A Three-Dimensional Field Study of Solute Transport Through Unsaturated, Layered, Porous
3-dimensional microstructure characterization of porous ...
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> 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
3-dimensional microstructure characterization of porous ceramic matrix composites by X-ray tomography and FIB-slicing as database for numerical modelling
M. Bartsch, K. Artzt, M. Eggeler, P. Watermeyer German Aerospace Center, Cologne
A. Manero
Mechanical and Aerospace Engineering, University of Central Florida, Orlando, Florida
P. Kenesei Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois
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Research Goals
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- Visualization of 3d meso- and microstructure of fiber reinforced porous all-oxide CMC’s
- Visualization of cracks and other defects, generated during processing, testing or in service - without producing artefacts
- Generating numerical models from 3d-Images of real microstructures
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CMC- Material – WHIPOX™ Wound Highly Porous Oxide
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30 mm
Combustion chamber for small gas turbine
Processing by winding of alumina fiber bundles infiltrated with aqueous slurry of alumina powder and subsequent sintering
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Characteristic length scales of WHIPOX™
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100 µm 10 µm
Diamond pattern of wound fiber bundles (mm – range)
Cross section of adjacent fiber bundles with different orientation
Fibers embedded in porous matrix
Single fiber embedded in porous matrix
Microstructure of porous matrix
2 µm 1 µm
TEM ?
TEM-image of porous matrix (courtesy of M. Müller, GFE an der RWTH Aachen)
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Non destructive generation of 3d-images by X-ray tomography
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Computing 3d-reconstruction from set of X-ray projections of rotated sample (stepwise from 0° to 360°)
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Experimental set-up at Argonne Advanced Photon source
• Argonne National Laboratory, Argonne, Illinois • Synchrotron high energy X-Ray beam-line;
65keV beam energy
> 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 www.DLR.de • Chart 6
Illustration by Arbeitskreis Tomographie
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Tomography Stage for Data Acquisition
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X-ray beam
Detector
Sample holder
Furnace for high temperature experiments
Beam width: 1.8mm
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Sample preparation and mounting
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Ultrasonic drilling
Sample with +/- 45° fiber bundle orientation
Mounted sample on high temperature and room temperature fixture
2mm 5mm
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Monitoring sets of X-ray projections
X-ray projection Sample Mounted Sample
2mm 5mm
Laminate with +/- 45° fiber bundles
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X-ray projection Sample Mounted Sample
Monitoring sets of X-ray projections
2mm 5mm
Laminate with +/- 45° fiber bundles
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X-ray projection Sample Mounted Sample
Monitoring sets of X-ray projections
2mm 5mm
Laminate with +/- 45° fiber bundles
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www.DLR.de • Chart 12 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
X-ray projection Sample Mounted Sample
Monitoring sets of X-ray projections
2mm 5mm
Laminate with +/- 45° fiber bundles
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www.DLR.de • Chart 13 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
X-ray projection Sample Mounted Sample
Monitoring sets of X-ray projections
2mm 5mm
Laminate with +/- 45° fiber bundles
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www.DLR.de • Chart 14 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
X-ray projection Sample Mounted Sample
Monitoring sets of X-ray projections
2mm 5mm
Laminate with +/- 45° fiber bundles
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Sample Overview
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Sample Nr. Fiber architecture Chemical composition
1 UD-single bundle Al2O3-fiber, mullite matrix (3Al2O32SiO2 or 2Al2O3 SiO2)
2 UD- laminate as processed (1300°C, 1h)
Al2O3-fiber and matrix; as processed
3 UD- laminate aged (1450°C, 1h)
Al2O3-fiber and matrix; aged
4 +/- 45° laminate, aged Al2O3-fiber and matrix
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Unidirectional fiber bundle embedded in porous matrix Al2O3 – fibers and Mullite matrix
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As processed: sintered 1h at 1300°C Shrinkage cracks visible and good separation between fibers and matrix
0,5 mm
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Unidirectional fiber bundle embedded in porous matrix Al2O3 – fibers and Mullite matrix
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Shrinkage cracks due to processing
Fibers, matrix not shown
0.5 mm 50 µm
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Unidirectional WHIPOX™- Laminate Al2O3 – fibers and matrix (aged 1h at 1450°C)
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0.5 mm
Pores in sub - millimeter range, matrix rich regions between fiber bundles, shrinkage cracks in matrix, difficult separation between fibers and matrix
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Difference between as processed and aged
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As processed – few matrix cracks Aged – abundant matrix cracks
0,2 mm
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Laminate with +/- 45° layers (Al2O3-fibers and matrix) www.DLR.de • Chart 20 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
Ø 1,6 mm
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Laminate with +/- 45° layers (Al2O3-fibers and matrix)
Ø 1,6 mm
Fiber bundles, sub – millimeter pores, shrinkage cracks, fiber bundle cross lines
Aged at 1450°C for 1 h
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Laminate with +/- 45° layers (Al2O3-fibers and matrix)
Aim: parametric description of cross line geometry (fiber flexure, spatial fiber – matrix distribution)
Challenge: Difficult fiber separation in all alumina CMC 1 cm
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Laboratory X-ray tomography for high resolution
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Illustration by XRadia inc., now Zeiss
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X-ray tomography with laboratory devices: Porous Matrix of CMC
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10 µm
Measurement courtesy of XRadia inc., now Zeiss
Cross section image by scanning electron microscope
Slice of 3d-reconstruction from X-ray projections 1µm
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From reconstructed X-ray data to Finite Element Model
Reconstructed sample volume Cropped volume for analysis
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From reconstructed X-ray data to Finite Element Model
Cropped volume Segmented pores Segmented ZrO2 particles
Surface model Meshed surface Meshed volume 2µm edge length
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Import of 3d-image into Numerical Calculation Tool
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Exemplary virtual mechanical experiment
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Generating compressive stress by displacement of top plane
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Exemplary virtual mechanical experiment
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Exemplary virtual mechanical experiment
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Tomography based on FIB-Slices
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FIB: Focused ion beam
SEM: Scanning
electron microscope
Generating 2d-slices by ion beam cutting and subsequent recording SEM-images
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Generating a 3d – image of porous ceramic
• alignment • scaling • cropping • segmentation 3D-Volume
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Generating a 3d – image of porous ceramic II
Challenge: segmentation of pores and matrix due to information from underlying planes
0,5 µm
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Porosity from 3d-images and by Archimedes method www.DLR.de • Chart 34 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
Method for porosity measurement Porosity % ZrO2-Vol. %
X-ray tomography 35 - 36 2-3
FIB-slice tomography 35,4 2,8
Archimedes 36,1 -
FIB-slices X-ray tomography
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Summary and Outlook www.DLR.de • Chart 35 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
• X-ray tomography can provide excellent 3d-images of microstructures down to sub-micron range
• Non destructive technique • Using high energy synchrotron X-ray radiation provides unique options:
• Short acquisition time • No (severe) restriction of sample size for high resolution images
• Acquisition at high temperature possible • Acquisition under mechanical load (in-situ testing)
• Using laboratory devices with x-ray point source (and additional x-ray optics) allows high resolution but sample size is restricted (ca. 50µm)
• Slice and view technique using focus ion beam and scanning electron microscope allows higher resolution
• But no in situ acquisition at high temperatures or under load • Possibility of generating artefacts when slicing • Challenge: porous samples, showing in each slice information from
underlying material
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Summary and Outlook II www.DLR.de • Chart 36 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
• Data from X-ray tomography and slice and view techniques can be used for generating numerical microstructure models
• Virtual experiments can be done with Finite Element software
• Image analyses can be used to identify geometry parameters of the microstructure, which allow for generating virtual microstructures
• Parameter studies for elucidating the microstructure - property relationship
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Thank to co authors and other colleagues who have contributed to the presented results:
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DLR-Institute of Materials Research in Cologne:
S. Hackemann, K. Kelm, M. Schmücker, J. Wischek Department Mechanical and Aerospace Engineering, University of Central Florida, Orlando, Florida:
S. Raghavan, S. Sofronsky Fenn College of Engineering, Cleveland State University, Ohio:
C. Lacdao Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois:
J. Almer and J. Okasinski
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Thank you for your attention! Questions?
> 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 www.DLR.de • Chart 38
Acknowledgements: • This material is based upon work supported by the National Science Foundation
Grants OISE 1157619 and CMMI 1125696 • German Aerospace Center – aeronautic research program • Use of the Advanced Photon Source, an Office of Science User Facility operated
for the U.S. Department of Energy (DOE) Office of Science by Argonne National Laboratory, was supported by the U.S. DOE under Contract No. DE-AC02-06CH11357.