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Single and multilayer polymer materials

Multilayer system with alternating layers of polymer with and without Fe2O3 particles (mass fractions from µg/g to wt%.

Systems of stacked thin layers of different materials with dimensions in the µm range as well as polymer multilayer systems are applied in many different fields, e.g. on tools to protect from corrosion, as dielectric layers in capacitors, as packaging films for food or as membranes in biosensors. Applications are also common in microelectronics and automotive industry, for example as car paints. In all cases mechanical, electrical, magnetic and/or optical properties are influence by the thickness of the individual layers in the stacked system, and by concentration and homogeneity of incorporated substances, which has to be proofed by suitable methods.

For this analytical methods are needed which produce the desired information after minimal sample preparation and without or with minimal sample destruction. In addition high lateral or 3D resolution is required to characterize layered systems properly in dependence on position or depth. Methods, like 3D µ-XRF, 3D µ-XANES, SIMS and LA-ICP-MS are beth choices to complete these requests. Nevertheless, proper calibration of composition and structure of layered materials is only possible by using appropriate reference materials, which are adapted to sample properties, like main matrix components, density, layer thicknesses and composition, and sometimes even species of the analytes. In most cases such materials are not commercially available and have to be synthesized. The availability of suited reference samples is especially important when new analytical methods and techniques are developed and quantification strategies are established.

In this context we develop and characterize layered polymer materials as in-house reference materials in which inorganic filler materials (compounds from Li ti U) are incorporated, if desired also with varying oxidation states, isotope ratios or as different species (e.g. Cu, Cu(I), Cu(II) or 204Pb enriched). Homogeneity of the analyte distribution, particle size and layer thickness are controlled carefully by several methods (µXRF, SEM, PIXE, ICP-OES, Microscopy, LA-ICP-MS).

The reference materials could afterwards applied to quantify trace element concentrations in biomineralization products and human, plant or animal tissue with high local resolution.

Determination of the beryllium concentration in a thin section of a plant root by application of Be-containing polymer standards. Left: Light microscopy image (200fold magnification), Center: Be-concentration in the root section, determined by LA-ICP-MS, right: calibration graph, obtained from 5 Be-containing reference samples with concentrations between 45 and 350 µg/g.

Publications

  • J. Thieleke, Beiträge zur Bestimmung von lokalen Verteilungen ausgewählter
  • toxischer Elemente ; Dissertation; Leibniz Universität Hannover, 2017
  • J. Thieleke, C. Vogt, Calibration stragtegy for LA-ICP-MS using isotope dilution for solid reference materials, JAAS 31 (2016) 1198 - 1205, DOI: 10.1039/C6JA00042H
  • G. Schwartze, Polymere Ein- und Mehrschichtmaterialien für die Kalibrierung moderner festkörperspektroskopischer Messsysteme; Dissertation; Leibniz Universität Hannover, 2013
  • L. Lühl, I. Mantouvalou, I. Schaumann, C. Vogt, B. Kanngießer, Three-Dimensional Chemical Mapping with a Confocal Setup, Anal. Chem. 85(7) (2013) 3682-3689
  • I. Schaumann, Herstellung und Charakterisierung von polymeren Schichtsystemen für die Validierung röntgenanalytischer Verfahren; Dissertation; Leibniz Universität Hannover, 2011
  • L. Lühl, I. Mantouvalou, W. Malzer, I. Schaumann, C. Vogt, O. Hahn, B. Kanngießer, Reconstruction procedure for 3D Micro X-ray Absorption Fine Structure, Anal. Chem. 2012, 84 (4), 1907–1914
  • I. Schaumann, W. Malzer, I. Mantouvalou, L. Lühl, B. Kanngiesser, Preparation and characterization of polymer layer systems for validation of 3D Micro X-ray fluorescence spectroscopy; Spectrochimica Acta Part B, 64, 334-340, 2009
  • I. Mantouvalou, W. Malzer, I. Schaumann, L. Lühl, R. Dargel, C. Vogt, B. Kanngiesser,  Reconstruction of thickness and composition of stratified materials by means of 3D micro X-ray fluorescence spectroscopy; Analytical Chemistry, 80, 819-826, 2008

Cooperations partners

  • Prof. Dr. Birgit Kanngießer, Institut für Optik und Atomare Physik, TU Berlin
    Dr. Burkhard Beckhoff, Physikalisch-Technische Bundesanstalt (PTB), Arbeitsgruppe 7.24, Röntgen- und IR-Spektrometrie, Berlin
  • Dr. U. Resch-Genger, BAM Berlin
  • ION-TOF GmbH, Münster