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Possible evidence for the stabilization of β–carbon nitride by high-energy ball milling

Published online by Cambridge University Press:  31 January 2011

Y. Fahmy ,
T. D. Shen ,
D. A. Tucker ,
R. L. Spontak  and
C. C. Koch
Y. Fahmy
Affiliation:
Materials Science and Engineering Department, North Carolina State University, Raleigh, North Carolina 27695-7907
T. D. Shen
Affiliation:
Materials Science and Engineering Department, North Carolina State University, Raleigh, North Carolina 27695-7907
D. A. Tucker
Affiliation:
Materials Science and Engineering Department, North Carolina State University, Raleigh, North Carolina 27695-7907
R. L. Spontak
Affiliation:
Materials Science and Engineering Department, North Carolina State University, Raleigh, North Carolina 27695-7907
C. C. Koch*
Affiliation:
Materials Science and Engineering Department, North Carolina State University, Raleigh, North Carolina 27695-7907
*
c)Address all correspondence to this author. e-mail: CARL_KOCH@NCSU.EDU
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Abstract

The possibility of stabilizing the theoretically predicted β–C3N4 phase by high-energy ball milling is investigated. Charges of graphitic carbon were milled with and without minor alloying additions under different atmospheric media, namely gas and/or liquid phases of nitrogen, air, or ammonia. Milling was performed at either of two energy levels for periods of up to 48 h. The β–C3N4 phase was found to exist as small crystallites in a matrix of primarily amorphous carbon at volume fractions estimated between 5 and 10 at.%. High-resolution electron diffraction and x-ray diffraction indicate that the crystalline nature of the C3N4 phase corresponds with a hexagonal lattice with a = 6.46 Å and c/a = 0.374, which are within 2% of the theoretically calculated lattice parameter values. Analysis of electron energy-loss spectroscopy (EELS), x-ray photoelectron spectroscopy (XPS), and Fourier transform infrared (FTIR) spectra verify the presence of chemically bonded carbon and nitrogen with chemical states reflecting combined sp2 and sp3 hybridization. Chemical analysis confirms nitrogen enrichment at levels consistent with the C3N4 stoichiometry and the estimated degree of stabilization. The possible mechanism(s) responsible for the stabilization of the β–C3N4 phase are briefly discussed.

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Journal of Materials Research , Volume 14 , Issue 6 , June 1999 , pp. 2488 - 2499
Copyright
Copyright © Materials Research Society 1999

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