> 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016

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1 Chart 1 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 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

2 Chart 2 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Research Goals - 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

3 Chart 3 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 CMC- Material WHIPOX Wound Highly Porous Oxide 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

4 Chart 4 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Characteristic length scales of WHIPOX 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 TEM? 2 µm 1 µm Single fiber embedded in porous matrix Microstructure of porous matrix TEM-image of porous matrix (courtesy of M. Müller, GFE an der RWTH Aachen)

5 Chart 5 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Non destructive generation of 3d-images by X-ray tomography Computing 3d-reconstruction from set of X-ray projections of rotated sample (stepwise from 0 to 360 )

6 Chart 6 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Experimental set-up at Argonne Advanced Photon source Argonne National Laboratory, Argonne, Illinois Synchrotron high energy X-Ray beam-line; 65keV beam energy Illustration by Arbeitskreis Tomographie

7 Chart 7 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Tomography Stage for Data Acquisition Sample holder X-ray beam Detector Furnace for high temperature experiments Beam width: 1.8mm

8 Chart 8 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Sample preparation and mounting Ultrasonic drilling 2mm 5mm Sample with +/- 45 fiber bundle orientation Mounted sample on high temperature and room temperature fixture

9 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 Laminate with +/- 45 fiber bundles 2mm 5mm Sample Mounted Sample X-ray projection

10 Chart 10 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Monitoring sets of X-ray projections Laminate with +/- 45 fiber bundles 2mm 5mm Sample Mounted Sample X-ray projection

11 Chart 11 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Monitoring sets of X-ray projections Laminate with +/- 45 fiber bundles 2mm 5mm Sample Mounted Sample X-ray projection

12 Chart 12 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Monitoring sets of X-ray projections Laminate with +/- 45 fiber bundles 2mm 5mm Sample Mounted Sample X-ray projection

13 Chart 13 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Monitoring sets of X-ray projections Laminate with +/- 45 fiber bundles 2mm 5mm Sample Mounted Sample X-ray projection

14 Chart 14 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Monitoring sets of X-ray projections Laminate with +/- 45 fiber bundles 2mm 5mm Sample Mounted Sample X-ray projection

15 Chart 15 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Sample Overview Sample Nr. Fiber architecture Chemical composition 1 UD-single bundle Al 2 O 3 -fiber, mullite matrix (3Al 2 O 3 2SiO 2 or 2Al 2 O 3 SiO 2 ) 2 UD- laminate as processed (1300 C, 1h) 3 UD- laminate aged (1450 C, 1h) Al 2 O 3 -fiber and matrix; as processed Al 2 O 3 -fiber and matrix; aged 4 +/- 45 laminate, aged Al 2 O 3 -fiber and matrix

16 Chart 16 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Unidirectional fiber bundle embedded in porous matrix Al 2 O 3 fibers and Mullite matrix 0,5 mm As processed: sintered 1h at 1300 C Shrinkage cracks visible and good separation between fibers and matrix

17 Chart 17 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Unidirectional fiber bundle embedded in porous matrix Al 2 O 3 fibers and Mullite matrix 0.5 mm 50 µm Shrinkage cracks due to processing Fibers, matrix not shown

18 Chart 18 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Unidirectional WHIPOX - Laminate Al 2 O 3 fibers and matrix (aged 1h at 1450 C) 0.5 mm Pores in sub - millimeter range, matrix rich regions between fiber bundles, shrinkage cracks in matrix, difficult separation between fibers and matrix

19 Chart 19 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Difference between as processed and aged 0,2 mm As processed few matrix cracks Aged abundant matrix cracks

20 Chart 20 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Laminate with +/- 45 layers (Al 2 O 3 -fibers and matrix) Ø 1,6 mm

21 Chart 21 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Laminate with +/- 45 layers (Al 2 O 3 -fibers and matrix) Aged at 1450 C for 1 h Ø 1,6 mm Fiber bundles, sub millimeter pores, shrinkage cracks, fiber bundle cross lines

22 Chart 22 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Laminate with +/- 45 layers (Al 2 O 3 -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

23 Chart 23 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Laboratory X-ray tomography for high resolution Illustration by XRadia inc., now Zeiss

24 Chart 24 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 X-ray tomography with laboratory devices: Porous Matrix of CMC 10 µm Cross section image by scanning electron microscope Slice of 3d-reconstruction from X-ray projections 1µm Measurement courtesy of XRadia inc., now Zeiss

25 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

26 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 ZrO 2 particles 2µm edge length Surface model Meshed surface Meshed volume

27 Chart 27 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Import of 3d-image into Numerical Calculation Tool

28 Chart 28 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Exemplary virtual mechanical experiment Generating compressive stress by displacement of top plane

29 Chart 29 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Exemplary virtual mechanical experiment

30 Chart 30 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Exemplary virtual mechanical experiment

31 Chart 31 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Tomography based on FIB-Slices FIB: Focused ion beam SEM: Scanning electron microscope Generating 2d-slices by ion beam cutting and subsequent recording SEM-images

32 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

33 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 0,5 µm Challenge: segmentation of pores and matrix due to information from underlying planes

34 Chart 34 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Porosity from 3d-images and by Archimedes method FIB-slices X-ray tomography Method for porosity measurement Porosity % ZrO 2 -Vol. % X-ray tomography FIB-slice tomography 35,4 2,8 Archimedes 36,1 -

35 Chart 35 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Summary and Outlook 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

36 Chart 36 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Summary and Outlook II 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

37 Chart 37 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Thank to co authors and other colleagues who have contributed to the presented results: 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

38 Chart 38 > 3d imaging of ceramic CMC for numerical modelling - 91st annual meeting of the DKG - 8. March 2016 Thank you for your attention! Questions? Acknowledgements: This material is based upon work supported by the National Science Foundation Grants OISE and CMMI 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.