J. Mater. Sci. Technol. ›› 2022, Vol. 109: 114-128.DOI: 10.1016/j.jmst.2021.08.077
• Research Article • Previous Articles Next Articles
Xubing Weia,b, Shaomiao Shia, Chuangming Ninga, Zhibin Lua,*(
), Guangan Zhanga,b,*()
Received:2021-01-13
Revised:2021-07-11
Accepted:2021-08-09
Published:2022-05-20
Online:2021-11-06
Contact:
Zhibin Lu,Guangan Zhang
About author:gazhang@licp.cas.cn (G. Zhang).Xubing Wei, Shaomiao Shi, Chuangming Ning, Zhibin Lu, Guangan Zhang. Si-DLC films deposited by a novel method equipped with a co-potential auxiliary cathode for anti-corrosion and anti-wear application[J]. J. Mater. Sci. Technol., 2022, 109: 114-128.
Fig. 1. Schematic diagram of the novel Si-DLC film deposition method by equipping a co-potential auxiliary cathode.
| Processing | Gas flow (sccm) | Deposition voltage (kV) | Vacuum degree (Pa) | Deposition time (min) | ||
|---|---|---|---|---|---|---|
| Ar | SiH4 | C2H2 | ||||
| Empty Cell | ||||||
| Cleaning | 200 | 6 | 1.5 | 20 | ||
| Adhesion | 150 | 50 | 15 | 12 | 25 | |
| SiX-DLC | 100 | 50 | 150 | 0.8 | 5.9-6.0 | 4.5 |
| SiY-DLC | 100 | 50 | 50 | 3.9-4.0 | 1.5 | |
Table 1. Deposition parameters of Si-DLC film by the novel deposition method by equipping a co-potential auxiliary cathode.
| Processing | Gas flow (sccm) | Deposition voltage (kV) | Vacuum degree (Pa) | Deposition time (min) | ||
|---|---|---|---|---|---|---|
| Ar | SiH4 | C2H2 | ||||
| Empty Cell | ||||||
| Cleaning | 200 | 6 | 1.5 | 20 | ||
| Adhesion | 150 | 50 | 15 | 12 | 25 | |
| SiX-DLC | 100 | 50 | 150 | 0.8 | 5.9-6.0 | 4.5 |
| SiY-DLC | 100 | 50 | 50 | 3.9-4.0 | 1.5 | |
Fig. 2. Raman spectra (a) of Si-DLC films deposited by a novel deposition method at different region and its G peak wavenumber (b), ID/IG (c) and FWHMG (d).
Fig. 3. ATR-FTIR spectra of Si-DLC films at different region by a novel deposition method equipping a co-potential auxiliary cathode.
Fig. 4. Cross-sectional images of Si-DLC films deposited by a novel deposition method and its thickness.
Fig. 5. Residual stress of Si-DLC films at different region by a novel deposition method equipping a co-potential auxiliary cathode.
Fig. 6. Surface roughness of Si-DLC films on the surface of HSS M2 (a) and 304SS (b).
Fig. 7. Load-depth curves (a, b), ER% (c), hardness, elastic modulus (d), H/E and H3/E2 (e) of HSS M2 and Si-DLC film deposited on the HSS M2 by a novel deposition method.
Fig. 8. Scratch images of Si-DLC film on the surface of HSS M2.
| Sample | Region 1 | Region 2 | Region 3 | Region 4 | Region 5 |
|---|---|---|---|---|---|
| Si-DLC/HSS M2 | 12.2 N | 10.5 N | 10.1 N | 10.5 N | 9.6 N |
Table 2. Critical load of Si-DLC film on the surface of HSS M2.
| Sample | Region 1 | Region 2 | Region 3 | Region 4 | Region 5 |
|---|---|---|---|---|---|
| Si-DLC/HSS M2 | 12.2 N | 10.5 N | 10.1 N | 10.5 N | 9.6 N |
Fig. 9. OCP as a function of time (a) and potentiodynamic polarization curves (b) of 304SS and Si-DLC film deposited by a novel deposition method in3.5 wt% NaCl solution.
| Samples | OCP (V) | Ecorr (V) | jcorr (A cm-2) | βc (V) | βa (V) | Rp (Ω cm2) | P (%) | □2 |
|---|---|---|---|---|---|---|---|---|
| 304SS | -0.269 | -0.266 | 1.98 × 10-6 | 0.26 | 1.01 | 4.53 × 104 | 100 | 1.6 × 10-1 |
| Region 1 | 0.108 | -0.165 | 2.14 × 10-8 | 0.16 | 1.06 | 2.82 × 106 | 1.29 | 5.2 × 10-2 |
| Region 2 | 0.102 | -0.161 | 2.04 × 10-8 | 0.16 | 0.91 | 2.90 × 106 | 1.20 | 2.6 × 10-2 |
| Region 3 | 0.077 | -0.144 | 2.66 × 10-8 | 0.18 | 0.96 | 2.47 × 106 | 1.37 | 4.6 × 10-2 |
| Region 4 | 0.087 | -0.152 | 2.44 × 10-8 | 0.16 | 0.78 | 2.36 × 106 | 1.24 | 4.3 × 10-2 |
| Region 5 | 0.083 | -0.154 | 4.05 × 10-8 | 0.19 | 0.95 | 1.70 × 106 | 2.04 | 1.9 × 10-2 |
Table 3. Polarization results of 304SS and Si-DLC film at different regions.
| Samples | OCP (V) | Ecorr (V) | jcorr (A cm-2) | βc (V) | βa (V) | Rp (Ω cm2) | P (%) | □2 |
|---|---|---|---|---|---|---|---|---|
| 304SS | -0.269 | -0.266 | 1.98 × 10-6 | 0.26 | 1.01 | 4.53 × 104 | 100 | 1.6 × 10-1 |
| Region 1 | 0.108 | -0.165 | 2.14 × 10-8 | 0.16 | 1.06 | 2.82 × 106 | 1.29 | 5.2 × 10-2 |
| Region 2 | 0.102 | -0.161 | 2.04 × 10-8 | 0.16 | 0.91 | 2.90 × 106 | 1.20 | 2.6 × 10-2 |
| Region 3 | 0.077 | -0.144 | 2.66 × 10-8 | 0.18 | 0.96 | 2.47 × 106 | 1.37 | 4.6 × 10-2 |
| Region 4 | 0.087 | -0.152 | 2.44 × 10-8 | 0.16 | 0.78 | 2.36 × 106 | 1.24 | 4.3 × 10-2 |
| Region 5 | 0.083 | -0.154 | 4.05 × 10-8 | 0.19 | 0.95 | 1.70 × 106 | 2.04 | 1.9 × 10-2 |
Fig. 10. Surface morphology images of 304SS and Si-DLC at different regions before and after electrochemical corrosion tests.
Fig. 11. EIS results of 304SS and Si-DLC film at different regions: (a, b) Bode plots, (c) Nyquist; and EC models for substrate (d) and Si-DLC films (e).
| Samples | R1 (Ω cm2) | CPE1 | R2 (Ω cm2) | CPE2 | R3 (Ω cm2) | CPE3 | WO | □2 | |||||
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
| C1 (F cm-2) | n1 | C2 (F cm-2) | n2 | C3 (F cm-2) | n3 | Rw (Ω cm2) | Cw (F cm-2) | nw | |||||
| 304SS | 10,900 | 6.42 × 10-5 | 0.85 | — | — | — | — | — | — | — | — | — | 6.91 × 10-2 |
| Region 1 | — | — | — | 9717 | 4.59 × 10-8 | 0.65 | 69,549 | 1.33 × 10-7 | 0.87 | 9041 | 0.073 | 0.44 | 1.42 × 10-3 |
| Region 2 | — | — | — | 12,074 | 5.98 × 10-8 | 0.62 | 90,280 | 7.96 × 10-8 | 0.87 | 11,736 | 0.080 | 0.44 | 1.41 × 10-3 |
| Region 3 | — | — | — | 5956 | 2.26 × 10-8 | 0.71 | 63,092 | 6.21 × 10-7 | 0.66 | 8202 | 0.092 | 0.53 | 2.81 × 10-3 |
| Region 4 | — | — | — | 5775 | 2.84 × 10-8 | 0.68 | 65,858 | 5.08 × 10-7 | 0.67 | 8561 | 0.048 | 0.50 | 2.31 × 10-3 |
| Region 5 | — | — | — | 5700 | 2.18 × 10-8 | 0.71 | 44,833 | 7.94 × 10-7 | 0.64 | 5828 | 0.065 | 0.52 | 2.34 × 10-3 |
Table 4. Detailed EC parameters obtained by EIS results of 304SS and Si-DLC film at different regions.
| Samples | R1 (Ω cm2) | CPE1 | R2 (Ω cm2) | CPE2 | R3 (Ω cm2) | CPE3 | WO | □2 | |||||
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
| C1 (F cm-2) | n1 | C2 (F cm-2) | n2 | C3 (F cm-2) | n3 | Rw (Ω cm2) | Cw (F cm-2) | nw | |||||
| 304SS | 10,900 | 6.42 × 10-5 | 0.85 | — | — | — | — | — | — | — | — | — | 6.91 × 10-2 |
| Region 1 | — | — | — | 9717 | 4.59 × 10-8 | 0.65 | 69,549 | 1.33 × 10-7 | 0.87 | 9041 | 0.073 | 0.44 | 1.42 × 10-3 |
| Region 2 | — | — | — | 12,074 | 5.98 × 10-8 | 0.62 | 90,280 | 7.96 × 10-8 | 0.87 | 11,736 | 0.080 | 0.44 | 1.41 × 10-3 |
| Region 3 | — | — | — | 5956 | 2.26 × 10-8 | 0.71 | 63,092 | 6.21 × 10-7 | 0.66 | 8202 | 0.092 | 0.53 | 2.81 × 10-3 |
| Region 4 | — | — | — | 5775 | 2.84 × 10-8 | 0.68 | 65,858 | 5.08 × 10-7 | 0.67 | 8561 | 0.048 | 0.50 | 2.31 × 10-3 |
| Region 5 | — | — | — | 5700 | 2.18 × 10-8 | 0.71 | 44,833 | 7.94 × 10-7 | 0.64 | 5828 | 0.065 | 0.52 | 2.34 × 10-3 |
Fig. 12. Friction coefficient curves (a), average friction coefficient (b) and wear rate (c) of Si-DLC films at different region; wear rate (d) of GCr15 steel ball.
Fig. 13. Optical microscope images (a) of Si-DLC films at different regions, HSS M2 and GCr15 steel ball after fiction tests; Raman spectra of GCr15 steel ball worn with Si-DLC film at different region (b).
Fig. 14. Optical images of Si-DLC films (～ 4 μm) on the surface of gears (a), drills (b) and bearings (c-e).
| Samples | Deposition rate (nm/min) | Intrinsic stress (GPa) | Surface roughness (nm) | Hardness (GPa) | Elastic modulus (GPa) | Adhesive strength (N) | Corrosion current density (A cm-2) | Friction coefficient | Wear rate (mm3 N-1 m-1) |
|---|---|---|---|---|---|---|---|---|---|
| This study | >30 | 0.1-0.3 | 5.8-14.7 | 15-17 | ∼125 | ∼10 | ∼2 × 10-8 | ∼0.05 | 3-4 × 10-7 |
| Ref. [ | ∼6 | 298 | 5.3 × 10-6 | 0.17 | 3.4 × 10-6 | ||||
| Ref. [ | ∼80 | 0.7-1.5 | 1.1-8.1 × 10-8 | ||||||
| Ref. [ | 1.5-1.8 μm (total thickness) | ∼0.15 | 3.2 × 10-7 | ||||||
| Ref. [ | 20-25 | >0.8 | 12-22 | 130-200 | |||||
| Ref. [ | 1.6-2.5 | 1.5-3 | 6-12 | 100-200 | 6-9.6 | ||||
| Ref. [ | ∼7 | 13.8 | 164.6 | 32.8 | 0.09-0.12 | 3.3-4.2 × 10-7 | |||
| Ref. [ | 40-58 | 17-21.5 | 141-160 | <0.1 | |||||
| Ref. [ | >40 | ∼0.5 | 20-25 |
Table 5. Comparison of Si-DLC deposited by different deposition methods.
| Samples | Deposition rate (nm/min) | Intrinsic stress (GPa) | Surface roughness (nm) | Hardness (GPa) | Elastic modulus (GPa) | Adhesive strength (N) | Corrosion current density (A cm-2) | Friction coefficient | Wear rate (mm3 N-1 m-1) |
|---|---|---|---|---|---|---|---|---|---|
| This study | >30 | 0.1-0.3 | 5.8-14.7 | 15-17 | ∼125 | ∼10 | ∼2 × 10-8 | ∼0.05 | 3-4 × 10-7 |
| Ref. [ | ∼6 | 298 | 5.3 × 10-6 | 0.17 | 3.4 × 10-6 | ||||
| Ref. [ | ∼80 | 0.7-1.5 | 1.1-8.1 × 10-8 | ||||||
| Ref. [ | 1.5-1.8 μm (total thickness) | ∼0.15 | 3.2 × 10-7 | ||||||
| Ref. [ | 20-25 | >0.8 | 12-22 | 130-200 | |||||
| Ref. [ | 1.6-2.5 | 1.5-3 | 6-12 | 100-200 | 6-9.6 | ||||
| Ref. [ | ∼7 | 13.8 | 164.6 | 32.8 | 0.09-0.12 | 3.3-4.2 × 10-7 | |||
| Ref. [ | 40-58 | 17-21.5 | 141-160 | <0.1 | |||||
| Ref. [ | >40 | ∼0.5 | 20-25 |
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