Early Periods of Low-Temperature Linear Antenna CVD Nucleation and Growth Study of Nanocrystalline Diamond Films
Abstract
:1. Introduction
2. Materials and Methods
2.1. Substrates
2.1.1. DND Seeding
2.1.2. CNT and EPD
2.2. LA-MPCVD
2.3. Physical Characterisations
3. Results and Discussion
3.1. First Hour of LA-MPCVD Growth
3.1.1. Silicon Substrates
3.1.2. Sapphire Substrates
3.1.3. CNT and EPD Substrates
3.2. Low MW Power
3.3. Pulse Mode MW Power
3.4. Fully Coalesced NCD Films
3.5. LA-MPCVD Growth without CO2
3.5.1. EPD-Diamond/CNT/Si Substrates
3.5.2. Silicon and Sapphire Substrates
Effect of CH4
Effect of Deposition Time
4. Conclusions
- (a)
- The substrate temperature keeps increasing during the first hours of LA-MPCVD and the NCD film remains discontinuous on the DND-seeded silicon and sapphire substrates.
- (b)
- The short duration LA-MPCVD runs for 15 min were not effective in coalescing the NCD films, but they were found to be appropriate for coating CNTs with NCDs.
- (c)
- The CNT/Si samples were found to be severely etched out under a H2/CH4/CO2 = 89/5/6 plasma recipe—more than the EPD-treated CNT/Si substrates. Pre-treatment with electrophoretic diamond seeds helped in protecting the carbon nanotubes from plasma etching, as evident from their longer CNT lengths after 15 min of LA-MPCVD runs.
- (d)
- Further prevention of plasma etching of the EPD-seeded CNT/Si substrate was observed without CO2 gas in the LA-MPCVD process recipe, with evidence of 25 µm long CNTs present even after 30 min of LA-MPCVD runs.
- (e)
- DND-seeded sapphire substrates were found to favor the formation of bigger and denser NCD particles than the silicon substrates. Moreover, the Raman signals were also found to be relatively better from sapphire substrates (FWHM of sp3 = 15 cm−1) than from the NCDs on silicon substrate, under identical LA-MPCVD parameters.
- (f)
- Lowering of the input microwave power level from 1500 to 1100 W in continuous wave mode favored the formation of connected NCDs.
- (g)
- On the other hand, pulse mode LA-MPCVD experiments were also found to help in improving NCD crystal formation with bigger grain sizes (40–90 nm on Si) and more effective surface coverage of the substrates.
- (h)
- Increasing the stage-to-antenna distance from 5 cm to 6.5 cm promoted the formation of secondary nucleation sites. Re-nucleation at longer substrate-to-quartz-tube distances, along with a longer deposition time of 2 h, are found to be essential in growing continuous NCD films.
- (i)
- The effect of increasing CH4 percentages in the process recipe was to supply more carbon atoms necessary for increasing the densities of diamond nanoparticles on DND-seeded substrates.
- (j)
- Deposition time is the most important factor for NCD growth during the early stages of LA-MPCVD. Even a higher input power of 2800 W (and therefore higher temperatures) could not significantly affect the NCD crystal sizes within short periods of time.
- (k)
- It was necessary to run the LA-MPCVD experiments for long enough (2 h) to achieve a flat stable substrate temperature (263 °C).
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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Sample id | Time (min.) | Substrate Temperature (°C) | Heating Rate (°C/min) | NCD Growth Size (nm) | H2/CH4/CO2 (%) | MW Power (W) | Pulse Mode (Frequency, Duty Cycle) | Quartz-Tube-to-Substrate Distance (cm) |
---|---|---|---|---|---|---|---|---|
LA200519-1 | 60 | 21–284 | 4.4 | 140 (sapphire) | 89/5/6 | 1500 | NO | 5 |
LA200519-2 | 30 | 108–272 | 5.5 | 30–70 (silicon) | ||||
LA200519-3 | 15 | 111–236 | 8.3 | - | ||||
LA200520-1 | 60 | 21–242 | 3.7 | 120 (sapphire) | 1100 | 5 | ||
LA200520-2 | 120 | Stable 263 | - | 20–120 (sapphire) | 6.5 | |||
LA200525-1 | 60 | 21–290 | 4.5 | 45–70 (sapphire) 40–90 (silicon) | 300 input/2000 output | YES, 20 kHz, 45% | 5 | |
LA200525-2 | 126–307 | 3 | 10–100 (silicon) | 6.5 | ||||
LA200526-1 | 15 | 21–178 | 10.5 | 30 (silicon) 20–60 (sapphire) | 97/3/0 | 1500 | NO | 5 |
LA200526-2 | 30 | 108–272 | 5.5 | 45 (silicon) 25–100 (sapphire) | 6.5 | |||
LA200605-1 | 15 | 21–170 | 9.9 | - | 96/4/0 | 5 | ||
LA200605-2 | 70–200 | 8.6 | - | 95/5/0 | ||||
LA200605-3 | 11 | 88–270 | 16.5 | - | 2800 |
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Mallik, A.K.; Shih, W.-C.; Pobedinskas, P.; Haenen, K. Early Periods of Low-Temperature Linear Antenna CVD Nucleation and Growth Study of Nanocrystalline Diamond Films. Coatings 2024, 14, 184. https://doi.org/10.3390/coatings14020184
Mallik AK, Shih W-C, Pobedinskas P, Haenen K. Early Periods of Low-Temperature Linear Antenna CVD Nucleation and Growth Study of Nanocrystalline Diamond Films. Coatings. 2024; 14(2):184. https://doi.org/10.3390/coatings14020184
Chicago/Turabian StyleMallik, Awadesh Kumar, Wen-Ching Shih, Paulius Pobedinskas, and Ken Haenen. 2024. "Early Periods of Low-Temperature Linear Antenna CVD Nucleation and Growth Study of Nanocrystalline Diamond Films" Coatings 14, no. 2: 184. https://doi.org/10.3390/coatings14020184