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Effects of hydrogen sulfide on the structure of carbon nanotubes (CNTs) were studied using high-resolution transmission electron microscopy (HRTEM) and electron energy loss spectroscopy (EELS). The CNTs were synthesized with an iron thin-film catalyst by microwave plasma-assisted CVD on the diamond substrate. The HRTEM images revealed that essentially all of the CNTs obtained in this study were multiwall (MWCNT). The addition of H2S resulted in nanotubes with split skins as cornhusks and/or frills. Electron energy loss spectra of the cornhusks indicated that they consist of sp2, sp3 and amorphous carbon phase. The spectra revealed that the sp3 to sp2 ratio at the points where cornhusks divide from the main stem was more than that at the edge of the cornhusks. No evidence of sulfur incorporation into the MWCNTs grown with the H2S addition was found. We speculate that the chemical nature of sulfur on the CNT growth yields such anomalous structure.
We investigated the growth of high-quality homoepitaxial diamond on the (111) face in a microwave-assisted plasma chemical-vapor-deposition system incorporating an individual substrate heating/cooling device. The grown diamond films were characterized by scanning electron microscopy, reflection high-energy electron diffraction, atomic force microscopy, confocal micro-Raman spectroscopy, and secondary ion mass spectrometry. The (111) diamond films show a tendency to incorporate a significant amount of hydrogen during chemical-vapor-deposition growth. Hydrogen incorporation degrades the crystal quality and surface smoothness. The amount of incorporated hydrogen decreases with the decrease in deposition temperature. We have shown that the crystal quality and surface smoothness of homoepitaxial diamond strongly depend on the substrate temperature. Independent control of the substrate temperature and incident microwave power is essential for high-quality diamond homoepitaxy.
We have characterized heteroepitaxial diamond films on Pt(111) using the nondestructive technique of confocal Raman spectroscopy to investigate the variation in structure and strain with depth. The spectral depth profiles of heteroepitaxial diamond showed the diamond peak at 1332–1335 cm-1 and four bands centered at 1230 cm-1, 1470–1490 cm-1, 1530–1580 cm-1, and 1640 cm-1 near the surface. The diamond peak shifted to the single crystal peak position at 1332 cm-1 as the linewidth was broadened with free surface proximity. The compressive strain in the heteroepitaxial diamond crystal decreased and turned into the random strain. At the same time, the Raman band at 1470–1490 cm-1 grew in intensity. The constituents of non-diamond phase in the heteroepitaxial growth regions are different from those formed in the randomly oriented regions.
In order to clarify the effect of bias treatments on the highly oriented growth of diamond, we investigated the relation between the silicon surface morphology changes after applying a bias voltage, and the orientation of the diamond crystallites after growth. We report two major findings. First, a textured structure on the Si surface after the bias pretreatment was found to be a necessary but insufficient indicator for the subsequent growth of highly oriented diamond. Second, although bias pretreatments effectively enhance nucleation, we did not find a clear relationship between the nucleation density and the percentage of oriented crystallites. The highest nucleation densities resulted in randomly oriented films. We conclude that bias pretreatments affect the nucleation enhancement and the diamond orientation through different mechanisms.
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