Growth of carbon nanotube arrays on various CtxMey alloy films by chemical vapour deposition method

doi:10.1016/j.jmst.2017.01.030

Abstract

Abstract:

Carbon nanotube (CNT) arrays were fabricated on Ct-Me-N-(O) alloys with content of Ct in the range of 6-40 at.% by chemical vapour deposition. The Ct was a catalytic metal from the group of the following elements: Ni, Co, Fe, Pd, while Me was a transition metal from the group of IV-VII of the periodic table (where Me = Ti, V, Cr, Zr, Nb, Mo, Ta, W, Re). Carbon nanotubes were found to grow efficiently on the alloy surface with its composition containing Ti, V, Cr, Zr, Hf, Nb or Ta. The growth of CNTs was not observed when the alloy contained W or Re. Additions of oxygen and nitrogen in the alloy facilitated the formation of oxynitrides and catalyst extrusion on the alloy surface. Replacement of the metals in alloy composition affected the diameter of the resulting CNTs. The obtained results showed that the alloy films of varying thickness (10-500 nm) may be used for the CNTs growth. The resulting CNT material was highly homogenous and its synthesis reproducible.

Key words: Carbon nanotubes, Amorphous alloys, Chemical vapour deposition, Catalytic processes, Thin films

Pawel Mierczynski, Sergey V. Dubkov, Sergey V. Bulyarskii, Alexander A. Pavlov, Sergey N. Skorik, Alexey Yu Trifonov, Agnieszka Mierczynska, Eugene P. Kitsyuk, Sergey A. Gavrilov, Tomasz P. Maniecki, Dmitry G. Gromov. Growth of carbon nanotube arrays on various Ct_xMe_y alloy films by chemical vapour deposition method[J]. J. Mater. Sci. Technol., 2018, 34(3): 472-480.

Figures/Tables 14

Table 1 CNT diameter, CNT height, CVD temperature, CVD time and elemental composition of the alloy Ct-Me-N-(O) used during the CVD synthesis.

Alloy^a	CNT diameter (nm)			CNT array height (μm)	Synthesis conditions		Raman analysis
	Minimum	Maximum	Average		Temp. (^°C)	Time (min)	I_D/I_G
Ni₁₀-Ti₃₅-N₁₅-O₄₀	12	27	21	2.1	650	10	0.92
Ni₁₀-V₃₅-N₂₀-O₃₅	12	37	22	1.0	650	10	-
Ni₁₀-Cr₃₅-N₂₀-O₃₅	9	24	18	1.2	650	10	-
Ni₁₀-Zr₃₅-N₁₅-O₄₀	5	15	7	2.2	650	10	-
Ni₁₀-Nb₃₀-N₄₀-O₂₀	9	30	18	4.6	550	10	0.99
Ni₁₀-Mo₃₅-N₂₀-O₃₀	6	27	9	0.1	550	10	-
Ni₁₅-Ta₃₅-N₂₀-O₃₀	6	15	9	1.4	650	10	1.10
Ni₁₅-W₃₅-N₂₀-O₃₀	no CNT growth; free-shape carbon build-ups			-	650	10	-
Ni₁₅-Re₃₅-N₂₀-O₃₀	no CNT growth; free-shape carbon build-ups			-	650	10	-
Co₁₀-Ti₃₅-N₁₅-O₄₀	6	33	18	2.5	600	10	0.93
Co₁₀-Zr₃₅-N₁₅-O₄₀	3	13	7	30	600	10	0.91
Co₁₅-Ta₃₅-N₂₀-O₃₀	10	35	24	12.4	550	10	1.03
Pd₁₀-Ta₃₅-N₂₀-O₃₅	no CNT growth; free-shape carbon build-ups			-	550	10	0.90
Pd₁₀-Zr₃₅-N₁₅-O₄₀	3	7	5	0.1	550	10	0.90
Fe₁₅-Ta₃₅-N₂₀-O₃₀	9	29	18	1.2	550	10	1.05

Fig. 1. SEM images of the final product by CVD method on the Ct-Me-N(O) alloy films: (a) CNT array formed on 25 nm thick Co-Zr-N-(O) film at 600 °C for 10 min; (b) free-shape carbon build-ups formed on 30 nm thick Ni-W-N-(O) film at 800 °C for 10 min.

Fig. 2. (a) SEM image of the final product obtained during CVD method on the Ni-Mo-N-(O) film at 800 °C for 10 min and (b) TEM image of the final product obtained during CVD method on the thick Ni-Mo-N-(O) film at 550 °C for10 min.

Fig. 3. Raman spectrum of CNTs as grown on a thin Co-Ta-N-(O) film formed at 550 °C for10 min.

Fig. 4. Height of the CNTs arrays versus Ct metal concentration in Ct-Me-N-(O) alloy (where Ct = Co and Me = Zr); thickness = 75 nm; temperature of 600 °C for 10 min.

Fig. 5. SEM images of the array of CNTs as grown at 650 °C during 2 min on Co-Zr-N-(O) alloy with different concentrations of the Ct metal: (а) 6 at.%; (b) 18 at.%.

Fig. 6. Dependence of CNT array height on the thickness of Co-Zr-N-(O) alloy film with concentration of Co of 18 at.% during the process performed at 600 °C for 10 min.

Fig. 7. Surface analysis of the Co-Zr-N-(O) alloy performed by Auger electron spectroscopy.

Fig. 8. Height of CNT array on Co-Zr-N-(O) alloy film (10 nm thick) versus nitrogen pressure that prevails in the magnetron chamber during film deposition at 550 °C for 10 min.

Fig. 9. CNT array height as grown on 10 nm thick Co-Zr-N-(O) alloy film versus synthesis temperature.

Fig. 10. SEM images of the final product obtained during CVD method: (a) on the Ni-Ti-N-(O) film at 380 °C for 10 min; (b) Co-Ti-N-(O) films at 380 °C for 10 min; (c) Fe-Ti-N-(O) film at 550 °C for 10 min; and (d) Pd-Ti-N-(O) films at 550 °C for 10 min at the same magnification.

Fig. 11. CNT’s array height as grown on 10 nm thick Co-Zr-N-(O) alloy film at 650 °C versus gas mixture pressure in the chamber (a) and versus C2H2 concentration (b).

Fig. 12. TEM images of 20 nm thick Ni-Nb-N-(O) alloy film: (a) initial film; (b) after annealing at 550 °C for 10 min; (c) after the CNT growth process performed at 550 °C for 7 s; (d) EDX spectrum of the individual CNT with metallic inclusion (TEM image of the object in the inset).

Fig. 13. Mechanism of CNT formation based on “phase separation” process in a thin film of Ct-Me-N-(O) alloy: (a) the initial film; (b) the film after crystallization process during annealing; (c) CNT growth [55].

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