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

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Title: High-Throughput Density Characterization of Combinatorial Thin Films Using X-ray Reflectivity.
Authors: Addamane, Sadhvikas J.1,2 (AUTHOR) saddama@sandia.gov, Dorman, Kyle R.2 (AUTHOR), Desai, Saaketh2 (AUTHOR), Rodriguez, Mark A.2 (AUTHOR), Heile, Jonathan2 (AUTHOR), Wampler, William2 (AUTHOR), Dingreville, Remi1,2 (AUTHOR), Adams, David P.2 (AUTHOR), Boyce, Brad L.1,2 (AUTHOR)
Source: Journal of Electronic Materials. Apr2026, Vol. 55 Issue 4, p3902-3909. 8p.
Subjects: X-ray reflectometry, Thin films, Gold-platinum alloys, Nondestructive testing, Materials science
Abstract: 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. [ABSTRACT FROM AUTHOR]
Copyright of Journal of Electronic Materials is the property of Springer Nature and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)
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  Data: 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 &lt; 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. [ABSTRACT FROM AUTHOR]
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  Data: &lt;i&gt;Copyright of Journal of Electronic Materials is the property of Springer Nature and its content may not be copied or emailed to multiple sites without the copyright holder&#39;s express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract.&lt;/i&gt; (Copyright applies to all Abstracts.)
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        Value: 10.1007/s11664-025-12591-2
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        Text: English
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      – SubjectFull: X-ray reflectometry
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      – SubjectFull: Thin films
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      – SubjectFull: Gold-platinum alloys
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      – SubjectFull: Nondestructive testing
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      – SubjectFull: Materials science
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              Text: Apr2026
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