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Micro-/nanostructure diagnostics

Studies on the basic characterization of materials with respect to the structure (materialography/image analysis), the chemical composition in the micro range (SEM/EPMA/EBSD), and the crystal structure (XRD) are a scientific and technical service offered by IEK-1.

Nanostrukturdiagnostik: Methodenkomplex für die Mikro-/Nanostrukturdiagnostik von Werkstoffen

  • Implementation of studies on the basic characterization of materials with respect to their structure, their chemical composition in the micro range, and their crystal structure as a scientific and technical service
  • Evaluation of the characterization findings together with the problem-oriented working groups
  • Advice on the diagnostic methods available at the institute and through cooperation, as well as on the optimal use of these methods for obtaining the required data from samples, components, and materials

Services

Nanostrukturdiagnostik: Microanalysis

The "Micro-/Nanostructure Diagnostics" working group performs basic characterization of the structure of materials in the set of methods.

By means of the close cooperation of the employees in the materialography, SEM & EPMA, and X-ray diffractometry labs, the research objects are observed from a number of different "sides", rather than just one.

Nanostrukturdiagnostik: Chema

This methodological spectrum is supplemented by the materials science expertise in the institute's research disciplines.

State-of-the-art equipment and practitioners with experience in the range of methods serve as the basis for deriving reliable characterization findings of the material under investigation on a micrometre and submicrometre scale.

Special experience

  • Preparation of composites with microstructural components with a wide range of hardness levels (cross/oblique sections, microstructural development)

    Nanostrukturdiagnostik: Y3Al5O12-belegte Korngrenzen

    Nanostrukturdiagnostik: Hochauflösungsabbildung im REM bei sehr niedriger Beschleunigungsspannung


  • Figure: High-resolution image in SEM at very low accelerating voltage
  • Microanalysis: Locally resolved, quantitative determination of light elements (oxides, carbides, nitrides, borides), detection of elements at low concentration levels and elemental analysis with lateral resolution < 1 µm.
  • In situ heating, tension, and bending experiments in the scanning electron microscope
  • Qualitative/quantitative X-ray phase analysis on polycrystalline materials (powders, compact samples, components)
  • In situ X-ray diffraction at low and high temperatures (80...1700 K) in various atmospheres (evaluation using the Rietveld method)
  • Locally resolved determination of residual stresses in layers and surface-near area (macro stress mapping)

    Nanostrukturdiagnostik:X-Ray Powder Diffraction

Materialography, ceramography, and image analysis

Mikro-/Nanostrukturdiagnostik: Materialografie, Keramografie & Bildanalyse

Services and competence

  • Sampling and formulation (cutting, grinding)
  • Protection of thin reaction/surface layers (additional coatings)
  • Embedding (cold/hot mounting, vacuum impregnation)
  • Preparation of cross-sections (perpendicular/inclined, grinding, lapping, polishing)
  • Development of microstructure by chemical, eletrolytical, and thermal etching
  • Contrasting by interference coatings
  • Development of microstructure with optical microscopy (bright/dark field, polarization/interference/differential interference contrast) and scanning electron microscope
  • Digital photography and image archiving with intranet access
  • Quantitative image analysis (grain size, grain size distribution, porosity, thickness of coatings, etc.)
  • Hardness texts (Vickers: macro-, meso-, and microhardness)

Equipment and specialized software

  • Cutting machines
    Buehler "PowerMet" (dmax = 140 mm), Presi "Mecatome T255/300" metallurgical cut-off saw up to 75 mm depth of cut for rough pre-assembly, ATM "Brilliant 221" precision cut-off machine with max. cutting capacity of up to 50 mm in diameter, Mutronic "Diadisc 4500" manual table-top saw for precision cutting work and Sommer "2400" diamond wire saw (wire thickness 0.3 mm) for precision cutting of sensitive materials
  • Grinding and polishing machines
    3 ATM "Saphir 550 programmable grinding and polishing stations, 12 Buehler "Minimet 1000" polishing stations for single samples with planetary-type motion and "Caloprep" station for grinding of cup-shaped profiles.
  • Coating equipment
    Balzers SCD40 sputter deposition device for Au, Pt and Pt-Ir films as a substrate for electroless Ni coatings
  • Microhardness
    Leitz "Miniload" low-load Vickers hardness tester (5 p to 2000 p) with digital evaluation of indentation
  • Optical microscopes
    Olympus "PMG3", Leitz "Metalloplan", Olympus "SZX 12" stereo microscope
  • Scanning electron microscope
    FEI "Phenom" with various sample holders
  • Digital cameras
    DP25 (up to 2560 pixels x 1920 pixels), ProgRes C10plus (up to 2080 pixels x 1542 pixels), ColorView II (up to 2048 pixels x 1436 pixels)
  • Specialized software
    Software for image acquisition and archiving "Stream Motion"
    Software for image acquisition and database storage "analySIS FIVE" (licence level Docu)
    Image analysis software "analySIS FIVE" (licence level Pro)
    Image analysis software "Omnimet Enterprise 8.5"

Scanning electron microscopy and electron probe microanalysis (SEM & EPMA)

Mikro-/Nanostrukturdiagnostik: Rasterelektronenmikroskopie und Elektronenstrahl-Mikroanalyse (REM & ESMA)

Services and competence

  • Imaging of surfaces and microstructural features at high local resolution with topography and material contrast (E0 = 0.3 ... 30 keV, magnification 20 ... 500,000 x)
  • Qual./quant. microanalysis (point, line, area) using semiconducting Si(Li) detectors (EDX) and/or crystal spectrometer (WDX)
  • Determination of grain orientation, crystal orientation mapping by means of electron backscatter diffraction (EBSD)
  • Imaging of ceramics and minerals using the cathodoluminescence signal (CL, panchromatic)
  • In situ deformation experiments: Tensile test up to approx. 600 °C, 3-/4-point bending in upper view or side view geometry
  • In situ heating experiments up to approx. 700 °C at 10-5 mbar
  • Documentation of results as data files with direct intranet access

Equipment and specialized software

  • Equipment for sample preparation
    Carbon evaporation devices CED020 (carbon cord evaporator) and Polaron E5050 (cord/rod evaporator, rotating/swinging specimen table)
    Sputter coater SCD050 (Au, Pt, Cu, quartz oscillator for thickness control)
    Universal coater MED 020 (turbo pump, Cr. Ni, Pt, Au, Cu, and C, quartz oscillator for thickness control, rotating specimen table)
  • Analytical scanning electron microscopes
    Zeiss "Ultra55" (FEG-HV ultra-high resolution microscope) with DC/enhancedIL/InLensSE/Robinson-SE/diode-SE/CL detectors and Si(Li) X-ray detector, motorized Cartesian 5-axis specimen stage
    FEI "Phenom" (simple table-top device with CeB6 cathode without EDX spectrometer for imaging with a magnification range of 200–20000 x at 5 kV, sample chamber prevacuum)
  • Specialized software
    Controller software SmartSEM for digitized scanning microscopes made by Carl Zeiss NTS GmbH
    INCAEnergy400, INCAWave, nad INCACrystal for X-ray spectral analysis and microdiffraction
    MTools 3.2 and IDFix 3.0 for quantification of X-ray emission spectra
    Image database "analySIS FIVE" (licence level docu)

X-ray diffractometry (XRD)

Services and competence

Mikro-/Nanostrukturdiagnostik: Röntgendiffraktometrie (XRD)

  • Qualitative/quantitative phase analysis of polycrystalline materials (deconvolution of superimposed interference diagrams of complex phase mixtures, crystalline phases, and X-ray amorphous components)
  • Phase identification via search-match in ICDD database (PDF-2 Release 2010)
  • Determination and refinement of lattice parameters
  • Crystal structure refinement by means of Rietveld analysis
  • Determination of crystallite size and microstress
  • In situ X-ray diffraction at low and high temperatures (T = 80...1700 K) in various atmospheres (oxidizing, reducing, inert, vacuum up to 10-5 mbar)
  • Determination of (local) residual stresses at surfaces and in coatings/layers (sin2(Psi) method in W- and y geometry), stress mapping with approx. 1 mm2 local resolution
  • Determination of crystal orientation, texture analysis
  • Study of thin films and coatings
  • Documentation of results as data files with direct intranet access

Equipment and specialized software

  • Theta-2Theta diffractometer with 66 sample position magazine (Bruker AXS D4 ENDEAVOR)
    Rotatable specimen stage, automatic divergence and antiscatter slits, various slit diaphragms, axial Soller slits 2.5 ° and 4 °, automatic receiving slit changer, graphite monochromator, NaJ szintillation counter, 2 kW ceramic long fine-focus Cu tube
  • Multi-purpose Theta-Theta diffractometer for materials research (Bruker-AXS/D8 Advance Series 2)
    Horizontal rotating sample stage, X-ray mirror, polycapillary half-lens, automatic divergence and antiscatter slits, various slit and aperture plates, Soller slits 2.5 ° and 4 °, parallel plate collimators 0.12 ° and 0.18 °, energy-dispersive SolX detector, NaJ szintillation counter, ceramic 2 kW long fine-focus Cu tube
  • Multi-purpose diffractometer for materials research (Panalytical/X'Pert MRD)
    Open Eulerian cradle with four-axis stage, X-ray mirror, polycapillary half-lens, 4xGe(220) channel-cut monochromator, XXX, automatic slit plates, Soller slit 0.04 rad, parallel plate collimator 0.27 °, secondary monochromators, Cu/Cr ceramic tubes 2kW
  • Theta-2Theta diffractometer (Siemens/D5000)
    High-temperature chamber HDK S1 up to about 1500 °C, low-temperature chamber TTK10 down to about -180 °C, focusing secondary monochromator for Cu-K radiation, 2kW ceramic Cu tubes, automatic divergence and anti-scatter slits, linear position-sensitive detector
  • Specialized software
    Powder Diffraction File (PDF-2, Release 2010)
    Crystallography Open Database (COD, 89,715 calculated patterns in 01/2010)
    Inorganic Crystal Sturcture Database (ICSD, online)
    X'Pert Suite (Data Collector 2.0, HighScore Plus 3.0), StressPlus, Texture
    DiffracPlus Evaluation Package V14 (Eva, search/match, DQuant, ...)
    Diffrac AT 3.3B (Eva, profile, search/match)
    Total Pattern Analysis Solution software (Topas 4.2)

Non-public

The "Micro-/Nanostructure Diagnostics" working group provides an extensive bilingual website on Forschungzentrum Jülich's intranet. There you will find:

  • physical fundamentals and details about methods
  • technical parameters of our analytical facilities and the software we use
  • data file structure/formats of the digital results and organization of files
  • links to servers with the analytical results and useful freeware.

You can access this intranet website via the links in Internet Explorer at the bottom of the page.

This internal information and auxiliary material is only accessible inside the web space of the institutes IEK-1 and IEK-2. We kindly ask for your understanding with respect to this restricted access. In cases of legitimate interest, temporary access may be granted for our external customers upon request.


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