416 Materials Science and Engineering A 179/A 180 (1994) 416-421
Heat treatment of rapidly solidified Fe63Cr18Ti4B15
I. T.H. Chang, K. Ishii* and B. Cantor
Oxford Centrefor Advanced Materials and Composites, Universityof Oxford, Parks Road, Oxford OX1 3PH (UK)
Abstract
The crystallization behaviour and microstructural development during the annealing of amorphous melt-spun
Fe63Cr18Ti4B15 ribbons have been investigated by a combination of differential scanning calorimetry, transmission
electron microscopy (TEM) and energy dispersive X-ray microanalysis. The crystallization onset, peak, and finish
temperatures of the amorphous alloy are 571,589 and 600 °C respectively during continuous heating at 5 °C min- 1. The
incubation time for the onset of crystallization obeys the Arrhenius law, with an activation energy of 1.5 eV. The crystalli-
zation process obeys the Johnson-Mehl-Avrami law, with an Avrami exponent near to three, indicating near-spherical
3D growth on pre-existing nuclei, producing an equiaxed structure as observed by TEM. The activation energy for crystal
growth is 1.8 eV. Isothermal annealing for 2 h at temperatures in the range 550-1000 °C produces microstructures
consisting of a mixture of ferrite, faulted Cr-rich body centre tetragonal M2B boride particles and small Ti-rich primitive
tetragonal M3B 2 boride particles depending on the annealing temperature.
1. Introduction
In situ Fe-based particulate composites have
attracted much attention recently because of their
unique properties, such as high strength, excellent
thermal stability and superior corrosion and oxidation
resistance [1-7]. The composites consist of stable
borides embedded in an Fe matrix and are manu-
factured from Fe-TM-B alloys (TM = transition metal)
by rapid solidification followed by hot consolidation
[1-4]. The alloys are fully or partially amorphous after
rapid solidification [3-5], and the final microstructures
are controlled by amorphous/crystalline and crystal-
line/crystalline transformations during subsequent
annealing and consolidation.
The present work concentrates on differential
scanning calorimetry (DSC) and transmission electron
microscopy (TEM) studies of the heat treatment of a
rapidly solidified Fe63CrlsTi4B15 quaternary alloy
prepared by melt spinning. This paper describes the
crystallization behaviour and microstructural evolution
in melt-spun Fe63CrlsTi4B~5 alloy during heat treat-
ment within the temperature range 500-10000 °C.
2. Experimental methods
Amorphous ribbons of Fe61CrlsTi4Br15, 30-50/zm
in thickness, were manufactured by chill block melt
*Present address: Kawasaki Steel Corporation, 1 Kawasaki-
cho, Chiba, Japan.
spinning in air. Specimens of the amorphous ribbons
were annealed for 2 h in sealed quartz tubes filled with
Ar gas, at different temperatures in the range
550-1000 °C. Crystallization kinetics were monitored
with a Dupont 2000 thermal analyzer/910 differential
scanning calorimeter during continuous heating at 5 °C
min-1 from 200-710 °C and isothermal heating in the
range 400-655 °C. The microstructures and micro-
compositions of the as-melt spun and annealed ribbons
were examined by a combination of TEM and energy
dispersive X-ray microprobe analysis (EDX). TEM
specimens were prepared by mechanical polishing
followed by twin-jet electro-polishing in 73 vol.%
ethanol + 8 vol.% perchloric acid + 10 vol.% butylcel-
losolve + 9 vol.% distilled water at - 10 °C to - 15 °C,
and were then examined in a Philips CM20 transmis-
sion electron microscope fitted with a LINK Systems
energy dispersive X-ray analyzer.
3. Results and discussion
3.1. DSCstudy
Figure 1 shows a typical DSC trace obtained during
continuous heating to 710 °C at a rate of 5 °C min -~.
The continuous heating DSC trace showed a small,
broad exothermic peak over the temperature range
510-570 °C, and a large, sharper exothermic peak with
onset, peak and finish temperatures of 571, 589 and
600 °C respectively, associated with crystallization of
the amorphous alloy. The crystallization temperature
of amorphous Fe63CrlsTi4B15 was higher than those of
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