Practical Guides for X-Ray Photoelectron Spectroscopy (XPS): First Steps in planning, conducting and reporting XPS measurements.

Over the past three decades, the widespread utility and applicability of X-ray photoelectron spectroscopy (XPS) in research and applications has made it the most popular and widely used method of surface analysis. Associated with this increased use has been an increase in the number of new or inexperienced users which has led to erroneous uses and misapplications of the method. This article is the first in a series of guides assembled by a committee of experienced XPS practitioners that are intended to assist inexperienced users by providing information about good practices in the use of XPS.

Atomic-scale phase composition through multivariate statistical analysis of atom probe tomography data.

We demonstrate for the first time that multivariate statistical analysis techniques can be applied to atom probe tomography data to estimate the chemical composition of a sample at the full spatial resolution of the atom probe in three dimensions. Whereas the raw atom probe data provide the specific identity of an atom at a precise location, the multivariate results can be interpreted in terms of the probabilities that an atom representing a particular chemical phase is situated there. When aggregated to the size scale of a single atom (∼0.

Characterization of dilute species within CVD-grown silicon nanowires doped using trimethylboron: protected lift-out specimen preparation for atom probe tomography.

Three-dimensional quantitative compositional analysis of nanowires is a challenge for standard techniques such as secondary ion mass spectrometry because of specimen size and geometry considerations; however, it is precisely the size and geometry of nanowires that makes them attractive candidates for analysis via atom probe tomography. The resulting boron composition of various trimethylboron vapour-liquid-solid grown silicon nanowires were measured both with time-of-flight secondary ion mass spectrometry and pulsed-laser atom probe tomography. Both characterization techniques yielded similar results for relative composition.

Effect of surface free energy on PDMS transfer in microcontact printing and its application to ToF-SIMS to probe surface energies.

Although polydimethylsiloxane (PDMS) transfer during microcontact printing (microCP) has been observed in previous reports, which generally focused on only one or a few different substrates, in this work we investigate the extent of PDMS transfer onto a series of surfaces with a wide range of hydrophobicities using an uninked, unpatterned PDMS stamp. These surfaces include clean silicon, clean titanium, clean gold, "dirty" silicon, polystyrene, Teflon, surfaces modified with PEG, amino, dodecyl, and hexadecyl monolayers, and also two loose molecular materials. The PDMS transferred onto planar surfaces is, in general, easily detected by wetting and spectroscopic ellipsometry.

Multivariate statistical analysis of three-spatial-dimension TOF-SIMS raw data sets.

Three-spatial-dimension (3D) time-of-flight-secondary ion mass spectrometry (TOF-SIMS) analysis can be performed if an X-Y image is saved at each depth of a depth profile. In this paper, we will show how images reconstructed from specified depths, depth profiles generated from specific X-Y coordinates, as well as three-spatial-dimensional rendering provide for a better understanding of the sample than traditional depth profiling where only a single spectrum is collected at each depth. We will also demonstrate, for the first time, that multivariate statistical analysis (MVSA) tools can be used to perform a rapid, unbiased analysis of the entire 3D data set.

Time of flight secondary ion mass spectrometry: a powerful high throughput screening tool.

Combinatorial materials libraries are becoming more complicated; successful screening of these libraries requires the development of new high throughput screening methodologies. Time of flight secondary ion mass spectrometry (ToF-SIMS) is a surface analytical technique that is able to detect and image all elements (including hydrogen which is problematic for many other analysis instruments) and molecular fragments, with high mass resolution, during a single measurement. Commercial ToF-SIMS instruments can image 500 microm areas by rastering the primary ion beam over the region of interest.

Chemomechanical nanolithography: nanografting on silicon and factors impacting linewidth.

We present a two-fold extension of previous work on Atomic Force Microscope-based chemomechanical functionalization: (1) chemomechanical nanografting, which extends chemomechanical functionalization to a more stable initial surface, and (2) linewidth studies that show the impact of force and Atomic Force Microscope probe tip wear on patterning resolution. Alkene, alcohol, and alkyl halide molecules were nanografted to silicon and imaged with in situ atomic force microscopy, time-of-flight secondary ion mass spectrometry with Automated eXpert Spectrum Image Analysis, and scanning electron microscopy. Chemomechanical nanografting demonstrated linewidths down to 50 nm.

Matrix implanted laser desorption ionization (MILDI) combined with ion mobility-mass spectrometry for bio-surface analysis.

The implantation of low velocity massive gold cluster ions allows homogeneous incorporation of a metallic matrix into the near-surface region of rat brain tissues. Subsequent analysis by laser desorption ionization mass spectrometry yields spectra exhibiting molecular ion peaks in the mass range up to 35 kDa similar to those observed by matrix-assisted LDI. Matrix-implanted LDI when combined with ion-mobility preseparation promises to be a useful technique for molecular imaging of biotissues with a laser microprobe.

Multivariate statistical analysis of concatenated time-of-flight secondary ion mass spectrometry spectral images. Complete description of the sample with one analysis.

Time-of-flight secondary ion mass spectrometry (TOF-SIMS) instruments are capable of saving an entire mass spectrum at each pixel of an image, allowing for retrospective analysis of masses that were not selected for analysis during data collection. These TOF-SIMS spectral images contain a wealth of information, but few tools are available to assist the analyst in visualizing the entire raw data set and as a result, most of the data are not analyzed. Automated, nonbiased, multivariate statistical analysis (MVSA) techniques are useful for converting the massive amount of data into a smaller number of chemical components (spectra and images) that are needed to fully describe the TOF-SIMS measurement.