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Journal of Advanced Ceramics 2013, 2(4): 325-332 https://doi.org/10.1007/s40145-013-0079-4
Research Article | Open Access | Issue | Published: 04 December 2013

Characterization of free carbon in the as-thermolyzed Si–B–C–N ceramic from a polyorganoborosilazane precursor

Show Author's Information Adhimoolam Bakthavachalam KOUSAALYAa,  Ravi KUMARa,*( ),  Shanmugam PACKIRISAMYb
Materials Processing Section, Department of Metallurgical and Materials Engineering, Indian Institute of Technology Madras, Chennai 600036, Tamil Nadu, India
Analytical Spectroscopy and Ceramics Group, PCM Entity, Vikram Sarabhai Space Centre, Thiruvananthapuram 695022, India
Keywords:
synthesis, Raman spectroscopy, polyorganoborosilazane, precursor-derived ceramic, Si–B–C–N, free carbon
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KOUSAALYA AB, KUMAR R, PACKIRISAMY S. Characterization of free carbon in the as-thermolyzed Si–B–C–N ceramic from a polyorganoborosilazane precursor. Journal of Advanced Ceramics, 2013, 2(4): 325-332. https://doi.org/10.1007/s40145-013-0079-4
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Abstract Full text About this article

Polyorganoborosilazane ((B[C2H4–Si(CH3)NH]3)n) was synthesized via monomer route from a single-source precursor and thermolyzed at 1300 ℃ in argon atmosphere. The as-thermolyzed Si–B–C–N ceramic was characterized using X-ray diffraction (XRD) and Raman spectroscopy. The crystallization behavior of silicon carbide in the as-thermolyzed amorphous Si–B–C–N matrix was understood by XRD studies, and the crystallite size calculated using Scherrer equation was found to increase from 2 nm to 8 nm with increase in dwelling time. Concomitantly, Raman spectroscopy was used to characterize the free carbon present in the as-thermolyzed ceramic. The peak positions, intensities and full width at half maximum (FWHM) of D and G bands in the Raman spectra were used to study and understand the structural disorder of the free carbon. The G peak shift towards 1600 cm-1 indicated the decrease in cluster size of the free carbon. The cluster diameter of the free carbon calculated using TK (Tuinstra and Koenl) equation was found to decrease from 6.2 nm to 5.4 nm with increase in dwelling time, indicating increase in structural disorder.


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Characterization of free carbon in the as-thermolyzed Si–B–C–N ceramic from a polyorganoborosilazane precursor

Show Author's information Adhimoolam Bakthavachalam KOUSAALYAa, Ravi KUMARa,*( ), Shanmugam PACKIRISAMYb
Materials Processing Section, Department of Metallurgical and Materials Engineering, Indian Institute of Technology Madras, Chennai 600036, Tamil Nadu, India
Analytical Spectroscopy and Ceramics Group, PCM Entity, Vikram Sarabhai Space Centre, Thiruvananthapuram 695022, India

Abstract

Polyorganoborosilazane ((B[C2H4–Si(CH3)NH]3)n) was synthesized via monomer route from a single-source precursor and thermolyzed at 1300 ℃ in argon atmosphere. The as-thermolyzed Si–B–C–N ceramic was characterized using X-ray diffraction (XRD) and Raman spectroscopy. The crystallization behavior of silicon carbide in the as-thermolyzed amorphous Si–B–C–N matrix was understood by XRD studies, and the crystallite size calculated using Scherrer equation was found to increase from 2 nm to 8 nm with increase in dwelling time. Concomitantly, Raman spectroscopy was used to characterize the free carbon present in the as-thermolyzed ceramic. The peak positions, intensities and full width at half maximum (FWHM) of D and G bands in the Raman spectra were used to study and understand the structural disorder of the free carbon. The G peak shift towards 1600 cm-1 indicated the decrease in cluster size of the free carbon. The cluster diameter of the free carbon calculated using TK (Tuinstra and Koenl) equation was found to decrease from 6.2 nm to 5.4 nm with increase in dwelling time, indicating increase in structural disorder.

Keywords: synthesis, Raman spectroscopy, polyorganoborosilazane, precursor-derived ceramic, Si–B–C–N, free carbon

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Publication history
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Publication history

Received: 15 May 2013
Revised: 11 August 2013
Accepted: 20 August 2013
Published: 04 December 2013
Issue date: December 2013

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© The author(s) 2013

Acknowledgements

We gratefully acknowledge the financial support from the Vikram Sarabhai Space Centre, Thiruvananthapuram through ISRO-IITM cell (Project No. ICSR/ISRO-IITM/MET/08-09/122/RAVK). We also would like to acknowledge the Department of Physics, IIT-M for performing Raman spectroscopy.

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Open Access: This article is distributed under the terms of the Creative Commons Attribution License which permits any use, distribution, and reproduction in any medium, provided the original author(s) and the source are credited.

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