3D-EBSD an CrossBeam-Systemen

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Seeburg, Luzern, Switzerland 1. Carl Zeiss NTS 2.

1 FIB- Workshop July D-EBSD an CrossBeam-Systemen Ulrike Zeile 1, Ali Gholinia 2 and Frank Bauer 3 Arbeitskreis FIB SSOM DGM/DGE ASEM Hotel Seeburg, Luzern, Switzerland 1. Carl Zeiss NTS 2. Oxford Instruments HKL A/S 3. OXFORD Instruments GmbH NanoAnalysis - Wiesbaden Fbauer07/2008

2 Nordlys Camera mounted on Crossbeam 1540EsB

3 NordlysF 400 advantages for 3-D EBSD Fastest EBSD detector available Drift mitigation Time for EBSD mapping portion of 3-D acquisition minimized 3-D EBSD can take tens of hours to days EBSD mapping is a major portion of that time Currently, only available with Zenith (thus Zeiss)

electrons Lower diode: Mainly orientation contrast, large angle scattered electrons

4 EBSD-Phosphor screen with forescatter-detectors ED-Detector: element analysis SEM pole piece Sample: tilted by 70 to improve interference contrast of scattered electrons Lower diode: Mainly orientation contrast, large angle scattered electrons Phosphor screen: converting electrons to photons Lowest diode: orientation contrast

5 Column and detector arrangement XB1540EsB 3-D EBSD requires very small working distances (~5 mm). SE FIB SEM The Nordlys design, especially the tapered nose, is a BIG advantage here EBSD -> ideale for 3D- EBSD

Forescatter Detector (FSD) BSE / FSE imaging

6 Forescatter Detector (FSD) BSE / FSE imaging with up to 6 detectors First information on phases and/or grain orientation BSE Z-contrast for phase differentiation (upper detectors). FSE orientation contrast for grain size and /or stress and strain imaging ( lower detectors)

7 Scheme of 3D-EBSD analysis Single image Acquisition Multiple image Acquisition Material Characterization and Conditioning Image Acquisition Multiple Image Acquisition Pattern Recognition & Analysis Software Image alignment FIB and image alignment Electron optic FIB equipment for Cross sections Image: BSE, FSE or SE Motorized sample stage Sample alignment Axes x,y,r,z,z Sample FIBing Cut- and polishing EBSD Camera: Pattern Acquisition Microscope or X-beam and Analysis Hardware Polished Samples, Stubs or other kind of material

Sample mounting in SEM Image coordination system Y Beam R X Y Randle, (1992) Microtexture Determination Institute of Materials Stage coordination system Orientation depends

8 Sample mounting in SEM Image coordination system Y Beam R X Y Randle, (1992) Microtexture Determination Institute of Materials Stage coordination system Orientation depends on the definition of cartesian coordination system (CS) relative precision better than 1 absolute precision depends on correlation between sample CS and stage CS (>2 ) R Z X

9 3D EBSD steps to go 1. Data acquisition and FIB control with the HKL Fast Acquisition Software 2. Data evaluation with HKL 3D-Viewer

10 Fast Acquisition : Data Collection easy control with Fast-Acquisition-Software Automized EBSD- Mapping and FIBing during complete time of acquisition and pattern interpretation High speed EBSD- Mapping by NordlysF400 camera on-line drift correction for automatic alignment of slides during acquisition and/or interpretation

11 Fast Acquisition : Data Collection No limitation in number of cuttings, of course dependend on thickness and sample size ( more than 12o slides tested ) Continued measuring, e.g. after interrupted acquisition No limitation in detection volume ( recommended volume less than 8000µm 3 ). High spatial resolution with EBSD, FIB and Alignment (20nm in x, y and z).

12 flexible EBSD stage Schematic view of the 55 pre-tilt sample holder

13 Chamber view

14 Chamber view during process ESV3.avi

15 Chamber view FIB position EBSD position EBSD

16 CrossBeam 3D-EBSD at Work

17 Software - Dialogue and Evaluation Carl-Zeiss (API) FIB SmartSEM OI-HKL (UIF) EBSD Acquisition Fast Acquisition OI-HKL (UIF) EBSD Post-Processing 3D Viewer Results

18 3D Viewer : Data processing and presentation Combining and cropping data of all individual slides Refinement and adjustment of layer positions ( Alignment ) Data presentation and export for individual grains

19 3D Viewer : Data processing and presentation 3D and free using 2D-planes in x,y and z with classical data presentations of EBSD-results and pole figures 3D noise reduction, based on voxels. 3D grain boundary reconstruction and visualization of grains. 3D orientation ellipsoidal sphere fitting on grains. 3D presentations and movies.

20 3D EBSD with Fast EBSD mapping Sample: Copper 51 layers 0.2µm resolution in X, Y and Z Number of voxels: 101x91x µm EBSD speed: 200^pic/s, 50 sec. per layer FIB speed: about 45 minutes per layer Total EBSD time: about 1 hour Total FIB time: about 38 hours Number of sessions/interupptions: 3

21 3D EBSD Data Presentation Note the blue grain in the next slide X Z Y Cross-sections in X, Y and Z planes Select and highlight a grain

22 Grain Boundary Analysis Z (2-11) (111) Y Y Coherent twin boundary Z

23 Grain Segmentation Data Region No. of Voxels Volume 1000x µm 3 Surface area µm 2 Mean Orientation, Euler angles, Mean Misorien -tation, Ellipsoid radii µm , 41.3, , 0.283, , 25.4, , 0.304, , 39.9, , 0.323, , 25.6, , 0.240, , 40.9, , 0.099, 0.054

24 Misorientation Data Regions Angle Axis X Axis Y Axis Z Direction Angle from <111> [1-1-1] [1-11] [-111] [1-11] 0.24 All misorientations are very close to 60 <111>

25 Dominant Axes Regions Dom. Axis X Dom. Axis Y Dom. Axis Z The table shows the direction of the boundary plane normal with respect to the sample coordinate system When converted to the crystal coordinate system, these are near to <111>. Therefore the boundary plane is near to {111}.

26 Fast Acquisition Program Pt - Draht

27 Data acquisition HKL Fast Acquisition Interface Pt-wire FIBcontrol

28 Data processing HKL 3D Viewer Pt-Wire IPF & Segments

29 Cropped Sections of Ti-Sample

30 Data processing HKL 3D Viewer individual grains Pt-pole figure of grain #1991

31 3D-View single grain

32 Conclusion 3D EBSD is a universal extensive tool for: 3D measurements for complete description of all grain / inclusion / particle form factors 3D characterization of grain boundaries 3D Analysis of micro texturs Vicinity effects of grains due to deformation or recrystallization Nucleation on recrystallization or phase transformation Epitaxy on CVD, PvD, LPE, etc. close to final end...

33 Possible limitations? Costs (SEM-FIB cross beam with 3D-EBSD Analysis) Practical limitations (time consuming analysis, analysis volumina, Isolators, material degradation from ions (FIB ), etc...) System stability over a long time period ( hours, days,...) Destructive method Huge data sets (3 dimensional data), for example 56MB for Pt-wire (42Schnitte)

EBSD Electron BackScatter Diffraction Principle and Applications

$EBSD Electron BackScatter Diffraction Principle and Applications$ EBSD Electron BackScatter Diffraction Principle and Applications Dr. Emmanuelle Boehm-Courjault EPFL STI IMX Laboratoire de Simulation des Matériaux LSMX emmanuelle.boehm@epfl.ch 1 Outline! Introduction!