Nondestructive analysis (NDA) based on x-ray emission is widely used, for example, in the semiconductor and concrete industries. Here, we demonstrate significant quantitative and qualitative improvements in broadband x-ray NDA by combining particle-induced emission with detection based on superconducting microcalorimeter arrays. We show that the technique offers great promise in the elemental analysis of thin-film and bulk samples, especially in the difficult cases where tens of different elements with nearly overlapping emission lines have to be identified down to trace concentrations. We demonstrate the efficiency and resolving capabilities by spectroscopy of several complex multielement samples in the energy range 1-10 keV, some of which have a trace amount of impurities not detectable with standard silicon drift detectors. The ability to distinguish the chemical environment of an element is also demonstrated by measuring the intensity differences and chemical shifts of the characteristics x-ray peaks of titanium compounds. In particular, we report measurements of the Kα=Kβ intensity ratio of thin films of TiN and measurements of Ti Kα satellite peak intensities in various Ti thin-film compounds. We also assess the detection limits of the technique, comment on detection limits possible in the future, and discuss possible applications.

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We have determined minimum detection limits, MDLs, for elements 14 ≤ Z ≤ 86 using a transition-edge sensor array, TES array, and as a comparison using an Amptek X-123SDD silicon drift detector, SDD. This was done using a 3 MeV proton beam and a 5.1 MeV helium beam. MDLs were determined for a thin film sample on top of C substrate, and for a bulk sample containing mostly Al. Due to the smaller peak-to-background ratio, lower detection limits were obtainable using the TES array for most of the elements. However, for elements 30 ≤ Z ≤ 45 the performance of the TES array was not as good as the SDD performance. This is due to the limitations of the TES used at energies > 10 keV. The greatest advantage of TES comes, however, when detecting low intensity peaks close to high intensity peaks. Such a case was demonstrated by measuring a fly ash with overlapping Ti, V, Ba, and Ce peaks, where minimum detection limits of V, Ba, and Ce were decreased by factor of 620, 400, and 680, respectively compared to the SDD.

In situ spectroscopic ellipsometry study on the growth of ultrathin TiN films by plasma-assisted atomic layer deposition Abstract. The performance, strengths and limitations of RBS and PIXE for the characterization of trace amounts of Cl in TiN thin films are critically compared. The chlorine atomic concentration in ALD grown TiN thin films on Si is determined for samples grown at temperatures ranging from 350°C to 550°C. We show that routine Rutherford backscattering spectrometry measurements (1.5 MeV He + ) and PIXE measurements (1.5 MeV H + ) on 20 nm thick TiN films allow one to determine the Cl content down to 0.3 at% with an absolute statistical accuracy reaching 0.03 at%. Possible improvements to push the sensitivity limit for both approaches are proposed.