This dissertation describes advances in the microfabrication of thin layer chromatography (TLC) plates. These plates are prepared by the patterning of carbon nanotube (CNT) forests on substrates, followed by their infiltration with an inorganic material. This document is divided into ten sections or chapters. Chapter 1 reviews the basics of conventional TLC technology. This technology has not changed substantially in decades. This chapter also mentions some of the downsides of the conventional approach, which include unwanted interactions of the binder in the plates with the analytes, relatively slow development times, and only moderately high efficiencies. Chapter 2 focuses primarily on the tuning of the iron catalyst used to grow the CNTs, which directly influences the diameters of the CNTs grown that are produced. Chapter 3 focuses on the atomic layer deposition (ALD) of SiO2 from a silicon precursor and ozone onto carbon-nanotubes to obtain an aluminum free stationary phase. This approach allowed us to overcome the tailing issues associated with the earlier plates prepared in our laboratory. Chapter 4 is a study of the hydroxylation state of the silica in our TLC plates. A linear correlation was obtained between the SiOH+/Si+ time-of-flight secondary ion mass spectrometry (ToF-SIMS) peak ratio and the isolated silanol peak position at ca. 3740 cm-1 in the diffuse reflectance infrared spectroscopy (DRIFT) spectra. We also compared the hydroxylation efficiencies on our plates of ammonium hydroxide and HF. Chapter 5 reports a series of improvements in TLC plate preparation. The first is the low-pressure chemical vapor deposition (LPCVD) of silicon nitride onto CNTs, which can be used to make very robust TLC plates that have the necessary SiO2 surfaces. These TLC plates are the best we have prepared to date. We also describe here the ALD deposition of ZnO into these devices, which can make them fluorescent. Chapters 6 – 10 consist of contributions to Surface Science Spectra (SSS) of ToF-SIMS spectra of the materials used in our microfabrication process. SSS is a peer-reviewed database that has been useful to many in the surface community. The ToF-SIMS spectra archived include those of (i) Si/SiO2, (ii) Si/SiO2/Al2O3, (iii) Si/SiO2/Al2O3/Fe, (iv) Si/SiO2/Fe (annealed at 750 °C in H2), and (v) Si/SiO2/Al2O3/Fe(annealed)/CNTs. Both positive and negative ion spectra have been submitted. In summary, the present work is a description of advances in the development, thorough characterization, optimization, and application development of microfabricated thin layer chromatography plates that are superior to their commercial counterparts.



College and Department

Physical and Mathematical Sciences; Chemistry and Biochemistry



Date Submitted


Document Type





Microfabrication, thin layer chromatography, carbon nanotubes, atomic layer deposition, silica, zinc oxide, low-pressure chemical vapor deposition, SIMS