The work presented herein evaluates silicon nano-pillar arrays for use in planar chromatography. Electron beam lithography and metal thermal dewetting protocols were used to create nano-thin layer chromatography platforms. With these fabrication methods we are able to reduce the size of the characteristic features in a separation medium below that used in ultra-thin layer chromatography; i.e. pillar heights are 1-2 μm and pillar diameters are typically in the 200-400 nm range. In addition to the intrinsic nanoscale aspects of the systems, it is shown they can be further functionalized with nanoporous layers and traditional stationary phases for chromatography; hence exhibit broad-ranging lab-on-a-chip and point-of-care potential. Because of an inherent high permeability and very small effective mass transfer distance between pillars, chromatographic efficiency can be very high but is enhanced herein by stacking during development and focusing while drying, yielding plate heights in the nm range separated band volumes. Practical separations of fluorescent dyes, fluorescently derivatized amines, and anti-tumor drugs are illustrated.
A fundamental problem with efficiency in capillary action driven planar chromatography results from diminishing flow rates as development proceeds, giving rise to molecular diffusion related band dispersion for most sample types. Overpressure and electrokinetic means to speed flow have been used successfully in TLC. We explore the use of centrifugal force (CF) to drive flow for reduced-dimension planar platforms (ultra-TLC, low micrometer features, and nano-TLC, nanoscale features). The silicon wafer platforms have two forms of continuous 2D arrays created by either photolithography or metal dewetting followed by deep reactive ion etching and coated with porous SiO . The flow pattern is unusual with co-planar flows above and within the arrays. The effects of parameters such as spin rate, solvent type, and surface character on flow rates is established and can be substantially greater than capillary action flow. Using fluorescent dyes, we investigate retardation factors and chromatographic plate height; the latter falls in the low to sub-micrometer range. To the best of our knowledge, we demonstrate the first analytical separations performed in pillar arrays using CF to augment solvent flow.
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