Microstructure and mechanical behavior of annealed

MP35N alloy wire

In a previous paper, the microstructure, monotonic, and cyclic response of
as-drawn ~100 µm diameter MP35N low-Ti alloy wire were presented and
discussed. In this sequel paper, the effects of annealing the same cold-drawn
wire on microstructure and mechanical properties are examined. Specifically,
segments of the wire were annealed for 1 hour at 973 K, 1023 K, 1073 K, 1123
K and 1173 K in a vacuum furnace. The resulting microstructure was
characterized by SEM, EBSD and TEM and compared to the as-drawn
microstructure. In-situ heating in the TEM of MP35N ribbon in a similarly cold
worked condition enabled corroboration of microstructure evolution during
annealing. Postdeformation structures and fracture surfaces were characterized
using TEM and SEM respectively. Yield strength decreases rapidly with
recrystallization to almost half the value of the as-drawn condition, but is
accompanied by an increase in modulus and tensile elongation reaching ~30
percent.

The multi-component alloy, MP35N with a nominal composition 35%Co,

35%Ni, 20%Cr and 10% Mo and exhibiting exceptional fracture strength and
corrosion resistance is used as conducting wires in active implantable medical
devices to bring the electrical signal from the pulse generator to the treatment
location.

This alloy retains a metastable face centered cubic structure at room

temperature and exhibits a low stacking fault energy a yield strength of around
2 GPa that is accompanied by ~3% tensile elongation to failure and negligible
strain hardening; deformation twinning and de-twinning appeared to be the
primary carriers of plasticity, while in the pronounced necked region of the
tensile specimens where extensive deformation had occurred, twin
intersections coupled with shearing resulted in twin fragmentation and the
development of nanocrystalline grains analogous to those observed in severe
plastic deformation.

A study of the cyclic deformation response of the alloy confirmed that at a

stress amplitude of ~400 MPa or less, the fatigue life is > 107 cycles whereas
at stress amplitude levels of 550 MPa-600 MPa, the fatigue life was < 5x10 5
cycles.
Furthermore, fracture initiation appeared to often be associated with
Al2O3 inclusions in the material. It is worth noting that the maximum stress
levels are quite high, and are of the order of 1 GPa or greater.
The presence of micron-size Al2O3 inclusions in the wire can lead to high
stress concentrations at the inclusion-matrix interfaces that can produce a
scatter in fatigue life, particularly at the higher stress levels and in the tension-
tension loading mode.
A rather intriguing set of results was recently published by Sorensen et al.
who showed a reduction in fracture strain from ~3.5% to 1% upon annealing of
37% and 60% cold-drawn wires of MP35N low Ti alloy for durations of 60 s at
different temperatures over the temperature range of 573-1173 K in air. The
grain size was found to remain unchanged in this temperature range. The
reduction in the ductility of the annealed alloy was attributed to the
segregation of Mo to faults and twins that made dislocation motion significantly
harder.
Nevertheless, it appears that a balance in strength and ductility through
controlled recrystallization via judicious heat-treatments could render
enhanced crack-tip plasticity in fatigue crack growth and reduce sensitivity to
loss in fatigue life due to the presence of inclusions. Therefore, in this
investigation, a series of heat treatments were conducted on the drawn wire,
the resulting microstructure was characterized in detail, and its mechanical
behavior by the way of monotonic and cyclic deformation response was
evaluated.
A low-Ti MP35N alloy wire having a 100-µm diameter and with 40% cold-
work in the s-drawn state was subjected to isothermal annealing for an hour at
various temperatures and microstructural evolution, uniaxial tensile response
and cyclic deformation behavior were studied.
Annealing at 973 K results in a partially recrystallized structure, where faceted
bulging of twin boundaries was noted and confirmed by in-situ heating in the
TEM; annealing at higher temperatures results in a fully recrystallized
microstructure that incorporates annealing twins. Crystallographic texture was
similar to that observed in the as-drawn wire and no additional phases were
detected.
Annealing at 973 K for one hour resulted in a loss in yield strength and tensile
elongation. Annealing at higher temperatures resulted in even further loss in
yield strength , significant improvements in ductility and noticeable work
hardening response.
In the fully recrystallized state, the yield strength response as a function of
grain size could be described by the Hall-Petch equation for the range of grain
size that could be obtained, with high values of Hall-Petch constants .
In agreement with an earlier study , a substantial increase in elastic modulus
was noted for the annealed microstructure as compared to the cold-drawn wire;
further work is needed to fully understand the origin of this change.
In the as-drawn condition, by virtue of its very high yield strength, the MP35N
low-Ti wire displays respectable stress-controlled cyclic response, although the
presence of micron-sized Al2O3 inclusions can trigger fatigue failure, and the
limited ductility and lack of strain hardening capacity in the as-drawn wire
results in rapid cyclic crack growth. This can result in a scatter in data,
particularly in the HCF regime. The annealed wire with the recrystallized
microstructure displays significant plasticity and therefore has the ability to
mitigate the deleterious effects of the inclusions but the overall yield strength
is significantly lower so that on an absolute basis, the annealed material
displays an S-N response that is comparable to the as-drawn wire but not any
better. However, when the maximum applied cyclic stress is normalized by
yield strength, then the beneficial effects of plasticity and strain hardening is
immediately recognized.