Influence of Atomic Oxygen on the Vacuum Tribological Performance of MoS2-Ti Composite Films Deposited by Unbalanced Magnetron Sputtering
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摘要: 对采用非平衡磁控溅射方法制备的柱状晶MoS2-Ti复合薄膜开展了原子氧(AO)辐照试验. 原子氧的平均动能是5 eV，累计辐照通量6.0×1022 atoms/cm2. 原子氧造成薄膜表面出现“绒毯”状形貌，表层的MoS2和内部的低价钛氧化物分别被氧化成硬质的MoO3和TiO2，但原子氧对距表层30 nm以下Mo的化学态没有影响. 薄膜的初始真空摩擦系数和磨损率分别由辐照前的大约0.018和4.49 × 10−17 m3/(N·m)升高至0.03 和5.5×10−17 m3/(N·m)，磨损机制也发生了由黏着磨损向磨粒磨损的转变.Abstract: MoS2-Ti composite film with columnar microstructure was fabricated by unbalanced magnetron sputtering, and was irradiated by an atomic oxygen (AO) beam with 5eV kinetic energy and total fluence of 6.0×1022 atoms/cm2. The MoS2-Ti composite film exhibited a “blanket-like” surface morphology after AO irradiation. The MoS2 phase on the film surface (within the depth of ~30 nm) and titanium suboxides (e.g. TiO2-x, where 0<x<2) inside the film were oxidized by AO into MoO3 and TiO2, respectively, leaving the MoS2 beneath the top 30 nm oxidation layer uninfluenced were oxidized to MoO3 and TiO2, leaving unchanged chemical state of element Mo in the film. After AO irradiation, initial friction coefficient and wear rate increased from 0.018 to 0.03 and 4.49 × 10−17 m3/(N·m) to 5.5 × 10−17 m3/(N·m), respectively, and its friction mechanism was transformed from adhesion to abrasion.
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Keywords:
- MoS2-Ti film /
- AO irradiation /
- vacuum /
- chemical components /
- tribological mechanism
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图 1 硅片表面沉积MoS2-Ti薄膜的断面显微结构
Figure 1. Cross-section morphology of MoS2-Ti film deposited on silicon wafer
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图 2 表面微观形态：(a)原子氧辐照前; (b)原子氧辐照后
Figure 2. Micro topography of surface: (a) before AO irradiation; (b) after AO irradiation
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图 3 原子氧辐照前表面(a)C1s , (b)N1s, (c)Ti2p, (d)Mo3d , (e)S2p和(f)O1s的精细谱分峰结果(无Ar+ ion 离子预溅射过程)
Figure 3. Curve-fitting of (a) C1s , (b) N1s, (c) Ti2p, (d) Mo3d , (e) S2p and (f) O1s spectra of the surface before AO irradiation (without pre-etching by Ar+ ion)
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图 4 原子氧辐照后表面(a)C1s , (b)N1s, (c)Ti2p, (d)Mo3d , (e)S2p和(f)O1s的精细谱分峰结果(无Ar+离子预溅射过程)
Figure 4. Curve-fitting of (a) C1s , (b) N1s, (c) Ti2p, (d) Mo3d , (e) S2p and (f) O1s spectra of the surface after AO irradiation( without pre-etching by Ar+ ion)
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图 5 Mo, S, O, Ti 和 Fe元素的浓度随Ar+累计溅射时间的变化曲线:(a)原子氧辐照前; (b)原子氧辐照后
Figure 5. Depth profile of the atomic concentrations of Mo, S, O, Ti and Fe: (a) before AO irradiation ; (b) after AO irradiation
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图 6 原子氧辐照后Mo (Mo3d5/2和Mo 3d3/2)深度剖析曲线(左图和右图每次采谱等时间间隔分别是5和10 min)
Figure 6. Profile spectra of Mo3d after AO irradiation (equal time intervals of 5 min and 10 min for left and right spectrum, respectively)
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图 7 原子氧辐照后Ti (Ti2p3/2和Ti2p1/2)深度剖析曲线(左图和右图每次采谱等时间间隔分别是5和10 min)
Figure 7. Profile spectra of Ti2p after AO irradiation (equal time intervals of 5min and 10 min for left and right spectrum, respectively)
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图 8 原子氧辐照前后摩擦系数随转数的变化曲线
Figure 8. Friction coefficient with revolution before and after AO irradiation
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图 9 4.2×105 r后磨痕的显微形貌：(a, b)原子氧辐照前; (c, d)原子氧辐照后
Figure 9. Micro morphology of the wear track after sliding 4.2×105 r: (a, b) before AO irradiation; (c, d) after AO irradiation
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图 10 4.2×105 r后磨斑的光学显微形貌：(a)原子氧辐照前；(b)原子氧辐照后
Figure 10. Optical micrographs of the corresponding wear scar after sliding 4.2×105 r: (a) before AO irradiation; (b) after AO irradiation
表 1 摩擦测试参数
Table 1 Friction testing parameters
Testing machine Friction couples Testing conditions Ball on disk in vacuum, made by CSM in Swiss Ball: Φ 8 mm stainless steel ball, Ra: 0.02.
Set1: MoS2-Ti film before AO irradiation;
Set2: MoS2-Ti film after AO irradiationVacuum: < 5×10−3 Pa，room temperature;
Sliding speed: 0.73 m/s of uni-direction;
Normal load and track radius: 5 N and 7 mm;
Revolving speed: 1 000 r/min;
Stopping criterion: terminated once reaching a total revolutions of 4.5 × 105 r (r represents revolution)
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表 2 原子氧辐照前和辐照后的薄膜表面粗糙度
Table 2 Surface roughness of the samples before and after AO irradiation
Specimen Ra/nm Rq/nm △q/(°) Before AO irradiation 51.4 68.6 2.95 After AO irradiation 50.2 64.3 2.58
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表 3 原子氧辐照前和辐照后表面的化学组成
Table 3 Chemical compositions on the surface before and after AO irradiation
Compositions Atoms fraction/% Before AO irradiation After AO irradiation Mo4+ as in MoS2 5.33 1.32 Mo6+ as in MoO3 2.66 2.85 Mo4+ as in MoO2 3.14 0.00 S2− as in MoS2 11.38 2.61 S6+ as in SO42− 0.43 3.23 Ti4+ as in TiO2 2.26 1.56 Ti3+ as in Ti2O3 0.33 0.00 O2- as in TiO2, Ti2O3, SO42−,
MoO3, MoO222.14 28.16 O2− as in −C−O, H2O 52.34 60.26
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