氣環境下1000oC持溫12hr的高溫氧化測試，由熱重分析儀測試各薄膜之重量變化，由實驗結果得知，各薄膜具有良好熱穩定性，本研究將探討不同氮含量對ZrTiNbSiFeNx 高熵合金薄膜的微結構與熱穩定性的影響。成分分析中氮氣流量由0 sccm增加至9sccm隨著氮氣，氮含量相應從0增加到58.2 at.%。 在含氮薄膜中，所有元素的含量隨著氮含量的增加而減少。計算ZrTiNbSiFeN及ZrTiNbSiFeNx 高熵薄膜混和熵皆大於或接近高熵合金定義1.5R。利用XRD低掠角模式進行高熵薄膜晶體結構分析。可以看到除了N2呈現ZrN cubic (B1 NaCl)結構，未含氮與不同氮含量的薄膜皆呈現單一的寬廣繞射峰。透過TEM可以看到N0電子繞射圖為奈米晶結構，之後，隨著氮含量增加至23.6 at% 繞射圖有明顯變寬，當氮含量增加至33.8 at%時可以明顯看到 (111)、(200)繞射環，之後隨著氮含量增加至48.1 at%氮含量趨於飽和，轉變為無序非晶結構。
橫截面分析。可以看到薄膜皆為緻密結構，在製成時間相同的情況下薄膜厚度隨著氮含量的增加而減少鍍率由未通氮15.8 nm/min/kw降低至8.7nm/min/kw。
未通氮高熵薄膜硬度僅10.9 GPa，隨著氮含量的增加，晶體結構由非晶轉變為N2氮含量33.8 at%時呈現ZrN (cubic)，因結晶產生晶界，晶界可以阻止差排滑移使其具有較高的硬度，之後由於結構轉變為非晶結構且氮含量趨於飽和使硬度下降13至14 Gpa之間。透過對高溫氧化實驗後的橫截面分析發現產生連續且緻密的氧化層 XRD分析得知氧化層以ZrO2為主，N3高熵氮化物薄膜在1000oC 持溫12hr表現出好熱穩定性其Kp斜率常數比N0低10倍， 這表示氮提高了抗氧化性。

In recent years, due to the exceptional properties such as high hardness and good thermal stability exhibited by high-entropy alloys, they have attracted extensive attention from both the academic research community and the industrial sector. Among them, ZrTiNbSiFe high-entropy alloy thin films are known for their excellent thermal stability. This study utilized a High-Power Impulse Magnetron Sputtering (HiPIMS) system to deposit six different ZrTiNbSiFeNx high-entropy alloy thin films with varying nitrogen content ratios on silicon wafers and 304 stainless steel surfaces. The chemical composition of each film was examined using Field Emission Electron Probe Microanalysis. The crystal structure of the films was analyzed using X-ray Diffraction (XRD) and Transmission Electron Microscopy (TEM), while the cross-sectional morphology of the films was observed using Field Emission Scanning Electron Microscopy (FESEM). The hardness, adhesion, and tribological properties of the HEAN films were investigated using a Nanoindentation Tester, Scratch Tester, and Tribometer, respectively.
Furthermore, ZrTiNbSiFeNx high-entropy alloy thin films deposited on Si substrates were subjected to high-temperature oxidation testing at 1000°C in an air environment for 12 hours. The weight changes of the films were measured using Thermogravimetric Analysis (TGA). The experimental results revealed that all the films exhibited excellent thermal stability. This study aims to explore the effects of different nitrogen contents on the microstructure and thermal stability of ZrTiNbSiFeNx high-entropy alloy films.In the composition analysis, the nitrogen flow rate increased from 0 sccm to 9 sccm, resulting in a corresponding increase in nitrogen content from 0 to 58.2 at.%. In the nitrogen-containing films, the content of all elements decreased with increasing nitrogen content. The mixing entropy of both ZrTiNbSiFeN and ZrTiNbSiFeNx high-entropy films was greater than or close to the defined value of 1.5R for high-entropy alloys. Crystal structure analysis of the high-entropy films was conducted using XRD with low-angle mode. Apart from N2, which exhibited a ZrN cubic (B1 NaCl) structure, films without nitrogen and those with different nitrogen contents showed a single broad diffraction peak. TEM analysis revealed that the electron diffraction pattern of the N0 film exhibited a nanocrystalline structure. As the nitrogen content increased to 23.6 at%, the diffraction pattern broadened significantly, and at 33.8 at% nitrogen content, distinct (111) and (200) diffraction rings became visible. Subsequently, as the nitrogen content increased to 48.1 at%, nitrogen saturation occurred, resulting in a transition to an amorphous structure.Cross-sectional analysis showed that all films had a dense structure, and under the same deposition time, film thickness decreased with increasing nitrogen content, and the deposition rate dropped from 15.8 nm/min/kW to 8.7 nm/min/kW for films deposited without nitrogen. The hardness of the high-entropy films without nitrogen was only 10.9 GPa. With increasing nitrogen content, the crystal structure transitioned from amorphous to ZrN cubic at 33.8 at% nitrogen content, resulting in the formation of grain boundaries which hindered dislocation slip and increased the hardness. However, as the structure transitioned back to an amorphous state with nitrogen content approaching saturation, the hardness decreased to a range of 13 to 14 GPa. Cross-sectional analysis following high-temperature oxidation experiments revealed the formation of a continuous and dense oxide layer primarily composed of ZrO2. The N3 high-entropy nitride film exhibited good thermal stability at 1000°C for 12 hours, with a Kp slope constant ten times lower than that of N0, indicating that nitrogen enhanced oxidation resistance.

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