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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
www.DLR.de • Chart 1
Research Goals
www.DLR.de • Chart 2 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
- 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
CMC- Material – WHIPOX™ Wound Highly Porous Oxide
www.DLR.de • Chart 3 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
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
Characteristic length scales of WHIPOX™
www.DLR.de • Chart 4 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
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)
Non destructive generation of 3d-images by X-ray tomography
www.DLR.de • Chart 5 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
Computing 3d-reconstruction from set of X-ray projections of rotated sample (stepwise from 0° to 360°)
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
Tomography Stage for Data Acquisition
www.DLR.de • Chart 7 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
X-ray beam
Detector
Sample holder
Furnace for high temperature experiments
Beam width: 1.8mm
Sample preparation and mounting
www.DLR.de • Chart 8 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
Ultrasonic drilling
Sample with +/- 45° fiber bundle orientation
Mounted sample on high temperature and room temperature fixture
2mm 5mm
www.DLR.de • Chart 9 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
Monitoring sets of X-ray projections
X-ray projection Sample Mounted Sample
2mm 5mm
Laminate with +/- 45° fiber bundles
www.DLR.de • Chart 10 > 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
www.DLR.de • Chart 11 > 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
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
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
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
Sample Overview
www.DLR.de • Chart 15 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
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
Unidirectional fiber bundle embedded in porous matrix Al2O3 – fibers and Mullite matrix
www.DLR.de • Chart 16 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
As processed: sintered 1h at 1300°C Shrinkage cracks visible and good separation between fibers and matrix
0,5 mm
Unidirectional fiber bundle embedded in porous matrix Al2O3 – fibers and Mullite matrix
www.DLR.de • Chart 17 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
Shrinkage cracks due to processing
Fibers, matrix not shown
0.5 mm 50 µm
Unidirectional WHIPOX™- Laminate Al2O3 – fibers and matrix (aged 1h at 1450°C)
www.DLR.de • Chart 18 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
0.5 mm
Pores in sub - millimeter range, matrix rich regions between fiber bundles, shrinkage cracks in matrix, difficult separation between fibers and matrix
Difference between as processed and aged
www.DLR.de • Chart 19 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
As processed – few matrix cracks Aged – abundant matrix cracks
0,2 mm
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
www.DLR.de • Chart 21 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
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
www.DLR.de • Chart 22 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
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
Laboratory X-ray tomography for high resolution
www.DLR.de • Chart 23 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
Illustration by XRadia inc., now Zeiss
X-ray tomography with laboratory devices: Porous Matrix of CMC
www.DLR.de • Chart 24 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
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
www.DLR.de • Chart 25 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
From reconstructed X-ray data to Finite Element Model
Reconstructed sample volume Cropped volume for analysis
www.DLR.de • Chart 26 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
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
Import of 3d-image into Numerical Calculation Tool
www.DLR.de • Chart 27 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
Exemplary virtual mechanical experiment
www.DLR.de • Chart 28 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
Generating compressive stress by displacement of top plane
www.DLR.de • Chart 29 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
Exemplary virtual mechanical experiment
www.DLR.de • Chart 30 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
Exemplary virtual mechanical experiment
Tomography based on FIB-Slices
www.DLR.de • Chart 31 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
FIB: Focused ion beam
SEM: Scanning
electron microscope
Generating 2d-slices by ion beam cutting and subsequent recording SEM-images
www.DLR.de • Chart 32 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
Generating a 3d – image of porous ceramic
• alignment • scaling • cropping • segmentation 3D-Volume
www.DLR.de • Chart 33 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
Generating a 3d – image of porous ceramic II
Challenge: segmentation of pores and matrix due to information from underlying planes
0,5 µm
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
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
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
Thank to co authors and other colleagues who have contributed to the presented results:
www.DLR.de • Chart 37 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016
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
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.