Helena Téllez

Secondary ion mass spectrometry of powdered explosive compounds for forensic evidence analysis.

RATIONALEnResidual quantities of explosives deposited on, or absorbed in, nearby surfaces can be of forensic value in post-blast analysis. As secondary ion mass spectrometry (SIMS) may be a suitable analytical approach for the screening of such residues, its performance was evaluated.nnnMETHODSnThe analyses were carried out in a SIMS instrument fitted with a quadrupole analyzer. The sample was sputtered at a 45º incidence angle with a 100 µm primary Ar(+) beam (3 keV, 500 nA). Surface sample compensation was performed with low-energy electrons (500 eV, 0.75 mA).nnnRESULTSnTNT, RDX, PETN and cloratite were deposited in powdered form on double-sided tape and introduced into the mass spectrometer, without further handling, for SIMS analysis. The analysis conditions including compensation were optimized. A mixture of energetic compounds commonly used for explosive preparation was also analyzed, proving the potential of SIMS in forensic analysis.nnnCONCLUSIONSnThis study demonstrated the possibility of detecting explosives by SIMS making use of a simple sampling procedure consisting of sticking the sample in powdered form (compatible with the collection performed in forensic post-blast analysis) onto double-sided tape without handling or preparation.

Energy‐resolved depth profiling of metal‐polymer interfaces using dynamic quadrupole secondary ion mass spectrometry

Quadrupole secondary ion mass spectrometry (qSIMS) characterization of a metallized polypropylene film used in the manufacturing of capacitors has been performed. Ar(+) primary ions were used to preserve the oxidation state of the surface. The sample exhibits an incomplete metallization that made it difficult to determine the exact location of the metal-polymer interface due to the simultaneous contribution of ions with identical m/z values from the metallic and the polymer layers. Energy filtering by means of a 45 degrees electrostatic analyzer allowed resolution of the metal-polymer interface by selecting a suitable kinetic energy corresponding to the ions generated in the metallized layer but not from the polymer. Under these conditions, selective analyses of isobaric interferences such as (27)Al(+) and (27)C(2)H(3) (+) or (43)AlO(+) and (43)C(3)H(7) (+) have been successfully performed.

Investigation of metallic interdiffusion in AlxGa1−xN/GaN/sapphire heterostructures used for microelectronic devices by SEM/EDX and SIMS depth profiling

Secondary ion mass spectrometry (SIMS) depth profiling has been applied to the study of the thermal annealing of ohmic contacts for high electron mobility transistors. The metallic stacks (Ti/Al/Ni/Au) were deposited over the Al0.28Ga0.72N/GaN/sapphire heterostructures and subjected to a rapid thermal annealing (850xa0°C for 30xa0s under N2 atmosphere) to improve the contact performance. The surface morphology and the in-depth chemical distribution of the layered contacts were severely modified due to the treatment. These modifications have been analyzed by SIMS depth profiling and scanning electron microscopy–energy-dispersive X-ray microanalysis. The SIMS analysis conditions have been optimized to achieve simultaneously good sensitivity and to avoid ion-induced mixing effects produced by the primary beam sputtering.

Atomic/molecular depth profiling of nanometric-metallized polymer thin films by secondary ion mass spectrometry.

The capability of secondary ion mass spectrometry (SIMS) to perform atomic and molecular in-depth analysis in complex nanometric-metallized thin polymer films used to manufacture capacitors is demonstrated through three different case studies related to failure analysis. The excellent repeatability and sensitivity of the technique allow us to study the degradation process of the nanometric-metallized layer in the capacitor films and the accurate location of the metal-polymer interface. The analysis of the sample is challenging due to the extreme difference in conductivity between layers, and the reduced thickness of the metallization grown on top of a rough polymeric base. However, SIMS has provided reliable and reproducible results with relative standard deviation (RSD) values better than 1.5% in the metallic layer thickness estimation. The detailed information of atomic and molecular ion in-depth distributions provided by SIMS depth profiling has allowed the identification of different factors (demetallization, generation of interstitial oxide regions, and diffusion processes or modification in the metallization thickness) that can be directly related to the origin of the lack of performance of the mounted devices.

SIMS investigation on the effect of the interstitial moisture in metallized polymer films

Dynamic SIMS depth profiling has been used to investigate the origin of the morphological and chemical degradation of metallized polymer films. The presence of the diverse oxidized species related to the main constituents of the metallization layer has been identified in samples exhibiting large decolourated regions. The in-depth analysis of these altered regions shows high contents of oxides and hydroxyl species (AlO+ and AlOH+). By comparison with pristine regions of the same sample, it has been demonstrated the pivotal role of interstitial moisture in the formation of the oxidized species in metallized polypropylene films. Care was taken to provide sufficient charge neutralization in the sample without an excess of electron flooding that could induce water emission by electron stimulated desorption.