Study of interface reaction in a B4C/Cr mirror at elevated temperature using soft X-ray reflectivity

Boron carbide is a prominent material for high-brilliance synchrotron optics as it remains stable up to very high temperatures. The present study shows a significant change taking place at 550°C in the buried interface region formed between the Cr adhesive layer and the native oxide layer present on...

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Main Authors: Mohammed H. Modi, Shruti Gupta, Praveen K. Yadav, Rajkumar Gupta, Aniruddha Bose, Chandrachur Mukherjee, Philippe Jonnard, Mourad Idir
Format: Article
Language:English
Published: International Union of Crystallography 2022-07-01
Series:Journal of Synchrotron Radiation
Subjects:
Online Access:http://scripts.iucr.org/cgi-bin/paper?S1600577522004738
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author Mohammed H. Modi
Shruti Gupta
Praveen K. Yadav
Rajkumar Gupta
Aniruddha Bose
Chandrachur Mukherjee
Philippe Jonnard
Mourad Idir
author_facet Mohammed H. Modi
Shruti Gupta
Praveen K. Yadav
Rajkumar Gupta
Aniruddha Bose
Chandrachur Mukherjee
Philippe Jonnard
Mourad Idir
author_sort Mohammed H. Modi
collection DOAJ
description Boron carbide is a prominent material for high-brilliance synchrotron optics as it remains stable up to very high temperatures. The present study shows a significant change taking place at 550°C in the buried interface region formed between the Cr adhesive layer and the native oxide layer present on the silicon substrate. An in situ annealing study is carried out at the Indus-1 Reflectivity beamline from room temperature to 550°C (100°C steps). The studied sample is a mirror-like boron carbide thin film of 400 Å thickness deposited with an adhesive layer of 20 Å Cr on a silicon substrate. The corresponding changes in the film structure are recorded using angle-dependent soft X-ray reflectivity measurements carried out in the region of the boron K-edge after each annealing temperature. Analyses performed using the Parratt recursive formalism reveal that the top boron carbide layer remains intact but interface reactions take place in the buried Cr–SiO2 region. After 300°C the Cr layer diffuses towards the substrate. At higher temperatures of 500°C and 550°C the Cr reacts with the native oxide layer and tends to form a low-density compound of chromium oxysilicide (CrSiOx). Depth profiling of Si and Cr distributions obtained from secondary ion mass spectroscopy measurements corroborate the layer model obtained from the soft X-ray reflectivity analyses. Details of the interface reaction taking place near the substrate region of boron carbide/Cr sample are discussed.
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spelling doaj.art-439cea6db34746d5868804eb25fc6c082022-12-22T01:21:10ZengInternational Union of CrystallographyJournal of Synchrotron Radiation1600-57752022-07-0129497898410.1107/S1600577522004738ve5157Study of interface reaction in a B4C/Cr mirror at elevated temperature using soft X-ray reflectivityMohammed H. Modi0Shruti Gupta1Praveen K. Yadav2Rajkumar Gupta3Aniruddha Bose4Chandrachur Mukherjee5Philippe Jonnard6Mourad Idir7Soft X-ray Applications Laboratory, Raja Ramanna Centre for Advanced Technology, Indore 452013, IndiaSoft X-ray Applications Laboratory, Raja Ramanna Centre for Advanced Technology, Indore 452013, IndiaSoft X-ray Applications Laboratory, Raja Ramanna Centre for Advanced Technology, Indore 452013, IndiaSoft X-ray Applications Laboratory, Raja Ramanna Centre for Advanced Technology, Indore 452013, IndiaSuperconducting Proton Linac Section, Raja Ramanna Centre for Advanced Technology, Indore 452013, IndiaOptical Coating Laboratory, Raja Ramanna Centre for Advanced Technology, Indore 452013, IndiaSorbonne Universite, Faculte des Sciences et Ingénierie, UMR CNRS, Laboratoire de Chimie Physique-Matiere et Rayonnement, 4 Place Jussieu, F-75252 Paris Cedex 05, FranceNational Synchrotron Light Source II (NSLS-II), Brookhaven National Laboratory, PO Box 5000, Upton, NY 11973, USABoron carbide is a prominent material for high-brilliance synchrotron optics as it remains stable up to very high temperatures. The present study shows a significant change taking place at 550°C in the buried interface region formed between the Cr adhesive layer and the native oxide layer present on the silicon substrate. An in situ annealing study is carried out at the Indus-1 Reflectivity beamline from room temperature to 550°C (100°C steps). The studied sample is a mirror-like boron carbide thin film of 400 Å thickness deposited with an adhesive layer of 20 Å Cr on a silicon substrate. The corresponding changes in the film structure are recorded using angle-dependent soft X-ray reflectivity measurements carried out in the region of the boron K-edge after each annealing temperature. Analyses performed using the Parratt recursive formalism reveal that the top boron carbide layer remains intact but interface reactions take place in the buried Cr–SiO2 region. After 300°C the Cr layer diffuses towards the substrate. At higher temperatures of 500°C and 550°C the Cr reacts with the native oxide layer and tends to form a low-density compound of chromium oxysilicide (CrSiOx). Depth profiling of Si and Cr distributions obtained from secondary ion mass spectroscopy measurements corroborate the layer model obtained from the soft X-ray reflectivity analyses. Details of the interface reaction taking place near the substrate region of boron carbide/Cr sample are discussed.http://scripts.iucr.org/cgi-bin/paper?S1600577522004738boron carbidex-ray mirrorssynchrotron radiationsoft x-ray reflectivityx-ray optics
spellingShingle Mohammed H. Modi
Shruti Gupta
Praveen K. Yadav
Rajkumar Gupta
Aniruddha Bose
Chandrachur Mukherjee
Philippe Jonnard
Mourad Idir
Study of interface reaction in a B4C/Cr mirror at elevated temperature using soft X-ray reflectivity
Journal of Synchrotron Radiation
boron carbide
x-ray mirrors
synchrotron radiation
soft x-ray reflectivity
x-ray optics
title Study of interface reaction in a B4C/Cr mirror at elevated temperature using soft X-ray reflectivity
title_full Study of interface reaction in a B4C/Cr mirror at elevated temperature using soft X-ray reflectivity
title_fullStr Study of interface reaction in a B4C/Cr mirror at elevated temperature using soft X-ray reflectivity
title_full_unstemmed Study of interface reaction in a B4C/Cr mirror at elevated temperature using soft X-ray reflectivity
title_short Study of interface reaction in a B4C/Cr mirror at elevated temperature using soft X-ray reflectivity
title_sort study of interface reaction in a b4c cr mirror at elevated temperature using soft x ray reflectivity
topic boron carbide
x-ray mirrors
synchrotron radiation
soft x-ray reflectivity
x-ray optics
url http://scripts.iucr.org/cgi-bin/paper?S1600577522004738
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