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Degradation of carbon fiber-reinforced ultra-high-temperature ceramic matrix composites at extremely high temperature using arc-wind tunnel tests

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Abstract

The heat resistance of carbon fiber-reinforced ultra-high-temperature ceramic matrix composites (C/UHTCMCs) was characterized by arc-wind tunnel testing with heat fluxes of 2, 4.54, and 6.68 MW/m2. C/UHTCMCs were fabricated via Zr-Ti binary alloy (Zr-20at%Ti, Zr-64at%Ti, Zr-80at%Ti) melt infiltration. The thickness and weight changes of the specimen were dependent on the composition of the infiltrated Zr-Ti alloy. Microstructural and thermodynamic analyses revealed that formed oxides on the surface of composites are composed of ZrO2 solid solution, ZrTiO4 solid solution, and TiO2 solid solution. The composition of oxides also depends on the composition of infiltrated alloys. The difference originates from the formation and composition of oxide scales and the dynamic pressure. Especially, formation of liquid oxides accelerates the recession of composites because liquid oxides are disappeared from the surface owing to the dynamic pressure during arc-wind tunnel testing. To withstand aerodynamic heating above 2000 °C, formation of a solid (and liquid) oxide on the exposed surface is required to reduce recession.

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Acknowledgments

The results of this study were obtained using the Arc Heating Facility of the Institute of Space and Astronautical Science (ISAS), Japan Aerospace Exploration Agency (JAXA). We are deeply grateful to Takayuki Shimoda and Tetsuo Yoshida for their assistance with the arc-wind tunnel tests.

Funding

This research was partially supported by the Japan Society for the Promotion of Science (JSPS) KAKENHI (Grant-in-Aid for challenging Exploratory Research), Grant Number 21K18782, and JSPS KAKENHI (Grant-in-Aid for Early-Career Scientists), Grant Number 22K14152.

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Authors and Affiliations

  1. Department of Mechanical Engineering, Tokyo University of Science, 6-3-1, Niijuku, Katsushika-ku, Tokyo, 125-8585, Japan

    Noriatsu Koide, Tomoki Marumo & Ryo Inoue

  2. Department of Materials Science and Technology, Tokyo University of Science, 6-3-1, Niijuku, Katsushika-ku, Tokyo, 125-8585, Japan

    Yutaro Arai

  3. Division of Systems Research, Faculty of Engineering, Yokohama National University, 79-5, Tokiwadai, Hodogaya-ku, Yokohama, 240-8501, Japan

    Makoto Hasegawa

  4. National Institute for Materials Science (NIMS), 1-2-1, Sengen, Tsukuba, Ibaraki, 305-0021, Japan

    Toshiyuki Nishimura

Authors
  1. Noriatsu Koide
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  2. Tomoki Marumo
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  3. Yutaro Arai
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  4. Makoto Hasegawa
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  6. Ryo Inoue
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Contributions

NK contributed to data curation; formal analysis; investigation; and writing—original draft. TM contributed to data curation; formal analysis; and investigation. YA contributed to data curation; formal analysis; methodology; writing—original draft; writing—review and editing. MH contributed to writing—review and editing. TN contributed to writing—review and editing. RI contributed to conceptualization; data curation; formal analysis; funding acquisition; resources; writing—original draft; writing—review and editing.

Corresponding author

Correspondence to Ryo Inoue.

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Handling Editor: M. Grant Norton.

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Appendix 1

Appendix 1

In this study, the crystalline structure of the matrix was characterized by X-ray diffraction. Typical X-ray diffraction profiles of the as-fabricated composites are shown in Fig. 

Figure 13
figure 13

XRD profiles of as-fabricated composites

Full size image

13. The diffraction peaks correspond to those of carbon, ZrC, and TiC, respectively.

As reported elsewhere, a solid solution of ZrC and TiC (hereafter denoted as (Zr,Ti)C) can be formed through the melt infiltration (MI) process, as both carbides possess face-centered cubic structures (NaCl-type structure). Furthermore, the lattice parameter of (Zr,Ti)C depends on the relative content of TiC and ZrC, varying from 0.4249 nm for TiC to 0.46976 nm for ZrC. Although the composition of Zr and Ti in the carbides varied in accordance with the Zr and Ti content in the alloys, the formation of carbides containing Ti and Zr was recognized and is independent of the Zr-Ti proportions in the alloys. It was concluded that the following reaction occurred:

$${\text{Zr - Ti}}\left( {\text{l}} \right) \, + {\text{ C}}\left( {\text{s}} \right) \, \to \, \left( {\text{Zr,Ti}} \right){\text{C}}\left( {{\text{s.s.}}} \right)$$
(5)

Since no residual alloys were detected by SEM–EDX and XRD analysis, the matrix in the composites is composed of (Zr, Ti) C.

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Koide, N., Marumo, T., Arai, Y. et al. Degradation of carbon fiber-reinforced ultra-high-temperature ceramic matrix composites at extremely high temperature using arc-wind tunnel tests. J Mater Sci 57, 19785–19798 (2022). https://doi.org/10.1007/s10853-022-07861-x

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