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<p>Combinatorial synthesis approaches are often coupled with high-throughput characterization techniques so as to effectively facilitate accelerated material discovery. In this study, a rapid and nondestructive method based on x-ray reflectivity (XRR) was developed to measure the density of combinatorial thin films without any prior microstructural assumptions. Utilizing automated methods, x-ray reflectograms were acquired from 560 combinatorial Pt-Au, 112 elemental Pt, and 112 elemental Au thin films fabricated on Si (100) wafers (112 deposition areas per wafer), and these datasets were evaluated using a unique analysis approach to rapidly deduce thin film densities. Traditionally, complex fitting procedures are applied to XRR to estimate the critical angle <i>θ</i><sub>c</sub> (angle at or below which total reflection occurs), which can then be used to calculate the film density. This study demonstrates an alternative, rapid method—using an indirect surrogate angle <i>θ</i><sub>s</sub> (instead of <i>θ</i><sub>c</sub>) that is numerically calculated (without any curve-fitting) as the minimum in the first derivative of the acquired XRR profiles. It was found that density values estimated using <i>θ</i><sub>s</sub> and adjusted with a systematic offset were generally in agreement with the traditional curve-fitting method, with typical average error percentages peaking at &lt; 2% (maximum deviation = 10%) and reduction in hands-on analysis time by ~95%. The systematic offset in density compensates for the difference between <i>θ</i><sub>c</sub> and <i>θ</i><sub>s</sub> and was determined by comparing densities computed using the traditional curve-fitting approach and densities calculated using <i>θ</i><sub>s</sub> at only four (out of 112) deposition areas per wafer that we defined as calibration anchors. The results of our approach were validated using two avenues: (1) densities deduced from traditional curve-fitting at all 112 deposition areas on several wafers, and (2) ground-truth density measurements at the anchor areas with Rutherford backscattering spectroscopy and thickness profilometry. This new method for rapid assessment of combinatorial thin film density with XRR using a numerically calculated surrogate angle and without any complex curve-fitting can be extended to other material systems (e.g., Cu-Ag, Ni-Co), thereby realizing the benefits of combinatorial synthesis for expedited discovery.</p>

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High-Throughput Density Characterization of Combinatorial Thin Films Using X-ray Reflectivity

  • 期刊论文

  • 发表日期：

    2025年12月19日

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  • Sadhvikas J. Addamane,
  • Kyle R. Dorman,
  • Saaketh Desai,
  • Mark A. Rodriguez,
  • Jonathan Heile,
  • William Wampler,
  • Remi Dingreville,
  • David P. Adams,
  • Brad L. Boyce

摘要

Combinatorial synthesis approaches are often coupled with high-throughput characterization techniques so as to effectively facilitate accelerated material discovery. In this study, a rapid and nondestructive method based on x-ray reflectivity (XRR) was developed to measure the density of combinatorial thin films without any prior microstructural assumptions. Utilizing automated methods, x-ray reflectograms were acquired from 560 combinatorial Pt-Au, 112 elemental Pt, and 112 elemental Au thin films fabricated on Si (100) wafers (112 deposition areas per wafer), and these datasets were evaluated using a unique analysis approach to rapidly deduce thin film densities. Traditionally, complex fitting procedures are applied to XRR to estimate the critical angle θc (angle at or below which total reflection occurs), which can then be used to calculate the film density. This study demonstrates an alternative, rapid method—using an indirect surrogate angle θs (instead of θc) that is numerically calculated (without any curve-fitting) as the minimum in the first derivative of the acquired XRR profiles. It was found that density values estimated using θs and adjusted with a systematic offset were generally in agreement with the traditional curve-fitting method, with typical average error percentages peaking at < 2% (maximum deviation = 10%) and reduction in hands-on analysis time by ~95%. The systematic offset in density compensates for the difference between θc and θs and was determined by comparing densities computed using the traditional curve-fitting approach and densities calculated using θs at only four (out of 112) deposition areas per wafer that we defined as calibration anchors. The results of our approach were validated using two avenues: (1) densities deduced from traditional curve-fitting at all 112 deposition areas on several wafers, and (2) ground-truth density measurements at the anchor areas with Rutherford backscattering spectroscopy and thickness profilometry. This new method for rapid assessment of combinatorial thin film density with XRR using a numerically calculated surrogate angle and without any complex curve-fitting can be extended to other material systems (e.g., Cu-Ag, Ni-Co), thereby realizing the benefits of combinatorial synthesis for expedited discovery.