TY - JOUR A1 - Reed, B.P. A1 - Radnik, Jörg A1 - Shard, A.G. T1 - Ionic liquid [PMIM]+[NTf2]− (Solarpur®) characterized by XPS JF - Surface Science Spectra N2 - X-ray photoelectron spectroscopy (XPS) was performed on the meniscus of a droplet of ionic liquid 1-propyl-3-methyl-imidazolium bis(trifluoromethylsulfonyl) imide [PMIM]+[NTf2]− (Solarpur®) in ultrahigh vacuum. High-resolution spectra of F 1s, O 1s, N 1s, C 1s, and S 2p are presented along with a survey spectrum and the valence band structure. The spectra presented here were generated using monochromatic Al Kα radiation (1486.6 eV). KW - Ionic liquid KW - 1-propyl-3-methyl-imidazolium bis(trifluoromethylsulfonyl)imide KW - X-ray Photoelectron Spectroscopy PY - 2022 DO - https://doi.org/10.1116/6.0001518 VL - 29 IS - 1 SP - 014001-1 PB - AVS AN - OPUS4-54335 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cant, D. J. H. A1 - Müller, Anja A1 - Clifford, C. A. A1 - Unger, Wolfgang A1 - Shard, A. G. T1 - Summary of ISO/TC 201 Technical Report 23173—Surface chemical analysis—Electron spectroscopies—Measurement of the thickness and composition of nanoparticle coatings JF - Surface and Interface Analysis N2 - ISO Technical Report 23173 describes methods by which electron spectroscopies, including X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES) and synchrotron techniques, can be employed to calculate the Coating thicknesses and compositions of nanoparticles. The document has been developed to review and outline the current state-of-the-art for such measurements. Such analyses of core–shell nanoparticles are common within the literature, however the methods employed are varied; the relative advantages and disadvantages of These methods, and the optimal usage of each may not be clear to the general analyst. ISO Technical Report 23173 aims to clarify the methods that are available, describe them in clear terms, exhibit examples of their use, and highlight potential issues users may face. The information provided should allow analysts of electron spectroscopy data to make clear choices regarding the appropriate analysis of electron spectroscopy data from coated nanoparticle systems and provide a basis for understanding and comparing results from different methods and systems. KW - Electron spectroscopy KW - Core-shell KW - Nanoparticles KW - ISO 23173 KW - XPS KW - Thickness KW - Composition PY - 2021 DO - https://doi.org/10.1002/sia.6987 SN - 0142-2421 VL - 53 IS - 10 SP - 893 EP - 899 PB - John Wiley & Sons Ltd AN - OPUS4-52976 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dietrich, Paul A1 - Horlacher, T. A1 - Gross, Thomas A1 - Wirth, Thomas A1 - Castelli, R. A1 - Shard, A.G. A1 - Alexander, M. A1 - Seeberger, P.H. A1 - Unger, Wolfgang T1 - Surface analytical characterization of carbohydrate microarrays JF - Surface and interface analysis N2 - Microarrays are a versatile platform for diagnostics and high-throughput analysis. Carbohydrate microarrays are valuable tools to investigate interactions with other molecules since many glycans are involved in fundamental biological processes. A combined X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (ToF-SIMS) surface analysis was used to investigate the basic steps in the production of carbohydrate microarrays. The preparation included coupling of a thiol-terminated mannoside to maleimide-functionalized glass surfaces derived from γ-aminopropyl silane (GAPS) slides. XPS results clearly demonstrate successful chemical modification in each fabrication step, and ToF-SIMS imaging revealed immobilized carbohydrates in the spotted regions of the final microarray. KW - Carbohydrates KW - Microarrays KW - XPS KW - ToF-SIMS KW - Nona-mannoside KW - Maleimide surfaces KW - Surface analysis PY - 2010 DO - https://doi.org/10.1002/sia.3255 SN - 0142-2421 SN - 1096-9918 VL - 42 SP - 1188 EP - 1192 PB - Wiley CY - Chichester AN - OPUS4-21500 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Belsey, N. A. A1 - Cant, D. J. H. A1 - Minelli, C. A1 - Araujo, J. R. A1 - Bock, B. A1 - Brüner, P. A1 - Castner, D. G. A1 - Ceccone, G. A1 - Counsell, J. D. P. A1 - Dietrich, Paul M. A1 - Engelhardt, M. H. A1 - Fearn, S. A1 - Galhardo, C. E. A1 - Kalbe, H. A1 - Kim, J. W. A1 - Lartundo-Rojas, L. A1 - Luftman, H. S. A1 - Nunney, T. S. A1 - Pseiner, J. A1 - Smith, E. F. A1 - Spampinato, V. A1 - Sturm, J. M. A1 - Thomas, A. G. A1 - Treacy, J. P. W. A1 - Veith, L. A1 - Wagstaffe, M. A1 - Wang, H. A1 - Wang, M. A1 - Wang, Y.-C. A1 - Werner, W. A1 - Yang, L. A1 - Shard, A. G. T1 - Versailles Project on Advanced Materials and Standards Interlaboratory Study on Measuring the Thickness and Chemistry of Nanoparticle Coatings Using XPS and LEIS JF - The Journal of Physical Chemistry C N2 - We report the results of a Versailles Project on Advanced Materials and Standards (VAMAS) interlaboratory study on the measurement of the shell thickness and chemistry of nanoparticle coatings. Peptide-coated gold particles were supplied to laboratories in two forms: a colloidal suspension in pure water and particles dried onto a silicon wafer. Participants prepared and analyzed these samples using either X-ray photoelectron spectroscopy (XPS) or low energy ion scattering (LEIS). Careful data analysis revealed some significant sources of discrepancy, particularly for XPS. Degradation during transportation, storage, or sample preparation resulted in a variability in thickness of 53%. The calculation method chosen by XPS participants contributed a variability of 67%. However, variability of 12% was achieved for the samples deposited using a single method and by choosing photoelectron peaks that were not adversely affected by instrumental transmission effects. The study identified a need for more consistency in instrumental transmission functions and relative sensitivity factors since this contributed a variability of 33%. The results from the LEIS participants were more consistent, with variability of less than 10% in thickness, and this is mostly due to a common method of data analysis. The calculation was performed using a model developed for uniform, flat films, and some participants employed a correction factor to account for the sample geometry, which appears warranted based upon a simulation of LEIS data from one of the participants and comparison to the XPS results. KW - VAMAS KW - Interlaboratory Study KW - Nanoparticle coating KW - XPS KW - LEIS KW - shell thicknss and chemistry PY - 2016 UR - http://pubs.acs.org/doi/pdf/10.1021/acs.jpcc.6b06713 DO - https://doi.org/10.1021/acs.jpcc.6b06713 IS - 120 SP - 24070 EP - 24079 PB - ACS Publications AN - OPUS4-38428 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cant, D. J. H. A1 - Minelli, C. A1 - Sparnacci, K. A1 - Müller, Anja A1 - Kalbe, H. A1 - Stoger-Pollach, M. A1 - Unger, Wolfgang A1 - Werner, W. S. M. A1 - Shard, A. G. T1 - Surface-Energy Control and Characterization of Nanoparticle Coatings JF - Journal of Physical Chemistry C N2 - Accurate and reproducible measurement of the structure and properties of high-value nanoparticles is extremely important for their commercialization. A significant proportion of engineered nanoparticle systems consist of some form of nominally core-shell structure, whether by design or unintentionally. Often, these do not form an ideal core-shell structure, with typical deviations including polydispersity of the core or shell, uneven or incomplete shells, noncentral cores, and others. Such systems may be created with or without intent, and in either case an understanding of the conditions for formation of such particles is desirable. Precise determination of the structure, composition, size, and shell thickness of such particles can prove challenging without the use of a suitable range of characterization techniques. Here, the authors present two such polymer core-shell nanoparticle systems, consisting of polytetrafluoroethylene cores coated with a range of thicknesses of either polymethylmethacrylate or polystyrene. By consideration of surface energy, it is shown that these particles are expected to possess distinctly differing coating structures, with the polystyrene coating being incomplete. A comprehensive characterization of these systems is demonstrated, using a selection of complementary techniques including scanning electron microscopy, scanning transmission electron microscopy, thermogravimetric analysis, dynamic light scattering, differential centrifugal sedimentation, and X-ray photoelectron spectroscopy. By combining the results provided by these techniques, it is possible to achieve superior characterization and understanding of the particle structure than could be obtained by considering results separately. KW - Nanoparticles KW - Core-shell KW - XPS KW - Size KW - Thickness KW - Damage PY - 2020 DO - https://doi.org/10.1021/acs.jpcc.0c02161 VL - 124 IS - 20 SP - 11200 EP - 11211 PB - ACS CY - Washington DC AN - OPUS4-50899 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Holzweber, Markus A1 - Shard, A.G. A1 - Jungnickel, H. A1 - Luch, A. A1 - Unger, Wolfgang T1 - Dual beam organic depth profiling using large argon cluster ion beams JF - Surface and interface analysis N2 - Argon cluster sputtering of an organic multilayer reference material consisting of two organic components, 4,4'-bis[N-(1-naphthyl-1-)-N-phenyl- amino]-biphenyl (NPB) and aluminium tris-(8-hydroxyquinolate) (Alq3), materials commonly used in organic light-emitting diodes industry, was carried out using time-of-flight SIMS in dual beam mode. The sample used in this study consists of a ~400-nm-thick NPB matrix with 3-nm marker layers of Alq3 at depth of ~50, 100, 200 and 300 nm. Argon cluster sputtering provides a constant sputter yield throughout the depth profiles, and the sputter yield volumes and depth resolution are presented for Ar-cluster sizes of 630, 820, 1000, 1250 and 1660 atoms at a kinetic energy of 2.5 keV. The effect of cluster size in this material and over this range is shown to be negligible. KW - SIMS KW - Organic depth profiling KW - Argon cluster KW - ToF-SIMS KW - Ar-GCIB KW - Secondary Ion Mass Spectrometry PY - 2014 DO - https://doi.org/10.1002/sia.5429 SN - 0142-2421 SN - 1096-9918 VL - 46 SP - 936 EP - 939 PB - Wiley CY - Chichester AN - OPUS4-32573 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sikora, A. A1 - Bartczak, D. A1 - Geißler, Daniel A1 - Kestens, V. A1 - Roebben, G. A1 - Ramaye, Y. A1 - Varga, Z. A1 - Palmai, M. A1 - Shard, A.G. A1 - Goenaga-Infante, H. A1 - Minelli, C. T1 - A systematic comparison of different techniques to determine the zeta potential of silica nanoparticles in biological medium JF - Analytical methods N2 - The surface charge density of nanoparticles plays an important role in the way they interact with biological systems. The ability to measure the surface charge density of nanoparticles in biological media is therefore of importance in understanding the magnitude of such interactions. There are a number of methods which may be used to assess surface charge density through the measurement of electrophoretic mobility. In order to better understand the comparability of these methods, the ζ-potential of silica nanoparticles in water, buffer and serum-based biological medium was measured by one ensemble and two particle-by-particle techniques: electrophoretic light scattering (ELS), tunable resistive pulse sensing (TRPS) and zeta particle tracking analysis (z-PTA). To allow the comparability of results from different techniques, test samples were prepared according to an established protocol, although some variations were necessary to meet specific instrument requirements. Here we compare, for the first time, measurement results from the different techniques and discuss how modifications related to parameters such as environmental pH, dilution factor and presence of biomolecules influence the charge measurements. PY - 2015 DO - https://doi.org/10.1039/C5AY02014J SN - 1759-9660 SN - 1759-9679 VL - 7 IS - 23 SP - 9835 EP - 9843 PB - RSC Publ. CY - Cambridge AN - OPUS4-34966 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Shard, A. G. A1 - Hodoroaba, Vasile-Dan A1 - Unger, Wolfgang ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A. G. T1 - Introduction T2 - Characterization of nanoparticles - Measurement processes for nanoparticles N2 - The purpose of this book is to provide a comprehensive collection of analytical methods that are commonly used to measure nanoparticles, providing information on one, or more, property of importance. The chapters provide up-to-date information and guidance on the use of these techniques, detailing the manner in which they may be reliably employed. Within this chapter, we detail the rationale and context of the whole book, which is driven by the observation of a low level of reproducibility in nanoparticle research. The aim of the book is to encourage awareness of both the strengths and weaknesses of the various methods used to measure nanoparticles and raise awareness of the range of methods that are available. The editors of the book have, for many years, been engaged in European projects and standardization activities concerned with nanoparticle analysis and have identified authors who are experts in the various methods included within the book. This has produced a book that can be used as a definitive guide to current best practice in nanoparticle measurement. KW - Nanoparticles KW - Size distribution KW - Shape KW - Chemistry KW - Coating KW - Concentration KW - Standards KW - Charge KW - Characterisation PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/B978-0-12-814182-3.00001-8 SP - 1 EP - 6 PB - Elsevier CY - Amsterdam AN - OPUS4-50166 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hodoroaba, Vasile-Dan A1 - Unger, Wolfgang A1 - Shard, A. G. ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A. G. T1 - Conclusions and perspectives T2 - Characterization of nanoparticles - Measurement processes for nanoparticles N2 - This chapter briefly summarizes the methods selected within this book for the characterization of nanoparticles with regard to commonly accessible properties: nanoparticle size and size distribution, shape, surface area, surface charge, aggregation state, structure, chemical composition, surface chemistry, and nanoparticle number concentration. Current progress of measurement and analysis, as far as possible according to standard operation procedures, has been the focus of this work. A number of new and less commonly used methods have not been covered, and we outline some of these in this chapter. Future challenges such as automated measurement and analysis, read-across approaches for the prediction of properties, knowledge of measurement uncertainties, the need for certified reference materials, and the necessity to complement measurements methods to obtain more reliable results are covered, and the unmet measurement requirements for real-world nanoparticles are described. KW - Physicochemical characterization KW - Standard operation procedures KW - Data correlation KW - Method development KW - Trends PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/B978-0-12-814182-3.00006-7 SP - 527 EP - 534 PB - Elsevier CY - Amsterdam AN - OPUS4-50167 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reed, B. P. A1 - Cant, D.J.H. A1 - Spencer, S.J. A1 - Carmona-Carmona, A. J. A1 - Bushell, A. A1 - Herrara-Gómez, A. A1 - Kurokawa, A. A1 - Thissen, A. A1 - Thomas, A.G. A1 - Britton, A.J. A1 - Bernasik, A. A1 - Fuchs, A. A1 - Baddorf, A.P. A1 - Bock, B. A1 - Thellacker, B. A1 - Cheng, B. A1 - Castner, D.G. A1 - Morgan, D.J. A1 - Valley, D. A1 - Willneff, E.A. A1 - Smith, E.P. A1 - Nolot, E. A1 - Xie, F. A1 - Zorn, G. A1 - Smith, G.C. A1 - Yasukufu, H. A1 - Fenton, J.L. A1 - Chen, J. A1 - Counsell, J.D.P. A1 - Radnik, Jörg A1 - Gaskell, K.J. A1 - Artyushkova, K. A1 - Yang, L. A1 - Zhang, L. A1 - Eguchi, M. A1 - Walker, M. A1 - Hajdyla, M. A1 - Marzec, M.M. A1 - Linford, M.R. A1 - Kubota, N. A1 - Cortazar-Martinez, O. A1 - Dietrich, P. A1 - Satoh, R. A1 - Schroeder, S.L.M. A1 - Avval, T.G. A1 - Nagatomi, T. A1 - Fernandez, V. A1 - Lake, W. A1 - Azuma, Y. A1 - Yoshikawa, Y. A1 - Compean-Gonzalez, C.L. A1 - Ceccone, G. A1 - Shard, A.G. T1 - ERRATUM: “Versailles project on advanced materials and standards interlaboratory study on intensity calibration for x-ray photoelectron spectroscopy instruments using low-density polyethylene” [J. Vac. Sci. Technol. A 38, 063208 (2020)] JF - Journal of Vacuum Science & Technology A N2 - The lead authors failed to name two collaborators as co-authors. The authors listed should include: Miss Claudia L. Compean-Gonzalez (ORCID: 0000-0002-2367-8450) and Dr. Giacomo Ceccone (ORCID: 0000-0003-4637-0771). These co-authors participated in VAMAS project A27, provided data that were analyzed and presented in this publication (and supporting information), and reviewed the manuscript before submission. KW - X-ray photoelectron spectroscopy KW - Transmission function KW - Low-density polyethylene PY - 2021 DO - https://doi.org/10.1116/6.0000907 VL - 39 IS - 2 SP - 027001 PB - American Vacuum Society AN - OPUS4-52380 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -