FeCrVTa0.4W0.4高熵合金氮化物薄膜的微觀結構與性能

王子鑫; 張勇

doi:10.13374/j.issn2095-9389.2020.09.28.004

FeCrVTa_0.4W_0.4高熵合金氮化物薄膜的微觀結構與性能

doi: 10.13374/j.issn2095-9389.2020.09.28.004

王子鑫^{1, 2},
張勇^{1, 2, 3, ,}

1.
青海大學青海省新型輕合金重點實驗室，西寧 810016
2.
北京科技大學新金屬材料國家重點實驗室，北京 100083
3.
北京科技大學順德研究生院，佛山 528399

基金項目: 區域聯合基金資助項目（2019B1515120020）；中央高校基本科研業務費資助項目（FRF-MP-19-013）

詳細信息

通訊作者:
E-mail：drzhangy@ustb.edu.cn

中圖分類號: TG139
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出版歷程
- 收稿日期: 2020-09-28
- 刊出日期: 2021-05-25

Microstructure and properties of FeCrVTa_0.4W_0.4 high-entropy alloy nitride films

WANG Zi-xin^{1, 2},
ZHANG Yong^{1, 2, 3
, ,}

1.
Qinghai Provincial Key Laboratory of New Light Alloys, Qinghai University, Xining 810016, China
2.
State Key Laboratory for Advanced Metals and Materials, University of Science and Technology Beijing, Beijing 100083, China
3.
Shunde Graduate School, University of Science and Technology Beijing, Foshan 528399, China

More Information

Corresponding author: E-mail: drzhangy@ustb.edu.cn

摘要

摘要: 實驗利用單靶射頻磁控濺射技術，在單晶硅基底上，制備了兩個系列FeCrVTa_0.4W_0.4高熵合金氮化物薄膜，即FeCrVTa_0.4W_0.4氮化物成分梯度多層薄膜和(FeCrVTa_0.4W_0.4)N_x單層薄膜，其中，多層薄膜用于太陽光譜選擇性吸收薄膜。通過掃描電子顯微鏡(SEM)、X射線衍射儀(XRD)、納米力學探針、原子力顯微鏡(AFM)、紫外?可見分光光度計、接觸角測量儀和四探針測試臺對FeCrVTa_0.4W_0.4高熵合金氮化物薄膜進行微觀結構分析以及性能表征。結果表明：在不通入氮氣時，薄膜為非晶結構，當氮氣含量升高后，轉變為面心立方固溶體結構；當表層氮氣流量為15 mL·min^?1時，FeCrVTa_0.4W_0.4氮化物多層薄膜及單層薄膜均具有最佳的力學性能，其中，多層薄膜的硬度為22.05 GPa，模量為287.4 GPa，單層薄膜的硬度為22.8 GPa，模量為280.7 GPa，隨著表層氮氣含量的繼續增加，力學性能下降；FeCrVTa_0.4W_0.4氮化物成分梯度多層薄膜在300～800 nm波長范圍內均具有太陽光譜選擇吸收性，當氮化物薄膜層數較少時具有較好的疏水性；(FeCrVTa_0.4W_0.4)N_x單層薄膜隨著氮氣含量的增加，薄膜方塊電阻增加。
- 高熵合金 /
- 磁控濺射 /
- 氮化物薄膜 /
- 成分梯度 /
- 光學性能
Abstract: Recently, research on high-entropy alloys has developed rapidly. While studying high-entropy alloys in bulk, scholars have also conducted in-depth research on high-entropy alloy films, especially high-entropy alloy nitride films. Compared with traditional binary and ternary nitride films, high-entropy alloy nitride films have a simpler and denser structure and better performance, and therefore have great prospects for application in many fields. Research on high-entropy alloy nitride films is still relatively scarce, and the influencing factors of phase structure transformation and mechanical properties need to be further explored. Therefore, it will be an important research direction in the future. Based on a single-target Radio Frequency (RF) magnetron sputtering technique, two series of FeCrVTa_0.4W_0.4 high-entropy alloy nitride films were fabricated on monocrystalline silicon substrates. These are FeCrVTa_0.4W_0.4 nitride composition gradient multilayer films and (FeCrVTa_0.4W_0.4)N_x single-layer films, in which multilayer films are used for solar spectral selective absorption films. Through scanning electron microscope (SEM), X-ray diffractometer (XRD), nanomechanical probe, atomic force microscopy, UV–visible spectrophotometry, contact angle measuring instrument, and four-probe tester, the microstructure, and properties of FeCrVTa_0.4W_0.4 high-entropy alloy nitride films were analyzed. The results show that the film is amorphous when nitrogen is not introduced. When nitrogen content increases, nitride films are face-center-cubic solid solution in structure. When the surface nitrogen flow rate is 15 sccm, the FeCrVTa_0.4W_0.4 nitride multilayer film and the single-layer film have the best mechanical properties. Among them, the hardness of the multilayer film is 22.05 GPa and the modulus is 287.4 GPa; the hardness of the single-layer film is 22.8 GPa, and the modulus is 280.7 GPa. As the nitrogen content on the surface continues to increase, the mechanical properties decrease. FeCrVTa_0.4W_0.4 nitride composition gradient multilayer films have solar spectrum selective absorptivity in the wavelength range of 300–800 nm and have better hydrophobicity when the number of nitride films layer is small. With increasing nitrogen content, the block resistance of (FeCrVTa_0.4W_0.4)N_x single-layer film increases.
- high-entropy alloy /
- megnetron sputtering /
- nitride films /
- composition gradient /
- optical property

HTML全文

圖 1 FeCrVTa_0.4W_0.4氮化物成分梯度多層薄膜的截面及表面顯微照片。（a）N₂-0截面；（b）N₂-0表面；（c）N₂-1截面；（d）N₂-1表面；（e） N₂-2截面；（f）N₂-2表面；（g）N₂-3截面；（h）N₂-3表面

Figure 1. Cross-sectional and plane-view micrograph of FeCrVTa_0.4W_0.4 nitride composition gradient multilayer films: cross-section (a) and plane-view (b) of N₂-0; cross-section (c) and plane-view (d) of N₂-1; cross-section (e) and plane-view (f) of N₂-2; cross-section (g) and plane-view (h) of N₂-3

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圖 2 不同氮氣流量下(FeCrVTa_0.4W_0.4)N_x單層薄膜的截面及表面顯微照片。（a）N₂-15截面；（b）N₂-15表面；（c）N₂-30截面；（d）N₂-30表面；（e）N₂-45截面；（f）N₂-45表面

Figure 2. Cross-sectional and plane-view micrograph of (FeCrVTa_0.4W_0.4)N_x single-layer films at different N₂ flows: cross-section (a) and plane-view (b) of N₂-15; cross-section (c) and plane-view (d) of N₂-30; cross-section (e) and plane-view (f) of N₂-45

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圖 3 FeCrVTa_0.4W_0.4氮化物成分梯度多層薄膜的AFM表面形貌。（a） N₂-0；（b）N₂-1；（c）N₂-2；（d）N₂-3

Figure 3. AFM surface morphology of FeCrVTa_0.4W_0.4 nitride composition gradient multilayer films: (a) N₂-0; (b) N₂-1; (c) N₂-2; (d) N₂-3

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圖 4 不同氮氣流量下(FeCrVTa_0.4W_0.4)N_x單層薄膜的AFM表面形貌。（a）N₂-15；（b）N₂-30；（c）N₂-45

Figure 4. AFM surface morphology of (FeCrVTa_0.4W_0.4)N_x single-layer films at different N₂ flows: (a) N₂-15; (b) N₂-30; (c) N₂-45

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圖 5 FeCrVTa_0.4W_0.4氮化物薄膜的XRD衍射圖。（a）FeCrVTa_0.4W_0.4氮化物成分梯度多層薄膜；（b） (FeCrVTa_0.4W_0.4)N_x單層薄膜

Figure 5. XRD diffraction patterns of FeCrVTa_0.4W_0.4 nitride films: (a)FeCrVTa_0.4W_0.4 nitride composition gradient multilayer films; (b) (FeCrVTa_0.4W_0.4)N_x single-layer films

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圖 6 FeCrVTa_0.4W_0.4氮化物薄膜的硬度和模量。（a） FeCrVTa_0.4W_0.4氮化物成分梯度多層薄膜；（b） (FeCrVTa_0.4W_0.4)N_x單層薄膜

Figure 6. Hardness and modulus of FeCrVTa_0.4W_0.4 nitride films: (a) FeCrVTa_0.4W_0.4 nitride composition gradient multilayer films; (b) (FeCrVTa_0.4W_0.4)N_x single-layer films

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圖 7 FeCrVTa_0.4W_0.4氮化物成分梯度多層梯度薄膜在不同波長下的反射率

Figure 7. Reflectivity ratio of FeCrVTa_0.4W_0.4 nitride composition gradient multilayer films at different wavelengths

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圖 8 FeCrVTa_0.4W_0.4氮化物成分梯度多層薄膜的水滴圖像。（a）N₂-0；（b）N₂-1；（c）N₂-2；（d）N₂-3

Figure 8. Water droplet image of FeCrVTa_0.4W_0.4 nitride composition gradient multilayer films: (a)N₂-0; (b) N₂-1; (c) N₂-2; (d) N₂-3

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圖 9 不同氮氣流量下(FeCrVTa_0.4W_0.4)N_x單層薄膜的方塊電阻

Figure 9. Square resistance of (FeCrVTa_0.4W_0.4)N_x single-layer films at different N₂ flows

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表 1 FeCrVTa_0.4W_0.4氮化物成分梯度多層薄膜制備參數

Table 1. Preparation parameters of FeCrVTa_0.4W_0.4 nitride composition gradient multilayer films

Number of film layer	Ar flow/ (mL·min^?1)	N₂ flow/ (mL·min^?1)	Time/min	Representation
1	130	0	90	N₂-0
2	130/130	0/15	40/40	N₂-1
3	130/130/130	0/15/30	40/40/40	N₂-2
4	130/130/130/130	0/15/30/45	40/40/40/40	N₂-3

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表 2 (FeCrVTa_0.4W_0.4)N_x單層薄膜制備參數

Table 2. Preparation parameters of (FeCrVTa_0.4W_0.4)N_x single-layer films

Number of film layer	Ar flow/ (mL·min^?1)	N₂ flow/ (mL·min^?1)	Time/min	Representation
1	130	0	90	N₂-0
1	130	15	60	N₂-15
1	130	30	60	N₂-30
1	130	45	60	N₂-45

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表 3 FeCrVTa_0.4W_0.4氮化物成分梯度多層薄膜在不同波長下的吸收率

Table 3. Absorptivity of FeCrVTa_0.4W_0.4 nitride composition gradient multilayer films at different wavelengths

Different wavelength ranges/nm	Absorptivity/%
Different wavelength ranges/nm	N₂-0	N₂-1	N₂-2	N₂-3
625–760	38.06	49.67	66.46	79.13
600–625	40.69	52.38	69.07	81.54
580–600	40.60	52.68	69.62	82.05
490–580	43.62	56.26	72.36	84.15
450–490	50.59	62.05	76.54	86.86
435–450	49.41	65.53	78.83	88.17
390–435	59.56	70.64	82.02	89.82
300–800	48.78	59.72	74.06	84.29

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