Real-time quantitative imaging of failure events in materials under load at temperatures above 1,600 °C

Journal name:
Nature Materials
Volume:
12,
Pages:
40–46
Year published:
DOI:
doi:10.1038/nmat3497
Received
Accepted
Published online

Abstract

Ceramic matrix composites are the emerging material of choice for structures that will see temperatures above ~1,500 °C in hostile environments, as for example in next-generation gas turbines and hypersonic-flight applications. The safe operation of applications depends on how small cracks forming inside the material are restrained by its microstructure. As with natural tissue such as bone and seashells, the tailored microstructural complexity of ceramic matrix composites imparts them with mechanical toughness, which is essential to avoiding failure. Yet gathering three-dimensional observations of damage evolution in extreme environments has been a challenge. Using synchrotron X-ray computed microtomography, we have fully resolved sequences of microcrack damage as cracks grow under load at temperatures up to 1,750 °C. Our observations are key ingredients for the high-fidelity simulations used to compute failure risks under extreme operating conditions.

At a glance

Figures

  1. In situ ultrahigh temperature tensile test rig.
    Figure 1: In situ ultrahigh temperature tensile test rig.

    a, Schematic illustration of in situ ultrahigh temperature tensile test rig for synchrotron X-ray computed microtomography (Beamline 8.3.2 of Advanced Light Source). b, Sectional view of the heating chamber illustrates X-ray transmission path through the heating chamber and sample. We have used this chamber to test materials at temperatures as high as 1,750 °C. c, Schematic of the rig in transmission mode for X-ray computed tomography.

  2. In situ testing of single-tow SiC–SiC composite specimens at room (25 °C) and ultrahigh (1,750 °C) temperatures.
    Figure 2: In situ testing of single-tow SiCSiC composite specimens at room (25 °C) and ultrahigh (1,750 °C) temperatures.

    Force–displacement curves are given in Fig. 3. a,b, Scanning electron micrographs (SEM) of room-temperature specimen after testing. Arrows in a indicate multiple matrix cracks normal to the applied tensile load. The image in b was taken after complete separation ex situ. Failure is associated with pullout of fibres from the matrix. c, Comparison of image resolution in a reconstructed μ-CT slice from the specimen in a before testing and a cross-sectional SEM image from another sample of the same composite. d, Longitudinal μ-CT slices from tests at 25 and 1,750 °C (both under an applied load of 127 N), showing a single planar crack in the former and bifurcated crack with two fibre breaks (indicated by arrows) in the latter. e, Cross-section μ-CT slices from the 1,750 °C specimen in d at two stages of loading (45 and 127 N). Red circles indicate a fibre that is intact at 45 N and broken at 127 N. f,g, 3D volume-rendered μ-CT images from specimens tested at room temperature (f) and at 1,750 °C (g) at several applied tensile loads, as indicated. False colours were applied in g to highlight the different test temperatures. * Load reading after first matrix crack initiated.

  3. Quantification of cracks in matrix and fibres of single-tow SiC–SiC composite specimens from Fig. 2.
    Figure 3: Quantification of cracks in matrix and fibres of single-tow SiCSiC composite specimens from Fig. 2.

    a,b, 3D rendering from μ-CT data shows matrix cracks and individual fibre breaks in specimens tested at 25 °C (a) and 1,750 °C (b). The red–blue colour scheme indicates opening displacements of matrix cracks, quantified by the processing of 3D tomography data. Yellow arrows indicate cylindrical holes remaining after relaxation of broken fibres. The fibre and matrix materials have been set transparent to reveal the cracks. * Load reading after first matrix crack initiated. c, Force–displacement curves from in situ tests in a,b. Red curve offset by 70 μm for visual clarity. Hollow circles indicate acquired μ-CT data at that load; blue and red solid circles indicate loads corresponding to images in a,b, respectively. d, Comparison of statistical data on fibre fracture at the peak loads in the specimens in a,b: each symbol indicates the distance of a fibre fracture from the nearest matrix crack and the separation of the fractured fibre ends after relaxation by sliding; red circles correspond to the 1,750 °C test, black circles to the 25 °C test. e, Histograms of the number of broken fibres as a function of distance from the closest matrix cracks at peak load. Further detailed animations of the complete sets of μ-CT data from these two tests are included in the Supplementary Movies S1 and S2.

  4. In situ tomography of C–SiC composite with textile-based carbon fibre reinforcements under a tensile load at 25 and 1,750 °C.
    Figure 4: In situ tomography of CSiC composite with textile-based carbon fibre reinforcements under a tensile load at 25 and 1,750 °C.

    a, Force–displacement curves showing loads at which μ-CT data were collected. Red curve offset by 60 μm for visual clarity. Hollow circles indicate acquired μ-CT data at that load; blue and red solid circles indicate loads corresponding to images in c,d respectively. b,  μ-CT image from the composite plate after partial infiltration of the SiC matrix illustrates the architecture of the woven fibre tows within the test samples. c,d,  μ-CT images showing development of damage in specimens tested at room temperature (c) and at 1,750 °C (d). The higher magnification slices at the right, from sections 1 and 2, show different cracking mechanisms (indicated by arrows) in the later stages of failure: at room temperature, splitting cracks grow within the axial fibre tows; at high temperature, cracks grow along the boundary between the axial fibre tows and the matrix. Further detailed animations of the complete sets of μ-CT data from these two tests are included in the Supplementary Movies S3 and S4.

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Author information

Affiliations

  1. Department of Materials Science and Engineering, University of California, Berkeley, California 94720, USA

    • Hrishikesh A. Bale &
    • Robert O. Ritchie
  2. Lawrence Berkeley National Laboratory, Berkeley, California 94720, USA

    • Abdel Haboub,
    • Alastair A. MacDowell,
    • James R. Nasiatka,
    • Dilworth Y. Parkinson &
    • Robert O. Ritchie
  3. Teledyne Scientific Company, Thousand Oaks, California 91360, USA

    • Brian N. Cox &
    • David B. Marshall

Contributions

B.N.C., D.B.M. and R.O.R. conceived the project, J.R.N. and A.A.M. designed the equipment and A.H. and H.A.B. built it. D.B.M. prepared the composite samples, H.A.B. performed the experiments and analysis with assistance from A.H., A.A.M., D.L.P. and D.B.M., and H.A.B., B.N.C., D.B.M. and R.O.R. wrote the manuscript with contributions from A.A.M.

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The authors declare no competing financial interests.

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Supplementary information

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    Supplementary Movie S1

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    Supplementary Movie S2

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    Supplementary Movie S3

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    Supplementary Movie S4

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