Pure iron, plasma nitrided in low pressure triode ion plating equipmen
t, has been investigated by optical reflection microscopy, scanning tr
ansmission electron microscopy and glancing-angle X-ray diffraction, u
sing conventional and synchrotron radiation. The total thickness of th
e compound layer does not obey the square-root time dependence, as a r
esult of the continuous Ar + N ion bombardment during the nitriding pr
ocess. The grain size is also reduced in the compound layer. In additi
on to the variation in thickness of the nitride layers with increasing
process time, a change in the nitrogen concentration at the top of th
e compound zone also is observed. Increasing the nitriding time and/or
the N-2 partial pressure in the nitriding apparatus results in a larg
er nitrogen concentration in the top layer of the epsilon phase. Also,
a sin(2) psi method analysis has been carried out to measure the resi
dual macroscopic stresses in the different nitride layers of the compo
und zone.