Silicon (100) substrates are ubiquitous in microfabrication and, accordingly, their surface characteristics are important. Herein, we report the analysis of Si (100) via X-ray photoelectron spectroscopy (XPS) using monochromatic Al Kα radiation. Survey scans show that the material is primarily silicon and oxygen with small amounts of carbon, nitrogen, and fluorine contamination. The Si 2p region shows two peaks that correspond to elemental silicon and silicon dioxide. Using these peaks the thickness of the native oxide (SiO2) is estimated using the equation of Strohmeier. The oxygen peak is symmetric. These silicon wafers are used as the substrate for subsequent growth of templated carbon nanotubes in the preparation of microfabricated thin layer chromatography plates.
We apply a suite of analytical tools to characterize materials created in the production of microfabricated thin layer chromatography plates. Techniques used include X-ray photoelectron spectroscopy (XPS), valence band spectroscopy, time-of-flight secondary ion mass spectrometry (ToF-SIMS) in both positive and negative ion modes, Rutherford backscattering spectroscopy (RBS), and helium ion microscopy. Materials characterized include: the Si(100) substrate with native oxide: Si/SiO 2 , alumina (35 nm) deposited as a diffusion barrier on the Si/SiO 2 : Si/SiO 2 /Al 2 O 3 , iron (6 nm) thermally evaporated on the Al 2 O 3 : Si/SiO 2 /Al 2 O 3 /Fe, the iron film annealed in H 2 to make Fe catalyst nanoparticles: Si/SiO 2 /Al 2 O 3 /Fe(NP), and carbon nanotubes (CNTs) grown from the Fe nanoparticles: Si/SiO 2 /Al 2 O 3 /Fe(NP)/CNT. The Fe films and nanoparticles appear in an oxidized state. Some of the analyses of the CNTs/CNT forests appear to be unique: (i) the CNT forest appears to exhibit an interesting 'channeling' phenomenon by RBS, (ii) we observe an odd-even effect in the SIMS spectra of C n -species for n = 1 -6, with the n ≥ 6 ions showing a steady decrease in intensity, and (iii) valence band characterization of CNTs using X-radiation is reported. Initial analysis of the CNT forest by XPS shows that it is 100 at.% carbon. After one year, only ca. 0.25 at.% oxygen is observed. The information obtained from the combination of the different analytical tools provides a more complete understanding of our materials than a single technique, which is analogous to the story of 'The Blind Men and the Elephant'. The raw XPS and ToF-SIMS spectra from this study will be submitted to Surface Science Spectra for archiving.
The authors report the ozonation of patterned, vertically aligned carbon nanotube (CNT) forests as a method of priming them for subsequent pseudo atomic layer deposition (ψ-ALD) (alternating layer deposition) of silica to produce microfabricated, CNT-templated thin layer chromatography (TLC) plates. Gas phase ozonation simplifies our deposition scheme by replacing two steps in our previous fabrication process: chemical vapor deposition of carbon and ALD of Al2O3, with this much more straightforward priming step. As shown by x-ray photoelectron spectroscopy (XPS), ozonation appears to prime/increase the number of nucleation sites on the CNTs by oxidizing them, thereby facilitating conformal growth of silica by ψ-ALD, where some form of priming appears to be necessary for this growth. (As shown previously, ψ-ALD of SiO2 onto unprimed CNTs is ineffective and leads to poor quality depositions.) In conjunction with a discussion of the challenges of good peak fitting of complex C 1s XPS narrow scans, the authors present an analysis of their C 1s data that suggests an increase in oxidized carbon, particularly the C=O group, with increasing oxygen content of the CNT forests. After coating with SiO2, the CNTs are removed by elevated temperature air oxidation, the SiO2 is rehydrated, and the plates are coated with 3-aminopropyltriethoxysilane (APTES). The resulting APTES-coated plates separate various fluorescent dyes giving results that are generally at least as good as those the authors reported previously with their more complicated fabrication/priming scheme. TLC plates with different geometries are microfabricated, where plates with narrower channels show longer run times (lower mobile phase velocities) and plates with narrower features appear to give higher efficiencies.
scite is a Brooklyn-based organization that helps researchers better discover and understand research articles through Smart Citations–citations that display the context of the citation and describe whether the article provides supporting or contrasting evidence. scite is used by students and researchers from around the world and is funded in part by the National Science Foundation and the National Institute on Drug Abuse of the National Institutes of Health.