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    <title language="eng">Toward determination of the surface roughness of particles from a SEM image</title>
    <abstract language="eng">In this communication, we address the issue of roughness measurement by investigating if the grayscale values from SEM images can be used for surface roughness determination of spherical particles.</abstract>
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    <author>Ardian Gojani</author>
    <author>Charlie Tobias</author>
    <author>Deniz Hülagü</author>
    <author>Knut Rurack</author>
    <author>Vasile-Dan Hodoroaba</author>
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    <subject>
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      <value>Particle characterisation</value>
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    <subject>
      <language>eng</language>
      <type>uncontrolled</type>
      <value>Roughness</value>
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    <collection role="ddc" number="543">Analytische Chemie</collection>
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    <collection role="institutes" number="">1.9 Chemische und optische Sensorik</collection>
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    <title language="eng">Towards 3D determination of the surface roughness of core–shell microparticles as a routine quality control procedure by scanning electron microscopy</title>
    <abstract language="eng">AbstractRecently, we have developed an algorithm to quantitatively evaluate the roughness of spherical microparticles using scanning electron microscopy (SEM) images. The algorithm calculates the root-mean-squared profile roughness (RMS-RQ) of a single particle by analyzing the particle’s boundary. The information extracted from a single SEM image yields however only two-dimensional (2D) profile roughness data from the horizontal plane of a particle. The present study offers a practical procedure and the necessary software tools to gain quasi three-dimensional (3D) information from 2D particle contours recorded at different particle inclinations by tilting the sample (stage). This new approach was tested on a set of polystyrene core-iron oxide shell-silica shell particles as few micrometer-sized beads with different (tailored) surface roughness, providing the proof of principle that validates the applicability of the proposed method. SEM images of these particles were analyzed by the latest version of the developed algorithm, which allows to determine the analysis of particles in terms of roughness both within a batch and across the batches as a routine quality control procedure. A separate set of particles has been analyzed by atomic force microscopy (AFM) as a powerful complementary surface analysis technique integrated into SEM, and the roughness results have been compared.</abstract>
    <parentTitle language="eng">Scientific Reports</parentTitle>
    <identifier type="issn">2045-2322</identifier>
    <identifier type="doi">10.1038/s41598-024-68797-7</identifier>
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    <licence>Creative Commons - CC BY - Namensnennung 4.0 International</licence>
    <author>Deniz Hülagü</author>
    <author>Charlie Tobias</author>
    <author>Radek Dao</author>
    <author>Pavel Komarov</author>
    <author>Knut Rurack</author>
    <author>Vasile-Dan Hodoroaba</author>
    <subject>
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      <value>Core–shell particles</value>
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      <value>Roughness</value>
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      <value>Scanning electron microscopy</value>
    </subject>
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      <value>Atomic force microscopy</value>
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      <value>Tilting</value>
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      <value>Batch analysis</value>
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    <title language="eng">Towards automated scanning electron microscopy image analysis of core-shell microparticles for quasi-3D determination of the surface roughness</title>
    <abstract language="eng">Core-shell (CS) particles have been increasingly used for a wide range of applications due to their unique properties by merging individual characteristics of the core and the shell materials. The functionality of the designed particles is strongly influenced by their surface roughness. Quantitative evaluation of the roughness of CS microparticles is, however, a challenging task for Scanning Electron Microscopy (SEM).&#13;
The SEM images contain two-dimensional (2D) information providing contour roughness data only from the projection of the particle in the horizontal plane. This study presents a practical procedure to achieve more information by tilting the sample holder, hence allowing images of different areas of a single particle to be recorded at different orientations under the same view angle. From the analysis of these images, quasi three-dimensional (3D) information is obtained.&#13;
Three types of home-made particles were investigated: i) bare polystyrene (PS) particles, ii) PS particles decorated with a first magnetic iron oxide (Fe3O4) nanoparticle shell forming CS microbeads, iii) PS/Fe3O4 particles closed with a second silica (SiO2) shell forming core-shell-shell (CSS) microbeads. A series images of a single particle were taken with stepwise tilted sample holder up to 10° by an SEM with high-resolution and surface sensitive SE-InLens® mode.&#13;
A reliable analysis tool has been developed by a script in Python to analyze SEM images automatically and to evaluate profile roughness quantitatively, for individual core-shell microparticles. Image analysis consists of segmentation of the images, identifying contour and the centre of the particle, and extracting the root mean squared roughness value (RMS-RQ) of the contour profile from the particle projection within a few seconds.&#13;
The variation in roughness from batch-to-batch was determined with the purpose to set the method as a routine quality check procedure. Flow cytometry measurements provided complementary data. Measurement uncertainties associated to various particle orientations were also estimated.</abstract>
    <enrichment key="eventName">ICASS 5th International Conference on Applied Surface Science</enrichment>
    <enrichment key="eventPlace">Palma, Mallorca, Spain</enrichment>
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    <author>Deniz Hülagü</author>
    <author>Charlie Tobias</author>
    <author>Ardian B. Gojani</author>
    <author>Knut Rurack</author>
    <author>Vasile-Dan Hodoroaba</author>
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      <value>Core-shell particles</value>
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      <value>Image analysis</value>
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    <subject>
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      <value>Roughness</value>
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    <subject>
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    <title language="eng">Dataset accompanying the publication "Towards 3D determination of the surface roughness of core-shell microparticles as a routine quality control procedure by scanning electron microscopy"</title>
    <abstract language="eng">This dataset accompanies the following publication:&#13;
&#13;
Hülagü, D., Tobias, C., Dao, R., Komarov, P., Rurack, K., Hodoroaba, V.-D., Towards 3D determination of the surface roughness of core-shell microparticles as a routine quality control procedure by scanning electron microscopy. Sci.Rep, 14, 17936 (2024), https://doi.org/10.1038/s41598-024-68797-7.&#13;
&#13;
It contains SEM and AFM-in-SEM images of polystyrene (PS) core particles, polystyrene-iron oxide (PS/Fe3O4) core-shell particles, and polystyrene-iron oxide-silica (PS/Fe3O4/SiO2) core-shell-shell particles. Please refer to the publication and its supporting information for more details on the acquisition and contents of the dataset, as well as the GitHub repository at https://github.Com/denizhulagu/roughness-analysis-by-electron-microscopy.&#13;
&#13;
 &#13;
&#13;
The investigated particles were produced at BAM laboratories as previously described in:&#13;
&#13;
Hülagü, D. et al. Generalized analysis approach of the profile roughness by electron microscopy with the example of hierarchically grown polystyrene–iron oxide–silica core–shell–shell particles. Adv. Eng. Mater. 24, 2101344, https://doi.org/10.1002/adem.202101344 (2022).&#13;
&#13;
Tobias, C., Climent, E., Gawlitza, K. &amp; Rurack, K. Polystyrene microparticles with convergently grown mesoporous silica shells as a promising tool for multiplexed bioanalytical assays. ACS Appl. Mater. Interfaces 13, 207, https://dx.doi.org/10.1021/acsami.0c17940 (2020).</abstract>
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    <licence>Creative Commons - CC BY - Namensnennung 4.0 International</licence>
    <author>Deniz Hülagü</author>
    <author>Charlie Tobias</author>
    <author>R. Dao</author>
    <author>P. Komarow</author>
    <author>Knut Rurack</author>
    <author>Vasile-Dan Hodoroaba</author>
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      <value>Core–shell particles</value>
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      <language>eng</language>
      <type>uncontrolled</type>
      <value>Image analysis</value>
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    <subject>
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      <value>Roughness</value>
    </subject>
    <subject>
      <language>eng</language>
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      <value>Scanning electron microscopy</value>
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    <subject>
      <language>eng</language>
      <type>uncontrolled</type>
      <value>Atomic force microscopy</value>
    </subject>
    <subject>
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      <value>Tilting</value>
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      <type>uncontrolled</type>
      <value>Batch analysis</value>
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    <collection role="unnumberedseries" number="">Forschungsdatensätze der BAM</collection>
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    <title language="eng">Luminescence Lifetime-Based Sensing Platform Based on Cyclometalated Iridium(III) Complexes for the Detection of Perfluorooctanoic Acid in Aqueous Samples</title>
    <abstract language="eng">Luminescence lifetimes are an attractive analytical method for detection due to its high sensitivity and stability. Iridium probes exhibit luminescence with long excited-state lifetimes, which are sensitive to the local environment. Perfluorooctanoic acid (PFOA) is listed as a chemical of high concern regarding its toxicity and is classified as a “forever chemical”. In addition to strict limits on the presence of PFOA in drinking water, environmental contamination from industrial effluent or chemical spills requires rapid, simple, accurate, and cost-effective analysis in order to aid containment. Herein, we report the fabrication and function of a novel and facile luminescence sensor for PFOA based on iridium modified on gold surfaces. These surfaces were modified with lipophilic iridium complexes bearing alkyl chains, namely, IrC6 and IrC12, and Zonyl-FSA surfactant. Upon addition of PFOA, the modified surfaces IrC6-FSA@Au and IrC12-FSA @Au show the largest change in the red luminescence signal with changes in the luminescence lifetime that allow monitoring of PFOA concentrations in aqueous solutions. The platform was tested for the measurement of PFOA in aqueous samples spiked with known concentrations of PFOA and demonstrated the capacity to determine PFOA at concentrations &gt;100 μg/L (240 nM).</abstract>
    <parentTitle language="eng">Analytical Chemistry</parentTitle>
    <identifier type="url">https://pubs.acs.org/doi/10.1021/acs.analchem.3c04289</identifier>
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    <title language="eng">Generalized Analysis Approach of the Profile Roughness by Electron Microscopy with the Example of Hierarchically Grown Polystyrene–Iron Oxide–Silica Core–Shell–Shell Particles</title>
    <abstract language="eng">The roughness as a property of core–shell (CS) microparticles plays a key role in their functionality. Quantitative evaluation of the roughness of CS microparticles is, however, a challenging task with approaches using electron microscopy images being scarce and showing pronounced differences in terms of methodology and results. This work presents a generalized method for the reliable roughness determination of nonplanar specimens such as CS particles from electron microscopic images, the method being robust and reproducible with a high accuracy. It involves a self-written software package (Python) that analyzes the recorded images, extracts corresponding data, and calculates the roughness based on the deviation of the identified contour. Images of single particles are taken by a dual mode scanning electron microscopy (SEM) setup which permits imaging of the same field-of-view of the sample with high resolution and surface sensitive in SE InLens mode as well as in transmission mode (TSEM). Herein, a new type of polystyrene core–iron oxide shell–silica shell particles is developed to serve as a set of lower micrometer-sized study objects with different surface roughness; the analysis of their images by the semiautomatic workflow is demonstrating that the particles’ profile roughness can be quantitatively obtained.</abstract>
    <parentTitle language="eng">Advanced Engineering Materials</parentTitle>
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    <author>Vasile-Dan Hodoroaba</author>
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      <value>Roughness</value>
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    <title language="eng">From 2D and Single Particle to 3D and Batch Analysis as a Routine Quality Check Procedure for the Morphological Characterization of Core-Shell Microparticles</title>
    <abstract language="eng">CS particles show unique properties by merging individual characteristics of the core and the shell materials. An alteration particularly in their surface roughness affects the final performance of the particles in the targeted application. Quantitative evaluation of the roughness of CS microparticles is, however, a challenging task employing microscopic techniques being scarce and showing large differences in terms of methodology and results.&#13;
In our previous work, we have reported a systematic study with a reliable analysis tool, which evaluates profile roughness quantitatively, for individual core-shell microparticles using electron microscopy (EM) images of both types, Scanning Electron Microscopy (SEM) and transmission mode SEM (or TSEM). The SEM images contain two-dimensional (2D) information, therefore, provide profile roughness data only from the projection in the horizontal plane (in other words, from the “belly”) of a spherical particle. The present study offers a practical procedure to give access to more information by tilting the sample holder and hence allowing images of a single particle to be recorded at different orientations under the same view angle. From the analysis of these images, extended information on surface roughness of the particle can be extracted. Thus, instead of obtaining 2D information from a single SEM image, three-dimensional (3D) information is obtained from 2D projections recorded at different particle orientations.</abstract>
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      <value>Tilting</value>
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    <title language="eng">Analysis of the profile roughness of core-shell microparticles by electron microscopy</title>
    <abstract language="eng">A particle roughness analysis tool, based on electron microscopy images (SEM and TEM). The influence of various parameters on the calculated roughness was also investigated: the setting of the proper threshold, accelerating voltage, etc. The samples were gradually tilted to extend imaging information of more than only one projection. Furthermore, the measurement uncertainty of the profile roughness of particles associated to various orientations was estimated.</abstract>
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    <collection role="themenfelder" number="">Umwelt</collection>
    <collection role="themenfelder" number="">Chemie und Prozesstechnik</collection>
    <collection role="literaturgattung" number="">Verlagsliteratur</collection>
    <collection role="fulltextaccess" number="">Datei im Netzwerk der BAM verfügbar ("Closed Access")</collection>
    <collection role="themenfelder" number="">Sensorik</collection>
  </doc>
</export-example>
