Materials Science Forum Vols.

503-504 (2006) pp 161-168

Online available since 2006/Jan/15 at www.scientific.net
© (2006) Trans Tech Publications, Switzerland
doi:10.4028/www.scientific.net/MSF.503-504.161

Enhancement of Ductility and Strength through Microstructural

Refinement by FSP of Nickel Aluminum Bronze

K. Oh-ishi1, a, A. P. Zhilyaev1, 2, b, and T. R. McNelley1, c

1
Department of Mechanical & Astronautical Engineering, Naval Postgraduate School,
700 Dyer Road, Monterey, CA 93943-5146 USA
2
Institute of Mechanics, Russian Academy of Science, 12 K. Marx, Ufa,
450000 Russia
a
koishi@nps.edu, apzhilya@nps.edu, ctmcnelley@nps.edu
b

Keywords: Friction Stir Processing, Nickel Aluminum Bronze, Phase Transformation,

Grain refinement, Tensile properties

Abstract. Friction stir processing (FSP) is a severe plastic deformation (SPD) method that has been
applied to as-cast NiAl bronze (NAB) materials, which are widely used for marine components.
The thermomechanical cycle of FSP results in homogenization and refinement, and the selective
conversion of microstructures from a cast to a wrought condition. The physical metallurgy of NAB
is complex and interpretation of the effects of FSP on microstructure has required detailed analysis
by optical and electron microscopy methods. Annealing and isothermal hot rolling have been
employed to confirm microstructure-based estimates of stir-zone peak temperatures. The variation
of mechanical properties was assessed by use of miniature tensile samples and correlated with
microstructure for samples from stir zones of single and multi-pass FSP. Exceptional improvement
in strength – ductility combinations may be achieved by FSP of NAB materials.

Introduction
FSP is an emerging metal working technology that can provide localized modification and control
of microstructures in near-surface layers of processed metallic components [1-3]. This technology
represents an adaptation of the principles of friction stir welding, a solid-state joining process
originally developed at The Welding Institute [4]. In FSP, a cylindrical, wear-resistant tool
consisting of a smaller diameter pin with a concentric, larger-diameter shoulder is rotated and
forced into the surface of a single piece of material. The tool shoulder acts to constrain upward
metal flow caused by pin insertion; friction at the tool-work piece interface results in heating and a
‘stirring’ action that, in turn, produces adiabatic heating and local softening of the material. A ‘stir
zone’ is created by severe plastic deformation with vertical as well as horizontal displacements of
material about the pin. Local thermomechanical cycles result in microstructure refinement and
homogenization, leading to improved strength and ductility of stir zone material [1-3; 5-10].
FSP of as-cast NAB alloys eliminates casting porosity and provides microstructure refinement [11].
Cast NAB alloys are widely used for marine components that often involve thick sections; slow
cooling rates (typically10-3 – 10-2 ºCs-1) result in coarse grain sizes (~1 mm) and reduced properties.
Thus, FSP represents a method for selectively strengthening such components. The constitution and
transformation characteristics of NAB have been reviewed and the effects of FSP on the
microstructure of an equilibrium-cooled material have been evaluated recently [11]. Phase
transformations during cooling of NAB materials are strongly dependent on the prior annealing
temperature and cooling rate. Heating and severe concurrent deformation during FSP accelerated
reactions such as the reversion of the eutectoid g + iii s , which took place in regions where the
peak temperature exceeded 800 ºC. The cooling rates in processed material resulted in various non-
equilibrium transformation products of the , which included mixtures of Widmanstätten g, bainite
and martensite. Microstructure - mechanical property correlations in FSP stir zones have been
examined by Mahoney, et al. [12], using mini-tensile specimens to facilitate mechanical property
evaluation in the presence of steep microstructure gradients. The objective of present study is to

All rights reserved. No part of contents of this paper may be reproduced or transmitted in any form or by any means without the written permission of TTP,
www.ttp.net. (ID: 128.118.88.48, Pennsylvania State University, University Park, USA-08/11/14,07:55:07)
162 Nanomaterials by Severe Plastic Deformation

examine mechanical properties through the stir zone and correlate them with the corresponding
microstructures in NAB materials performed by various process conditions.
Microstructure of NAB processed by FSP. Fig. 1(a) shows a representative microstructure from a
transverse cross section in a sample following a single pass using rotation and traversing rates of
800 rpm and 6 ipm [11]. The direction of tool advance is into the page so that the advancing side is
on the right while the retreating side is to the left. Microstructure of stir zone is much refined when
compared to as-cast NAB material. The boundary between the stir zone and base metal is sharp on
the advancing side and directly under the tool, but it is less distinct on the retreating side. Region 2
is from a location further below the surface, and shows a banded structure consisting of primary g
(light-etched) and phase transformation products (dark-etched). Fig. 1(b) is a TEM micrograph
for the location corresponding to dark-etched phase of the bands in region 2. Fine globular
precipitates and a very fine structure having a lamellar appearance are evident. An elongated, rod-
like grain and martensite structure are apparent. Those structures have formed by bainitic and
martensitic transformations during cooling from d phase induced by heating to high temperature
during FSP. Below these bands a grain flow pattern due to tool rotation is evident. Fig. 1(c) shows
a TEM micrograph from region 4. In this location, the microstructure is highly refined and exhibits
g grains about 1 - 2 om in size. Particles of the various phases that have been broken up and
partially spheroidized by the severe deformation are apparent along boundaries and in between g
grains in the structure. The predominance of g and of deformation-induced changes in the phases
likely reflects little or no d phase formation due to lower peak temperatures in this region. Thus, stir
zone microstructures reflect local peak temperature distributions during FSP as well as the
subsequent cooling rates. Peak temperature is confirmed to have temperature gradients, and be
higher near the upper stir zone based on observed stir zone microstructures.

Experimental Procedure
The material examined in this investigation conforms to the composition specification for UNS
C95800 NAB [13]. The data are summarized in Table 1. Isothermal hot rolling was accomplished

Fig.1 (a) Optical micrograph of stir zone and (b)(c) TEM micrographs from region 2 and
region 4 in the stir zone, respectively. [11]
 Materials Science Forum Vols. 503-504 163

by preheating NAB billets 20 mm in thickness to the intended hot rolling temperature, and then
rolling, with reheating between successive passes, to a final thickness of 2 mm, corresponding to a
nominal strain of 2.3. FSP was accomplished at the Rockwell Scientific Company, Thousand Oaks,
CA using a Densimet® tool having stepped spiral threads. Pin depth was 12.7 mm (0.5 in). In the
present investigation as-cast NAB material was processed using either a single linear traverse
(material and process designated FSP858; Table 1) or a raster pattern (FSP754; Table 1). In all case
the tool was inclined ~ 3 º opposite to the direction of tool advance [14].

Table 1. Composition specification [13] and data for UNS C95800 NAB alloys processed by
FSP
Element Cu Al Ni Fe Mn Si Pb
Min-max (min)79.0 8.5-9.5 4.0-5.0 3.5-4.5 0.8-1.5 0.10(max) 0.03(max)
Nominal 81 9 5 4 1 - -
FSP858 81.03 9.27 4.62 3.45 1.40 0.06 0.01
FSP754 80.16 9.38 4.66 4.41 1.20 0.05 <0.005

Optical microscopy involved standard sample preparation and observation methods. Samples were
etched in a two-step process. Samples were first immersed for 1 – 2 s in a solution of 40 ml water –
40 ml ammonium hydroxide – 2 ml hydrogen peroxide (30 %), rinsed in water, and then immersed
1 –2 s in a solution of 60 ml water – 30 ml phosphoric acid – 10 ml hydrogen peroxide. Etched
samples were examined using bright-field illumination in a Jenaphot 2000 equipped with a digital
imaging system [11].
Miniature tensile coupons having gage dimensions of 7.7 mm length, 2.7 mm width and 1mm
thickness were cut from stir zones by electric discharged machining. The gage length was aligned
with the direction of tool advance and coupons were deformed at room temperature to failure at a
constant cross head speed. Fractography was performed with a Topcon SM-510 scanning electron
microscope (SEM) for selected samples.

Results
Fig. 2 summarizes results from annealing and air cooling (100 Cs-1 – 10+2 °Cs-1) as well as from the
isothermal hot rolling of NAB material. As-cast NAB typically exhibits an ultimate tensile strength
(UTS) of 380 – 410 MPa, with ~11 % elongation to failure; annealing at various temperatures in
the range 870 – 1000 °C, followed by air cooling, results in a slight increases in UTS coupled with
decreased ductility. Isothermal hot rolling to a strain of 2.3, followed by air cooling, resulted further
strengthening, and an increase in UTS with increasing hot rolling temperature. Furthermore, hot
rolling this temperature range resulted in substantial increases in ductility, and nearly 30 %
elongation to failure was attained in material hot rolled at 1000 °C. Representative microstructures
for annealed and for hot rolled material are included in Fig. 2(b) and 2(c), respectively, for a
temperature of 950 °C. The light- and dark-etching phases are the primary g phase and the products
of transformation during cooling, respectively [11]. The primary g has become elongated in the
rolling direction by the concurrent deformation, as seen in Fig. 2(c). Widmanstätten g as well as
bainitic and martensitic transformation products of the prior are evident in both microstructures,
although hot rolling results in an elongated morphology in the prior and refines these
transformation products when compared to annealing alone.
Fig. 3(a) shows a montage of optical micrographs from a transverse cross section in the FSP858
sample, which had experienced a single pass using 1000 rpm and 4 ipm. Again, the direction of tool
advance is into the page so that the advancing side is on the right while the retreating side is to the
left. The white dashed frames indicate the grip-end outline of tensile samples corresponding to the
indicated locations. The upper region and bottom of the stir zone show band-like structures that
comprise of light- and dark-etching phases that are elongated and aligned in a horizontal direction
164 Nanomaterials by Severe Plastic Deformation

(a)
800 40 (b)

600 30

Ductility, %
UTS, MPa

400 20 100 µm
UTS_Ann
UTS_HR ( )
Ductility_Ann
200 Ductility_HR 10

0 0
850 900 950 1000 100 µm
T, °C

Fig.2 Mechanical properties (a) and optical microstructures (b and c) of annealed or

hot rolled (10:1 reduction) NAB, respectively.
(Fig. 3(b), region 1). Such structures are reminiscent of the hot rolled condition for 950 °C (Fig.
2(c)). At the top of the stir zone these band structures extend horizontally from a location under the
tool shoulder on the retreating side inward across the stir zone. A swirl pattern, or ‘onion-ring
structure’, is apparent in the central region of the stir zone. At higher magnification (Fig. 3(b),
region 5), the onion-ring structure is seen to consist of fine g, fine Widmanstätten g, and unresolved
transformation products of . Outside of the stir zone a narrow thermomechanically affected zone
(TMAZ) and a broader heat affected zone (HAZ) are both apparent. Region 9 (Fig. 3(b)) includes
the boundary between the stir zone and TMAZ as well as HAZ material, and includes primary g
and transformation products of from annealing alone. This reflects the eutectoid reversion
reaction g + iii s accompanied by little or no deformation. The boundary between the stir zone
and TMAZ is more distinct on the advancing side than on the retreating side.
Fig. 4 shows a corresponding montage of optical micrographs from traverse cross section for
FSP754. The FSP of this sample involved rastering but using the same rotation and traversing rate
as FSP858, i.e., 1000 rpm and 4 ipm. The center of this montage corresponds to the line of the last
pass in the raster. Again, individual white frames indicate the locations of the grip ends of tensile
samples. The raster spacing is ~8.3 mm so that stir zones overlap to the bottom of the pin. Thus,
during rastering the advancing side of a pass overlaps retreating side of the adjacent pass. The
montage includes three stir zones, each having the onion-ring structure. The onion structure of a
given pass is always distorted by a successive pass. At higher magnification (Fig. 4(b)), region 3
exhibits a refined Widmanstätten g structure, while region 5 is within the onion-ring structure and
comprises bands of fine Widmanstätten g and fine g grains. Such distinct and refined
Widmanstätten g regions were not observed in samples after a single linear pass (e.g., see data for
FSP858, Fig. 3).
Stress-strain data were obtained using miniature tensile samples, and UTS and elongation to failure
results were correlated with stir zone location. Fig. 5 shows mesh plots of the data for FSP858 and
FSP754. In FSP858, i.e. for a single FSP pass, both strength and ductility are high in the central
region of the stir zone. However, both strength and ductility are low on either side of the stir zone,
i.e., both the advancing and retreating sides, in the TMAZ or HAZ locations under the tool
shoulder. In some locations the ductility is below that of as-cast material. In FSP754 the mesh plots
include tensile data for the TMAZ, HAZ and base metal underneath the stir zone for locations
having depth greater than ~12.1 mm. In this rastered material the upper region of the stir zone
exhibits uniformly high strength and ductility. Uniformly high strengths persist to the bottom of the
 Materials Science Forum Vols. 503-504 165

(a)

(b)

Fig.3 (a) A montage of optical micrographs from a transverse cross section for
FSP858, and (b) the higher magnification micrographs at regions 1, 5 and 9.

(a)

(b)

Fig.4 (a) A montage of optical micrographs from a transverse cross section for
FSP754, and (b) the higher magnification micrographs at regions 3 and 5.
166 Nanomaterials by Severe Plastic Deformation

(a) (b)

Fig.5 Mesh plots of ultimate tensile stress and engineering strain for (a) FSP858 and (b)
754.

stir zone (i.e., to a depth of ~12.1 mm), while the ductility is high to a depth of ~5 mm and then
decreases with increasing the stir zone depth. Low values in the ductility mesh plot correspond to
samples containing the stir zone – TMAZ interface or samples in the HAZ. At depths beyond ~12.1
mm depth the data correspond to base metal strength and ductility.
Fig. 6 shows SEM fractography for samples having either higher or lower ductility in
FSP754. Fig. 6 (a) exhibits uniform and fine microvoids, which suggest the occurrence of ductile
fracture by microvoid formation and coalescence. This may reflect the refined g grain size shown in
Fig. 4(b) for region 3. Isolated, darker contrast features ~20 µm in size (the arrow in Fig. 6(a))
likely correspond to fractured ii particles [11]. The fractograph in Fig. 6(b) shows a crack-like
feature and a mixture of ductile and brittle fracture modes including cleavage cracking. This sample
was at region 9 and so it contained the stir zone – TMAZ boundary. The apparent cleavage
cracking most likely reflect fracture of transformation products such as martensite formed by
heating in the absence of large strain deformation during FSP.

Discussion
In this investigation, high strengths and tensile ductilities approaching 30 % elongation to failure
were observed along stir zone center lines. Tensile axes always were parallel to the direction of tool
advance. The highest ductility values were observed in multi-pass and processes involving raster
patterns. This suggests that increased strains and additional thermomechanical cycles during FSP
continue to refine microstructures and further reduce defects within the stir zone volume. The
 Materials Science Forum Vols. 503-504 167

(a) (b)
Fig.6 Fractographs for samples exhibiting (a) higher elongation, if =33 % (region 3),
and (b) lower elongation, if =3 % (region 9), in FSP754.

highest ductilities were observed in association with fully Widmanstätten-type microstructures or

fine, equiaxed g grain structures. From prior work [11], these microstructures reflect local peak stir
zone temperatures > 950 ºC, at which a high volume fraction of forms upon heating and then
transforms during subsequent cooling. Thus, within the stir zone, strength and ductility are
improved due to FSP. This reflects refined microstructures formed by severe deformation of
followed by its transformation during subsequent cooling. These results are consistent with high
combinations of strength and ductility in materials hot rolled at temperatures œ 950 ºC.
Low ductility values were observed at the stir zone – TMAZ boundary, where there is a composite
microstructures and interface in the tensile samples, and within the HAZ, where base metal is
heated but not strained. Composite microstructures would comprise a mixture of highly refined stir
zone structures, such as fine-grained g, and coarse g grains surrounded by transformation
products. The tensile behavior would be dominated by the properties of the lower strength portion.
Also, from fracture surface analysis, the lower ductilities may be attributed in part to defects and to
coarse transformation products in locations experiencing heating in the absence of deformation.
Indeed, in contrast to hot rolled material, samples subjected to annealing alone exhibited limited
strengthening and ductility values below those of base metal. Altogether, these results demonstrate
the enhanced mechanical properties associated with the thermomechanical processing of FSP but
also suggest that HAZs may be prone to reduced ductility.

Conclusions
1. The stir zone generally exhibits improved strength and ductility in comparison to base
metal.
2. Multi-pass and raster processes generally give higher strength and ductility combinations
than single-pass materials.
3. Low ductility generally coincided with mixed stir zone / TMAZ or HAZ microstructures.

Acknowledgements
The authors acknowledge the provision of FSP’ed materials by Mr. Murray Mahoney of the
Rockwell Scientific Corporation. The Naval Surface Warfare Center, Carderock, MD, supplied the
NAB material and the Defense Advanced Research Projects Agency (DARPA), with Dr. Leo
Christodolou as program sponsor, provided funding for this work.

References
1. R.S. Mishra: Advanced Materials and Processes, 2003, vol. 161(10), pp. 43-46
2. R.S. Mishra, Z.Y. Ma and I. Charit: Mater. Sci. Engng. A, 2003, vol. A341, pp. 307-10
168 Nanomaterials by Severe Plastic Deformation

3. Z.Y. Ma, R.S. Mishra and M. W. Mahoney: Friction Stir Welding and Processing II, K.V.
Jata, M.W. Mahoney, R.S. Mishra, S.L. Semiatin and T. Lienert, eds., TMS, Warrendale,
PA, 2003, pp. 221-30
4. W.M. Thomas, E.D. Nicholas, J.C. Needham, M.G. Murch, P. Templesmith and C.J. Daws:
G.B. Patent Application No. 9125978.8, December, 1991; U.S. Patent No. 5460317,
October, 1995
5. R.S. Mishra and M.W. Mahoney: Superplasticity in Advanced Materials – Proceedings of
ICSAM2000, N. Chandra, ed., Materials Science Forum, Trans Tech Publications,
Switzerland, 2001, vol. 357-59, pp. 507-14
6. P.B. Berbon, W.H. Bingel, R.S. Mishra, C.C. Bampton and M.W. Mahoney: Scripta Mater.,
2001, vol. 44, pp. 61-66
7. R.S. Mishra, M.W. Mahoney, S.X. McFadden, N.A. Mara and A.K. Mukherjee: Scripta
Mater., 2000, vol. 42, pp. 163-68
8. I. Charit and R.S. Mishra: Mater. Sci. Engng. A, 2003, vol. A359, pp. 290-96
9. Z.Y. Ma, R.S. Mishra and M.W. Mahoney: Acta Mater., 2002, vol. 50, pp. 4419-30
10. Z.Y. Ma, R.S. Mishra M.W. Mahoney and R. Grimes: Mater. Sci. Engng. A, 2003, vol.
A351, pp. 148-53
11. K. Oh-ishi and T.R. McNelley: Metal. Mater. Trans. A, 2004, vol. 35A, pp. 2951-61
12. M.W. Mahoney, W.H. Bingel, S.R. Sharma and R.S. Mishra: Mater. Sci. Forum, 2003, vol.
426-4, pp. 2843-48
13. A. Cohen, Metals Handbook, 10th Ed., vol. 2, ASM International, Metals Park, OH, 1990,
pp. 386-87
14. M.W. Mahoney, Rockwell Scientific Company, Thousand Oaks, CA, Private
Communication, April, 2004
Nanomaterials by Severe Plastic Deformation
10.4028/www.scientific.net/MSF.503-504

Enhancement of Ductility and Strength through Microstructural Refinement by FSP of Nickel

Aluminum Bronze
10.4028/www.scientific.net/MSF.503-504.161

DOI References
[8] I. Charit and R.S. Mishra: Mater. Sci. Engng. A, 2003, vol. A359, pp. 290-96
doi:10.1016/S0921-5093(03)00367-8
[11] K. Oh-ishi and T.R. McNelley: Metal. Mater. Trans. A, 2004, vol. 35A, pp. 2951-61
doi:10.1007/s11661-004-0242-1
[12] M.W. Mahoney, W.H. Bingel, S.R. Sharma and R.S. Mishra: Mater. Sci. Forum, 2003, vol. 26-4, pp.
2843-48
doi:10.4028/www.scientific.net/MSF.426-432.2843