Single source precursor derived SiBCNHf ceramic with enhanced high‐temperature microwave absorption and antioxidation

doi:10.1016/j.jmst.2022.03.015

Abstract

Abstract:

Electromagnetic (EM) wave-absorbing materials with high-temperature-resistance are urgently desirable to eliminate EM interference in extreme conditions. Precursor derived ceramics (PDC) route is being evolved as an effective strategy to solve the puzzle. Herein, a single source hyperbranched polyborosilazane precursor containing hafnium (hb-PBSZ-Hf) is introduced and the SiBCNHf ceramic is obtained by further pyrolysis. The micro-sized tissues including HfC, SiC, HfB₂ nanocrystals and segregated carbons are in situ generated during annealing which not only increase EM wave absorption ability (minimum reflection coefficient (RC_min) is -56.71 dB with a thickness of 2.5 mm, effective absorption bandwidth (EAB) is 3.4 GHz), but also improve antioxidation property (less than 2 wt.% mass fluctuation at 1400 °C in air). Theoretical simulation of complex permittivity suggests that SiBCNHf ceramic has an RC_min of less than -5 dB for the whole X-band even at 1100 °C. Such SiBCNHf ceramic with superior high-temperature-resistance and antioxidation performance derived from single source precursors possesses great potential for EM wave absorbing coatings in high-temperature and harsh environments.

Key words: hb-PBSZ-Hf precursor, SiBCNHf ceramic, EM wave absorption, Antioxidation performance

Yan Song, Ziyu Liu, Xicheng Zhang, Runqiu Zhu, Youwei Zhang, Pinggui Liu, Lihua He, Jie Kong. Single source precursor derived SiBCNHf ceramic with enhanced high‐temperature microwave absorption and antioxidation[J]. J. Mater. Sci. Technol., 2022, 126: 215-227.

Figures/Tables 13

Scheme 1. Synthesis route for hb-PBSZ-Hf precursor by the reaction of hb-PBSZ and TDEAH compound.

Fig. 1. Structure characterization of TDEAH, hb-PBSZ and hb-PBSZ-Hf precursor, (a) FT-IR spectra, (b) FT-IR spectra from 1700 cm−1 to 400 cm−1, (c) 1H NMR spectra and (d) 11B-NMR spectra.

Fig. 2. TG curves of hb-PBSZ-Hf precursors with different Hf contents (a), TG-MS spectra of a typical hb-PBSZ-Hf precursor (b), TG curves of the different Hf contents SiBCNHf ceramics with different Hf contents under argon atmosphere and air atmosphere, respectively (c, d).

Fig. 3. XPS spectra of SiBCNHf ceramics with different Hf contents, (a) XPS survey wide scan spectra of SiBCNHf ceramics, (b)-(f) C 1 s scan spectrum, Hf 4f scan spectrum, B 1s scan spectrum, Si 1s scan spectrum and O 1s scan spectrum, respectively, of a typical SiBCNHf ceramic.

Fig. 4. Raman spectra of SiBCNHf ceramics with different Hf content and annealed at different temperatures, (a) SiBCNHf(20) ceramics annealed at 1200-1700 °C, (b) SiBCNHf(25) ceramics annealed at 1200-1700 °C, (c) SiBCN ceramics annealed at 1500-1700 °C, (d) SiBCNHf ceramics annealed at 1700 °C.

Fig. 5. XRD patterns of SiBCNHf ceramics with different Hf contents and annealed at different temperatures, (a) SiBCNHf(20) ceramics annealed at 1200-1700 °C, (b) SiBCNHf(25) ceramics annealed at 1200-1700 °C, (c) SiBCN ceramics annealed at 1500-1700 °C, (d) SiBCNHf ceramics annealed at 1700 °C.

Fig. 6. TEM, HRTEM and SAED images of SiBCN ceramic (a-c) and SiBCNHf(20) ceramic (d-f) annealed at 1500 °C.

Fig. 7. TEM, HRTEM and SAED images of SiBCN ceramic (a-c) and SiBCNHf(20) ceramic (d-f) annealed at 1700 °C.

Fig. 8. Real part ε', imaginary part ε" and dielectric loss (tan δ) of SiBCNHf(20)−1200 from 25 °C to 600 °C (a-c), real part ε', imaginary part ε" and dielectric loss (tan δ) of SiBCNHf(25)−1100 from 25 °C to 600 °C (d-f).

Fig. 9. RC curves vs frequency and sample thickness, (a, b) SiBCNHf(20)−1200 at 25 °C, (c, d) SiBCNHf(25)−1100 at 25 °C, (e) RC of SiBCNHf(20)−1200 from 25 °C to 600 °C with a thickness of 2.90 mm, (f) RC of SiBCNHf(25)−1100 from 25 °C to 600 °C with a thickness of 2.60 mm.

Fig. 10. Dependence of real permittivity, imaginary permittivity, and loss tangent on temperature (a-c). The square point is the average value of the measured value at each temperature (25-600 °C), the line represents the linear curve fitted according to the test values, and the dot represents the values calculated according to the fitted curve at a specific temperature (a, b, c), RC at 600 °C calculated from simulated values (d), RC at 600 °C calculated from test values (e), RC at 1100 °C calculated from simulated values (f) (For interpretation of the references to color in this figure legend, the reader is referred to the web version of this article).

Fig. 11. SiBCNHf ceramic coating on the graphite plate with a thickness of 0.256 mm (a-d), SiBCNHf ceramic coating on the graphite plate after heat treatment in Ar at 1100 °C for 2 h with a thickness of 0.204 mm (e-h).

Fig. 12. Schematic diagram of the proposed EM wave absorption mechanism corresponding to SiBCNHf ceramic.

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