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Use of plasma treatment to grow carbon nanotube forests on TiN substrate
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10.1063/1.3587234
/content/aip/journal/jap/109/11/10.1063/1.3587234
http://aip.metastore.ingenta.com/content/aip/journal/jap/109/11/10.1063/1.3587234
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Figures

Image of FIG. 1.
FIG. 1.

(Color online) PP results for CNT growth and nanoparticle formation. Cross-section SEM images of CNTs grown for 10 min in 0.5 mbar of C2H2 on previously plasma pretreated (a) TiN/Fe and (c) TiN/Co films; the growth temperatures are 600 °C and 480 °C, respectively; (b) is a HRTEM image of CNTs grown in (a). (d) to (f) are respectively top-view SEM images of 1 nm Ni, Co, and Fe deposited onto TiN after PP for 5 min at 600 °C in 100 mbar of H2 and dc plasma power of 50 W. (g) and (h) are histograms respectively showing lateral size distribution and diameter with Gaussian fitting (blue solid lines) of nanoparticles and nanotubes obtained using PP TiN/Fe system.

Image of FIG. 2.
FIG. 2.

(Color online) Root growth on PP samples. Cross-section SEM image of CNTs grown in 0.5 mbar of C2H2 at 600°C on 1 nm Fe previously subject to PP. C2H2 was supplied for 1 min, stopped for 5 min, and restarted for another 5 min. (b) is a schematic cartoon of root growth processes for PP on TiN films.

Image of FIG. 3.
FIG. 3.

(Color online) TiN stability during PP. (a) XRD spectra (logarithmic scale) of bare TiN, bare TiN after PP for 5 min at 600°C in 100 mbar of H2 and dc plasma power of 50 W, bare TiN after identical PP followed by CVD conditions (10 min in 0.5 mbar of C2H2 at same temperature), and Fe-coated TiN after same PP and CNT CVD. (b) and (c) are temperature-resolved XPS Ti 2p and N 1s core level lines of bare TiN upon vacuum heating. The black circles correspond to experimental data, while the gray line to fit results. The Ti 2p levels are reproduced using a Shirley background (dotted line) and 3 doublets, corresponding to Ti-N (thin continuous line), Ti4+ (thick line) and an intermediate state (dots) including Ti 2p shake up losses and Ti sub-oxides. The N 1s photoemission spectra are reproduced using a Shirley background (not shown) and 3 Gian components, corresponding to N-Ti (thick continuous line), N in interstitial sites (dotted line) and N in TiNxOy (dots).

Image of FIG. 4.
FIG. 4.

Fe-TiN interactions. (a) and (b) are respectively XPS Ti 2p, Fe 2p 3/2 core level lines of TiN subject to in situ RT Fe deposition at a constant deposition rate of ∼0.341 Å min−1 and different Fe coverage. The black circles correspond to experimental data, while the gray line to fit results. The Ti 2p levels are reproduced using a Shirley background (dotted line) and 3 doublets, corresponding to Ti-N (thin continuous line), Ti4+ (thick line) and an intermediate state (dots) including Ti 2p shake up losses and Ti sub-oxides. The Fe 2p 3/2 spectra are reproduced using a Shirley background (not shown) and 3 Gian components, corresponding to metallic Fe0 (thin line), Fe2+ (dots) and Fe3+ (dotted line, negligible within our experimental resolution). Note that Fe progressively reduces Ti4+ (present at the TiN surface after air exposure) and forms Fe2+ at the interface. Ti4+ intensity is negligible for Fe coverage higher than 0.51 nm.

Image of FIG. 5.
FIG. 5.

Stability of TiN/Fe nanoparticles. XRD spectra of (a) bare TiN at RT, (b) bare TiN upon heating up to a temperature of 650 °C in 200 mbar of Ar:H2 (30:10 sccm) for 30 min, (c) bare TiN upon heating at same conditions followed by 30 min of same conditions plus 1 sccm of C2H2, (d) TiN coated with 4 nm Fe at same conditions as (c), and (d) TiN coated with 4 nm Fe previously subject to PP/air exposure and same processing as (c).

Image of FIG. 6.
FIG. 6.

Stability of PP nanoparticles. (a) and (b) are respectively XPS Ti 2p and Fe 2p core level lines of TiN coated with 1 nm Fe, as such, or subject to PP or TP. PP was performed at 600 °C in 100 mbar of H2 and dc plasma power of 50 W for 5, 10, and 15 min, while TP was performed at exactly same conditions except for plasma off.

Image of FIG. 7.
FIG. 7.

(Color online) Growth model for PP nanoparticles. Schematic diagram of PP sequence (of Fe-coated TiN) as function of time or temperature. At PP critical time nanoparticles start diffusing into the underlying support. Uncontrolled growth after PP critical time is similar to TP growth.

Image of FIG. 8.
FIG. 8.

(Color online) Electrical evaluation of nanotube forests on TiN. I-V curves of (a) bare TiN after processing and (c) after growth of nanotube forests. (b) Schematic diagram of equivalent circuit of the electrical characterization.

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/content/aip/journal/jap/109/11/10.1063/1.3587234
2011-06-07
2014-04-16
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752b84549af89a08dbdd7fdb8b9568b5 journal.articlezxybnytfddd
Scitation: Use of plasma treatment to grow carbon nanotube forests on TiN substrate
http://aip.metastore.ingenta.com/content/aip/journal/jap/109/11/10.1063/1.3587234
10.1063/1.3587234
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