Shrouding Gas Plasma Deposition Technique for Developing Low-Friction, Wear-Resistant WS2-Zn Thin Films on Unfilled PEEK: The Relationship Between Process and Coating Properties
Abstract
:1. Introduction
2. Experimental Method
2.1. Manufacturing of the Specimen
2.2. Substrate Cleaning/Feedstock/Coating Investigations
2.3. Shrouding Gas Atmospheric Pressure Plasma Deposition
2.4. Tribological Tests
2.5. Indentation Tests
3. Results and Discussion
3.1. Feedstock, Roughness and Coating Thickness Analysis
3.2. Tribological Analysis
3.3. SEM/EDS Analysis
3.4. XPS Analysis
3.5. Creep Analysis
4. Conclusions
- The dry lubricant WS2 was well embedded into a Zn matrix giving low-friction coatings with an averaged coating thickness >14 µm, where no delamination (i.e., as deposited) was observed.
- By increasing the plasma current from 100 to 150 A, the coating thickness increases independently of the powder gas flow rate (i.e., increase of >35% with 10 L·min−1, >10% with 15 L·min−1 and >35% with 20 L·min−1 powder gas flow).
- By increasing the plasma current (i.e., from 100 to 150 A), the tungsten content increases independently of the powder gas flow rate with respect to the as-deposited coatings by SEM/EDS area analysis (i.e., increase of >19 wt% with 10 L·min−1, >20 wt% with 15 L·min−1 and >26 wt% with 20 L·min−1 powder gas flow).
- By increasing the plasma current (i.e., from 100 to 150 A), the zinc content decreases independently of the powder gas flow rate according to the as-deposited coatings by SEM/EDS area analysis (i.e., factor of 2 with 10 L·min−1, factor of 1.8 with 15 L·min−1 and factor of 1.9 with 20 L·min−1 powder gas flow).
- “Harder” coatings are generated by tuning the powder gas flow rate to lower levels (i.e., a 10 L·min−1 powder gas flow is more beneficial than 20 L·min−1 powder gas flow) in terms of aging. In addition, the Zn content variation inside the wear track represents a clear trend in terms of ductility properties, which is independent on the applied plasma current setting.
- According to the high-resolution sulfur (at.%) spectra (XPS), the quantitative loss of sulfur was significantly high as a result of the plasma coating process dependent on the plasma setup (i.e., parameters such as plasma current or powder flow rate) in contrast to the initial WS2-Zn feedstock, which was mainly affected by the plasma current and the powder gas flow rate. In fact, a loss between 81 and 89 at.% was determined (i.e., 100 A plasma jet setting).
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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APPJ Setting | Applied Parameter |
---|---|
Plasma jet current [A] | 100; 125; 150 |
Powder gas flow [L·min−1] to the plasma | 10; 15; 20 |
Plasma nozzle exit-substrate distance [mm] | 30 |
Coating velocity [mm·s−1] | 200 |
Linear coating passes [#] | 5 |
Feedstock supply [g·min−1] | 2 |
Ar gas flow [L·min−1] | 10 |
N2 shrouding gas flow [L·min−1] | 20 |
Wear Track Diameter | Linear Velocity | Static Counterpart | Test Length | Normal Load | Hertzian Stress |
---|---|---|---|---|---|
10 mm | 25 mm·s−1 | 100Cr6 ball | 100 m | 1 N | 79 MPa |
20 mm | 25 mm·s−1 | 100Cr6 ball | 628 m | 1 N | 79 MPa |
Sample Type/Coating Number | Ra (μm) | Coating Thickness (µm) |
---|---|---|
Uncoated PEEK | ≤0.50 | - |
100 A coating with 10 L·min−1 powder gas flow/E1 | 4.90 ± 0.92 | 16.14 ± 0.41 |
125 A coating with 10 L·min−1 powder gas flow/E2 | 4.14 ± 0.71 | 24.83 ± 0.12 |
150 A coating with 10 L·min−1 powder gas flow/E3 | 5.36 ± 0.88 | 25.98 ± 0.16 |
100 A coating with 15 L·min−1 powder gas flow/E4 | 4.89 ± 0.93 | 17.23 ± 0.15 |
125 A coating with 15 L·min−1 powder gas flow/E5 | 4.08 ± 0.67 | 18.99 ± 0.05 |
150 A coating with 15 L·min−1 powder gas flow/E6 | 4.58 ± 0.95 | 19.57 ± 0.04 |
100 A coating with 20 L·min−1 powder gas flow/E7 | 5.49 ± 1.18 | 14.32 ± 0.23 |
125 A coating with 20 L·min−1 powder gas flow/E8 | 4.56 ± 1.06 | 15.04 ± 0.11 |
150 A coating with 20 L·min−1 powder gas flow/E9 | 5.12 ± 0.84 | 22.17 ± 0.37 |
SEM/EDS Analysis | wt% | |||||
---|---|---|---|---|---|---|
W | Zn | S | O | Fe | Total | |
WS2-Zn as deposited of E1 | 61.0 | 30.5 | 5.5 | 3.0 | - | 100 |
WS2-Zn wear track of E1 | 57.4 | 31.9 | 6.1 | 4.1 | 0.5 | 100 |
WS2-Zn as deposited of E4 | 59.1 | 31.8 | 6.4 | 2.7 | - | 100 |
WS2-Zn wear track of E4 | 50.8 | 36.7 | 8.2 | 4.2 | 0.1 | 100 |
WS2-Zn as deposited of E7 | 53.5 | 37.6 | 5.7 | 3.2 | - | 100 |
WS2-Zn wear track of E7 | 18.9 | 65.5 | 2.5 | 13.1 | <LOD | 100 |
SEM/EDS Analysis | wt% | |||||
---|---|---|---|---|---|---|
W | Zn | S | O | Fe | Total | |
WS2-Zn as deposited of E2 | 74.0 | 16.3 | 6.5 | 3.2 | - | 100 |
WS2-Zn wear track of E2 | 69.1 | 19.0 | 6.7 | 4.3 | 0.9 | 100 |
WS2-Zn as deposited of E5 | 73.1 | 18.3 | 7.6 | 1.0 | - | 100 |
WS2-Zn wear track of E5 | 63.9 | 26.3 | 6.5 | 2.8 | 0.5 | 100 |
WS2-Zn as deposited of E8 | 65.9 | 25.5 | 6.2 | 2.4 | - | 100 |
WS2-Zn wear track of E8 | 48.5 | 42.4 | 4.9 | 4.0 | 0.2 | 100 |
SEM/EDS Analysis | wt% | |||||
---|---|---|---|---|---|---|
W | Zn | S | O | Fe | Total | |
WS2-Zn as deposited of E3 | 75.4 | 15.0 | 5.7 | 3.9 | - | 100 |
WS2-Zn wear track of E3 | 71.3 | 16.4 | 5.9 | 5.1 | 1.3 | 100 |
WS2-Zn as deposited of E6 | 74.8 | 17.2 | 6.4 | 1.6 | - | 100 |
WS2-Zn wear track of E6 | 64.8 | 25.7 | 5.3 | 3.7 | 0.5 | 100 |
WS2-Zn as deposited of E9 | 72.9 | 19.7 | 6.5 | 0.9 | - | 100 |
WS2-Zn wear track of E9 | 62.5 | 28.3 | 4.7 | 4.1 | 0.4 | 100 |
SEM/EDS Analysis | wt% | ||||||
---|---|---|---|---|---|---|---|
C | W | Zn | S | O | Fe | Total | |
WS2-Zn wear track of E1 | - | 43.1 | 46.4 | 3.6 | 6.6 | 0.3 | 100 |
WS2-Zn wear track of E4 | - | 27.5 | 61.3 | 2.6 | 8.5 | 0.1 | 100 |
WS2-Zn wear track of E7 | 60.4 | 3.9 | 27.6 | 0.4 | 7.7 | <LOD | 100 |
Feedstock | Coating E1 | Coating E4 | Coating E7 | |||||
---|---|---|---|---|---|---|---|---|
avg. | SD | avg. | SD | avg. | SD | avg. | SD | |
S2p | 35.5 | 0.9 | 3.9 | 0.5 | 6.7 | 0.9 | 6.2 | 0.5 |
W4f | 14.9 | 0.9 | 7.7 | 0.5 | 6.2 | 0.6 | 5.7 | 0.0 |
O1s | 16.6 | 1.6 | 46.3 | 0.9 | 53.2 | 2.6 | 46.7 | 5.0 |
C1s | 30.2 | 1.7 | 29.9 | 1.6 | 17.6 | 5.2 | 26.5 | 2.7 |
Zn2p | 2.8 | 0.5 | 12.2 | 0.6 | 16.3 | 1.2 | 12.5 | 1.6 |
Sample | G [GPa] | E [GPa] | K [GPa] |
---|---|---|---|
WS2-Zn (E1) | 0.51 ± 0.24 | 1.32 ± 0.64 | 1.10 ± 0.53 |
Min–max. | 0.25–0.99 | 0.64–2.57 | 0.54–2.14 |
WS2-Zn (E4) | 0.96 ± 0.59 | 2.49 ± 1.53 | 2.07 ± 1.28 |
Min–max. | 0.53–2.43 | 1.39–6.31 | 1.16–5.26 |
WS2-Zn (E7) | 0.26 ± 0.14 | 0.68 ± 0.36 | 0.57 ± 0.30 |
Min–max. | 0.13–0.49 | 0.34–1.27 | 0.28–1.06 |
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Kopp, D.; Bandl, C.; Kaindl, R.; Prethaler, T.; Coclite, A.M.; Waldhauser, W. Shrouding Gas Plasma Deposition Technique for Developing Low-Friction, Wear-Resistant WS2-Zn Thin Films on Unfilled PEEK: The Relationship Between Process and Coating Properties. Coatings 2024, 14, 1365. https://doi.org/10.3390/coatings14111365
Kopp D, Bandl C, Kaindl R, Prethaler T, Coclite AM, Waldhauser W. Shrouding Gas Plasma Deposition Technique for Developing Low-Friction, Wear-Resistant WS2-Zn Thin Films on Unfilled PEEK: The Relationship Between Process and Coating Properties. Coatings. 2024; 14(11):1365. https://doi.org/10.3390/coatings14111365
Chicago/Turabian StyleKopp, Dietmar, Christine Bandl, Reinhard Kaindl, Thomas Prethaler, Anna Maria Coclite, and Wolfgang Waldhauser. 2024. "Shrouding Gas Plasma Deposition Technique for Developing Low-Friction, Wear-Resistant WS2-Zn Thin Films on Unfilled PEEK: The Relationship Between Process and Coating Properties" Coatings 14, no. 11: 1365. https://doi.org/10.3390/coatings14111365