Multilayer samples of nickel and aluminum with the compositions of Al-20 at
% Ni and Al-25 at% Ni were Prepared by the repeated folding and cold rollin
g (F&R) of elemental foils. Characterization by X-ray diffraction, scanning
electron microscopy and transmission electron microscopy/selected-area ele
ctron diffraction reveals that the rolling procedure results in a decrease
in thickness of the elemental layers to below 0.1 mum and a reduction in gr
ain size to below 50 nm, but does not induce Formation of an intermediate p
hase. Differential scanning calorimetry (DSC) measurements on samples subje
cted to different numbers of F&R cycles show double exotherms related to an
initial nucleation and lateral growth and a subsequent thickening of react
ively formed AI,Ni. The DSC data agree qualitatively with predictions of an
existing kinetic model fur multilayer reactions, but a decisively improved
quantitative fit is obtained when a distribution of layer spacings is cons
idered, rather than a well-defined modulation wavelength. The modified kine
tic model can be inverted to yield information on the evolution of the dist
ribution of layer sizes during deformation from DSC data. (C) 2001 Acta Mat
erialia Inc. Published by Elsevier Science Ltd. All rights reserved.