Reduction of spectral interferences using ultraclean gold nanowire arrays in the LDI-MS analysis of a model peptide.

The surface chemistry of gold nanowires (AuNWs) has been systematically assessed in terms of contamination and cleaning processes. The nanomaterial's surface quality was correlated to its performance in the matrix-free laser desorption ionization mass spectrometry (LDI-MS) analysis of low molecular weight analytes. Arrays of AuNWs were deposited on glass slides by means of the lithographically patterned nanowire electrodeposition technique. AuNWs were then characterized in terms of surface chemical composition and morphology using X-ray photoelectron spectroscopy, scanning electron microscopy and atomic force microscopy. AuNWs were subjected to a series of well-known cleaning procedures with the aim of producing the best performing surfaces for the LDI-MS detection of leucine enkephalin, chosen as a model analyte with a molar mass below 1,000 g/mol. Prolonged cyclic voltammetry in 2 M sulfuric acid and, most of all, oxygen plasma cleaning for 5 min provided the best results in terms of simpler (interference-free) and more intense mass spectrometry spectra of the reference compound. The analyte always ionized as the sodiated adduct, and leucine enkephalin limits of detection of 0.5 and 2.5 pmol were estimated for the positive and negative analysis modes, respectively. This study points out the tight correlation existing between the chemical status of the nanostructure surface and the AuNW-assisted LDI-MS performance in terms of reproducibility of spectra, intensity of analyte ions and reduction of interferences.

Synthesis of PbTe nanowire arrays using lithographically patterned nanowire electrodeposition.

We describe the preparation by electrodeposition of arrays of lead telluride (PbTe) nanowires using the lithographically patterned nanowire electrodeposition (LPNE) method. PbTe nanowires had a rectangular cross-section with adjustable width and height ranging between 60-400 nm (w) and 20-100 nm (h). The characterization of these nanowire arrays using X-ray diffraction, transmission electron microscopy and electron diffraction, scanning electron microscopy, atomic force microscopy, and X-ray photoelectron spectroscopy (XPS) is reported. PbTe nanowires were electrodeposited using a cyclic electrodeposition-stripping technique that produced polycrystalline, stoichiometric, face-centered cubic PbTe with a mean grain diameter of 10-20 nm. These nanowires were more than 1 mm in length and two additional processing steps permitted their suspension across 25 microm air gaps microfabricated on these surfaces. The LPNE synthesis of lithographically patterned PbTe nanowires was carried out in unfiltered laboratory air. Nanowires with lengths of 70-100 microm showed an electrical resistivity comparable to bulk PbTe. XPS reveals that exposure of PbTe nanowires to air causes the formation on the nanowire surface of approximately one monolayer of a mixed lead oxide and tellurium oxide within a few minutes.