Carl Zeiss Crossbeam Introduction and Oil & Gas Applications Heiko Stegmann Application Specialist Crossbeam Carl Zeiss Microscopy GmbH 22.01.2014 Carl Zeiss Crossbeam Introduction and Oil & Gas Applications 1 Introduction to Crossbeam: Components 2 Introduction to Crossbeam: Examples 3 Crossbeam application in Oil & Gas Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 2 Introduction to Crossbeam Components of a Crossbeam High resolution imaging Nanoscale material shaping Nanoscale gas chemistry Highly extensible SEM ZEISS Crossbeam GIS FIB Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 3 Introduction to Crossbeam Components of a Crossbeam High resolution imaging Nanoscale material shaping Nanoscale gas chemistry Highly extensible SEM ZEISS Crossbeam GIS FIB Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 4 Introduction to Crossbeam GEMINI SEM column Chamber and Inlens SE detectors: Topographic and high resolution information Secondary electrons Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) Inlens Energy Selective Backscatter detector: Compositional contrast ZEISS GEMINI detection principle Backscattered electrons 22.01.2014 5 Introduction to Crossbeam Components of a Crossbeam High resolution imaging Nanoscale material shaping Nanoscale gas chemistry Highly extensible SEM ZEISS Crossbeam GIS FIB Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 6 Introduction to Crossbeam Liquid Metal Ion Source (LMIS) Gallium Ion Source Taylor cone From: US Patent 6531811B1 Form a Focused Ion Beam (FIB) Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) Driesel et al., MPI Halle, Germany, 1996. 22.01.2014 7 Introduction to Crossbeam Components of a Crossbeam High resolution imaging Nanoscale material shaping Nanoscale gas chemistry Highly extensible SEM ZEISS Crossbeam GIS FIB Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 8 Introduction to Crossbeam: High SEM resolution at low voltage Backscattered Electrons Stopped Electrons C +Os C 10nm C +Os C E = 10 keV High electron energies not suitable for high resolution imaging! C +Os C 10nm C +Os C E = 1.5 keV Escape depth for single scattered BSE < 5 nm In-lens detectors allow high resolution imaging at low voltage Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 9 Introduction to Crossbeam Components of a Crossbeam High resolution imaging Nanoscale material shaping Nanoscale gas chemistry Highly extensible SEM ZEISS Crossbeam GIS FIB Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 10 Introduction to Crossbeam Basic FIB operation modes FIB imaging SE and SI generation by I-beam FIB milling Sputtering of substrate atoms by I-beam Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) Chemical processes I-beam induced deposition Gas enhanced I-beam etching 23.01.2014 11 Introduction to Crossbeam Example: FIB imaging Visualisation of intergranular corrosion in a Ni based superalloy by secondary ion detection. Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 12 Introduction to Crossbeam Example: Nanopatterning • Nanometer precision material removal and deposition by FIB and Ebeam • Easy creation of arbitrary patterns • Full control of the whole patterning process (dwell times, pixel spacing, scan regime, etc.) • Resolution 65k x 65k Pixel AFM tip modification Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 13 Introduction to Crossbeam Example: Nanopatterning Movie FE-tips in Si Fresnel zone plate Pillar array in Si “NanObama” Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) Microfluidic device Photonic pattern 22.01.2014 14 Introduction to Crossbeam Components of a Crossbeam High resolution imaging Nanoscale material shaping Nanoscale gas chemistry Highly extensible SEM ZEISS Crossbeam GIS FIB Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 15 Introduction to Crossbeam Example: FIB deposition and gas enhanced etch Freestanding carbon coil. Pitch is a function of the dwell time. 200 nm thick free standing iridium wire on silicon FIB induced material deposition from precursor gases Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 16 Introduction to Crossbeam Components of a Crossbeam High resolution imaging Nanoscale material shaping Nanoscale gas chemistry Highly extensible SEM ZEISS Crossbeam GIS FIB Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 17 Introduction to Crossbeam Example: FIB milling X-sectioning for SEM imaging In-lens SE Chamber SE ZnTe CdS Au ZnTe CdS? CdTe ~2µm CdTe ZnTe? EsB CdS SnO2 ZnTe glass Nominal Layer Stack FIB cross-section of a CdTe thin film solar cell Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) Imgaging with different SEM detectors at 2 kV 22.01.2014 18 Introduction to Crossbeam Example: FIB milling with live SEM imaging FIB and SEM optics are completely independent! Observing the milling process with the SEM in real time Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 19 Introduction to Crossbeam Example: TEM sample preparation In-Situ Lift Out Sample after milling Micromanipulator tip is welded to lamella Lamella cut-out TEM Sample Lamella lift-out Lamella transfer to TEM grid and welding to grid by GIS metal deposition Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 20 Introduction to Crossbeam Example: Automatic TEM sample preparation H-bar type lamellas Lift-out type lamellas Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 21 Introduction to Crossbeam Tomography 1. Remove a slice of material with the focused ion beam 2. Acquire an SEM image 3. Repeat until the complete volume of interest is sectioned (automated) 1 µm Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 22 Introduction to Crossbeam Tomography y 1. Remove a slice of material with the focused ion beam 2. Acquire an SEM image 3. Repeat until the complete volume of interest is sectioned (automated) 4. Align images x SEM images Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 23 Introduction to Crossbeam Tomography Projection Rendering Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 1. Remove a slice of material with the focused ion beam 2. Acquire an SEM image 3. Repeat until the complete volume of interest is sectioned (automated) 4. Align images 5. Visualise volume and calculate geometrical properties 22.01.2014 24 Introduction to Crossbeam Tomography FIB/SEM fills the gap between TEM tomography and X-ray tomography (10 mm) 3 Large Large volume, volume, high resolution low resolution Volume of Material Analyzed (1 mm) 3 X-ray tomography/ microscopy (100 µm) 3 (10 µm) 3 FIB Tomography (1 µm) 3 Electron tomography (100 nm) 3 Small volume, high resolution 3D atom probe/LEAP (10 nm) 3 0.1 nm 1 nm 10 nm 100 nm 1 µm 10 µm 100 µm 1 mm Approximate Voxel Dimensions Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 23.01.2014 25 Introduction to Crossbeam: Typical tomography parameters Voxel size can be easily adapted to resolution requirements. Typically below 50 nm. Below 5 nm possible by imaging with low-loss, low-kV BS electrons. Volume 5 to 30 µm3 Image dimensions and data size (8-bit grey level tiff): 1024 x 786: 800 slices -> 640 MB 2048 x 1572: 1600 slices -> 5 GB 3096 x 2358: 3000 slices -> 21 GB Goal: Isotropic voxel size dx = dy = dz SEM 1-2 kV, dwell time 5-10µsec/pixel -> high S/N ratio FIB 30 kV, 0.5-1.5nA Acquisition time ≈ 1min/slice (40-60 slices/hour) Completely automated acquisition of data cube (several hours). Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 23.01.2014 26 Introduction to Crossbeam Tomography examples Cement Shale Rock Retina tissue Rat brain Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) Courtesy of Marco Cantoni, EPFL Lausanne 22.01.2014 27 Introduction to Crossbeam Tomography with ATLAS 3D Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 28 Introduction to Crossbeam Components of a Crossbeam High resolution imaging Nanoscale material shaping Nanoscale material deposition Highly extensible SEM ZEISS Crossbeam GIS FIB Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 29 Introduction to Crossbeam Components of a Crossbeam High resolution imaging Nanoscale material shaping Nanoscale material deposition Highly extensible (BSE, SE, SI and STEM detectors, EDS, WDS, EBSD, CL, SIMS, flood gun, micromanipulators, cryo, SEM electrical test equipment, …) ZEISS Crossbeam GIS FIB Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 30 Introduction to Crossbeam Example: Gun shot residual analysis Identification of gun shot residual origin by combination of FIB, EBSD and EDX analysis. Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 31 Introduction to Crossbeam Example: 3D EDS elemental analysis Lead free solder Ag(SnO2, In2O3) Quantitative 3D silver L-series map Zn , In and O 3D map Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 32 Introduction to Crossbeam Example: 3D EBSD crystalline structure analysis Simultaneous 3D EBSD and EDS analytics Slice 1 (0 µm) Slice 6 (0.5 µm) Slice 11 (1.0 µm) Slice 16 (1.5 µm) 3D microstructur al information Slice 21 (2.0 µm) 3D chemical information Sample: Friction steer welded Al Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 33 Introduction to Crossbeam Laser option for extremely fast material removal Method Scanner head Laser Coupling tube Process chamber FIB High current FIB FIB combined with GIS Plasma ion source FIB Milling rate Time needed to remove of silicon 0.3 mm3 [µm3/s] 2.7 3.5 years 30 116 days 250 14 days 2 000 1.7 days 355-nm 1 000 000 DPSS laser Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 5 minutes 22.01.2014 34 Introduction to Crossbeam Example: Laser applications Flip chip Laser micromachining Electric drive power module 1 mm Mobile display Lacquered sheet steel Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 35 Crossbeam application in Oil & Gas Correlating images with SmartBrowse Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 36 Crossbeam application in Oil & Gas Large area high resolution imaging with ATLAS Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 37 Crossbeam application in Oil & Gas Large area high resolution imaging Conventional: Small tile acquisition and stitching → many stage movements, large overlap areas. Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) ZEISS ATLAS: Tile size and overlap optimized → Less acquisition time → Higher sample throughput. 22.01.2014 38 Crossbeam application in Oil & Gas Large area high resolution imaging Conventional: Small tile acquisition and stitching → many stage movements, large overlap areas. Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) ZEISS ATLAS: Image only selected ROIs → Even less acquisition time! → Even higher sample throughput! 22.01.2014 39 Crossbeam application in Oil & Gas Laser sample preparation Shale rock cut Shale rock micropillars for XRM Sandstone micropillar Noses for Crossbeam tomography Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 40 Crossbeam application in Oil & Gas Tomography of shale rock Volume 12x10x12 µm3 Voxel size 15x15x30 nm3 405 slices Acquisition time 3:15 h Coarse cuts and Pt deposition Top view before and after tomography series acqusition Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 41 Crossbeam application in Oil & Gas Tomography of shale rock EsB detector SESI detector Raw image series After translational alignment Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 42 Crossbeam application in Oil & Gas Tomography of shale rock Virtual sectioning of the data cube XY Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) YZ XZ 22.01.2014 43 Crossbeam application in Oil & Gas: Tomography of shale rock Edit LUT Data processing: for pore segmentation from two detector signals Auto Local Threshold (Sauvola algorithm) EsB detector Auto Local Threshold (Sauvola algorithm) Invert, Min, Remove Outliers SESI detector Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 23.01.2014 44 Crossbeam application in Oil & Gas Tomography of shale rock Segmentation → Pore connectivity (pores of same colour are connected) Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 Volume (µm^3) Surface (µm^2) Nb of obj. voxels 3.38E-06 0.001 1 1.86E-04 0.048 55 6.75E-06 0.002 2 0.068 5.045 20171 3.38E-06 0.001 1 30.443 878.279 9020262 1.76E-04 0.028 52 6.14E-04 0.102 182 6.08E-05 0.013 18 4.39E-05 0.01 13 3.98E-04 0.068 118 2.03E-05 0.005 6 0.02 2.021 5960 1.15E-04 0.022 34 2.13E-04 0.037 63 0.004 0.252 1268 0.041 2.073 12106 6.31E-04 0.112 187 3.85E-04 0.068 114 0.004 0.28 1095 3.38E-06 0.001 1 2.03E-05 0.005 6 1.35E-05 0.004 4 2.90E-04 0.05 86 4.05E-04 0.057 120 9.79E-05 0.019 29 7.76E-05 0.016 23 5.81E-04 0.089 172 1.11E-04 0.028 33 8.78E-05 0.018 26 4.15E-04 0.072 123 8.44E-05 0.015 25 4.39E-05 0.009 13 0.011 15 5.06E-05 4.05E-05 0.009 12 2.36E-05 0.006 7 2.03E-05 0.005 6 2.70E-05 0.007 8 1.01E-04 0.019 30 4.32E-04 0.071 128 3.38E-05 0.009 10 3.38E-06 0.001 1 2.57E-04 0.04 76 2.36E-04 0.044 70 1.11E-04 0.021 33 7.76E-05 0.016 23 3.75E-04 0.071 111 5.74E-05 0.012 17 0.002 0.332 717 0.004 0.42 1196 1.69E-05 0.005 5 6.75E-06 0.002 2 4.05E-05 0.01 12 4.05E-05 0.011 12 2.70E-04 0.047 80 3.04E-05 0.007 9 5.74E-05 0.013 17 3.11E-04 0.07 92 6.75E-06 0.002 2 7.76E-05 0.015 23 2.70E-04 0.046 80 → Pore statistics 22.01.2014 45 Crossbeam application in Oil & Gas Pore space segmentation in shale rock Simple greyvalue thresholding segmentation leads to artifacts. Empty pores Filled pores Empty and filled pores cannot be clearly separated in the BSE image alone. Chamber SE2 detector Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 46 Crossbeam application in Oil & Gas Pore space segmentation in shale rock Simple greyvalue thresholding segmentation leads to artifacts. Empty pores Filled pores Empty and filled pores cannot be clearly separated in the SE image alone. Inlens EsB detector Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 47 Crossbeam application in Oil & Gas Pore space segmentation in shale rock Empty pores from combined SE+BSE image Filled pores from combined SE+BSE image Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) Precise separation of filled and empty pores by combination of SE and BSE images 22.01.2014 48 Crossbeam application in Oil & Gas Tomography of shale rock 3D imaging of pores in organic matter One slice from the EsB image stack. Organic regions can be identified by their grey value. One slice from the SE image stack. Nanometer sized pores can be clearly identified. Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 49 Crossbeam application in Oil & Gas Tomography of shale rock Volume: 5.7 x 3.7 x 3.9 µm3 Voxel size 3 x 3 x 5 nm3 770 slices Acquisition time 10 h Segmentation calculated by combining the BSE and SE data. Gold: Organic fraction Blue: Pores Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) Surface [µm2] Volume [µm3] Total 114.06 80.03 Organic 85.90 2.82 3.5 Pores 50.14 2.93 3.7 Volume fraction [%] 22.01.2014 50 Carl Zeiss Microscopy GmbH, Dr. Heiko Stegmann, Training, Application and Support Center (TASC) 22.01.2014 51
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