Applied Surface Science 253 (2006) 14241430

www.elsevier.com/locate/apsusc

Microstructure study of direct laser fabricated

Ti alloys using powder and wire
Fude Wang, J. Mei, Xinhua Wu *
IRC in Materials, The University of Birmingham, Edgbaston B15 2TT, UK
Received 5 October 2005; received in revised form 30 January 2006; accepted 13 February 2006
Available online 31 March 2006

Abstract
A compositionally graded material has been fabricated using direct laser fabrication (DFL). Two types of feedstock were fed simultaneously
into the laser focal point, a burn resistant (BurTi) alloy Ti25V15Cr2Al0.2C powder and a Ti6Al4V wire. The local composition of the alloy
was changed by altering the ratio of powder to wire by varying the feed rate of the powder whilst maintaining a fixed feed rate of wire-feed. For the
range of compositions between about 20% and 100% BurTi only the beta phase was observed and the composition and lattice parameter varied
monotonically. The grain size was found to be much finer in these functionally graded samples than in laser fabricated Ti64. Some samples were
made using the wire-feed alone, where it was found that the microstructure is different from that found when using powder feed alone. The results
are discussed in terms of the power requirements for laser fabrication of powder and wire samples.
# 2006 Elsevier B.V. All rights reserved.
Keywords: Direct laser fabrication; Functionally graded materials; Microstructure and phases; Titanium alloys

1. Introduction
The concept of functionally graded materials (FGM) was
introduced in 1984 as a means for preparing thermal barrier
materials [1]. It is a class of advanced materials in which the
composition and microstructure change gradually from one
side to the other, resulting in a gradient in composition, and thus
properties.
Since then, an effort to develop high-performance heatresistant materials using functionally gradient technology has
continued. In recent years, five methods such as CVD/PVD,
powder metallurgy, plasma sprays, centrifugal casting and self
propagating combustion synthesis (SHS) [26], have been
employed to manufacture a gradient in composition for various
applications, such as chemical, biochemical and mechanical
properties. Among the FGMs, the ceramicmetal FGMs are
widely used in industry, military and aerospace. These kinds of
FGMs combine the wear and refractory properties resistance
properties of ceramics with the toughness of metals, leading to
smooth transitions in thermal stress along the thickness direction
and a minimized stress concentration at the interface. A similar

* Corresponding author. Tel.: +44 121 414 7842; fax: +44 121 414 7890.
E-mail address: X.Wu.1@bham.ac.uk (X. Wu).
0169-4332/$ see front matter # 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.apsusc.2006.02.028

concept could also apply to metal to metal functional graded

material so that different functions could be provided in different
parts of a component, e.g., a variation of wear resistance,
corrosion resistance or burn resistance at defined locations.
Direct laser fabrication (DLF) or laser engineered net
shaping (LENS) [7] is a manufacturing technique developed
about a decade ago which can directly fabricate 3-D near net
shape and fully dense components from metal powders in one
step [810]. The LENS process was developed at the Sandia
National Laboratories and was commercialized by Optomec
Design Company of Albuquerque, New Mexico while the
DLF process was developed at the Los Alamos National
Laboratories in the early 1990s. Both processes are similar in
that they used a focused laser beam as a heat source to melt
metallic powder and create a solid, three-dimensional object
[1114].
During fabrication, powder is fed at a controlled rate into the
focal point of a laser where individual particles are melted as
the movement of the laser follows the path defined by a CAD
file of a component. This technique has a great potential for
repairing components or for manufacturing individual components simply from a CAD file without any tooling. In this
study, DLF is used to investigate the feasibility of producing
compositionally graded material by feeding two different
alloys at defined, variable rates at different locations. The

F. Wang et al. / Applied Surface Science 253 (2006) 14241430

problem with this process is that low capture rate of the powder
(1030%), therefore leading to wastage of the scattered
powder if two powders are mixed with each other. In order to
overcome this problem Ti6Al4V wire has been used in the
present work as one of the feedstock, which is simultaneously
fed with a burn-resistant Ti alloy (Ti25Cr15V2Al0.2C)
powder to create functionally graded materials, in this case an
improved burn-resistance at an end of the sample. The use of
wire feeding alone to deposit one layer and several layers of
stainless steel has been reported previously [8,9]. However, it
is more difficult to melt both forms of materials without leaving
any un-melted powder or wire in the sample due to different
laser powers required for melting powder and for wire. In
addition to the technical challenge of feeding wire and powder
simultaneously, this study focused firstly on optimising the
processing conditions to avoid any un-melted powders/wires
since these can lead to low ductility of the laser fabricated
materials [10] and secondly, on understanding the microstructure of the compositionally/functionally graded material.
2. Experimental procedures
The materials used in this work are Ti6Al4V (wt.%) wire
with a diameter of 0.45 mm and a burn resistant titanium alloy
Ti25V15Cr2Al0.2C (wt.%) (BurTi) powder. The powder
was gas-atomised by Crucible Research, Pittsburgh, USA, from
an ingot produced using the plasma melter in the IRC. The
oxygen content in the atomised powder was 1900 ppm
(0.19 wt.%). A hot rolled Ti6Al4V plate of 20 mm thick was
used as substrates for all DLF work and the substrates were
ground with 320 grit SiC paper, and then degreased with
acetone and ethanol before use.
The laser used in this study was a ROFIN SINAR TRIAGON
1750 W CO2 laser. The fabrication was carried out in an
atmosphere-controlled glove box with the oxygen kept below
5 ppm. A CNC controlled wire-feed system, including a
precision wire-feed nozzle developed in-house, was used which
can deliver wires with a minimum diameter of 0.4 mm. A
TWIN 10-COMPACT powder feeder system was employed to
deliver the Ti25V15Cr2Al0.2C (wt.%) powder. Some
modification has been carried out on the powder feed system so
that the powder feed speed can be accurately controlled by the
CNC system. Fig. 1 shows the schematic of the DLF facility
used in this study for the manufacture of compositionally
graded Ti alloys using simultaneous powder and wire feed.
A Leica light optical microscope with Zeiss KS 300 software
has been used to measure the grain size distribution in the
samples. A PHILIPS XL 30 scanning electron microscope interfaced to an Oxford Instruments X-ray EDX analytical system was
used for microstructural and compositional analysis. A Philips
Xpert X-ray diffractometer was used to measure the lattice
parameters of the samples at different positions along their length.
Several thin wall samples with a width of 20 mm, a thickness
of 2 mm and a height of 42 mm were built. The laser power
used in this work was 755 W and the laser scan speed was
100 mm/min. The burn-resistant titanium alloy powder was fed
at a rate varying from a nominal minimum of 2.64 g/min to a

1425

Fig. 1. Schematic of direct laser fabrication facility with simultaneous powder

and wire feed.

nominal maximum of 18.21 g/min whilst the Ti6Al4V wire

feed was kept at a constant rate of 0.4 g/min. For a sample with
a total height of 42 mm eleven compositional variations were
assigned during the fabrication. For the purpose of providing a
wetting or bonding of the sample to the substrate, only the burnresistant titanium alloy powder was fed to the laser focal point
at a powder feed rate of 2.64 g/min until a height of 2 mm was
achieved. Above a height of 2 mm, the fabrication of
compositionally graded material actually begins. From 2 to
6 mm high, only Ti6Al4V wire was fed to the laser focal
point at a feed rate of 0.4 g/min. From 6 mm high, at every
4 mm increment the powder feed rate was changed automatically by the CNC program and at the same time the wire
feed rate was kept at a feed rate of 0.4 g/min until reaching a
height of 38 mm. During the fabrication of the last 4 mm, the
wire feed was stopped and only BurTi powder was used. In order
to gain more insight into the process when the feed conditions are
changed, some experiments were also carried out in which only
wire or powder was fed into the laser. Clearly from the known
feed rates of the two alloys the nominal composition of the
resultant alloy can be calculated based on the assumption that
100% of the powder is melted. For example, for a powder feed
rate of 2.64 g/min for BurTi and Ti6Al4V wire feed rate at
0.4 g/min the ratio of Ti:V:Cr:Al would be 79:13:5:3 (wt.%) if
100% of the powder and wire were melted and became part of the
build. The actual measurements of the alloy composition along
the height of the sample (obtained by EDX) can be compared
with this calculated composition so that the efficiency of powder
capture can be calculated.
The samples were ground and polished longitudinally for
microstructural examination. Within each composition variation, a sample was cut for X-ray diffraction analysis. The
composition in each section was measured by EDX.
3. Results and discussion
3.1. DLF only using wire as feedstock
Optical and SEM micrographs of laser fabricated samples
of Ti6Al4V only using wire as a feedstock are shown in Fig. 2.

1426

F. Wang et al. / Applied Surface Science 253 (2006) 14241430

Fig. 2. Microstructural and diffraction data of DLFed Ti64 wire samples: (a) macrostructure of DLFed Ti6Al4V wire, (b) SEM low magnification of DLFed Ti64
wire, (c) SEM high magnification of (b) and (d) comparison of X-ray diffraction pattern of annealed Ti64 commercial bar and DLFed Ti64 wire.

The morphology of DLFed Ti6Al4V using wire as feedstock is

dominated by columnar grains (Fig. 2(a)) which is similar to
that obtained using powder [15,16]. However, microstructural
examination shows that the DLFed samples made from wire
consists of Widmanstatten structure (Fig. 2(b and c)) rather than
martensite as was observed when using powder as feedstock
[17]. X-ray diffraction has been used to determine the lattice
parameter of laser fabricated Ti6Al4V made from wire
feedstock and the observations compared with those obtained
from annealed Ti6Al4V commercial bar feedstock. Fig. 2(d)
shows the peaks for (0 0 0 1) and {10  11} planes where it can
be seen that there is no significant difference between the lattice
parameters of DLFed sample made from wire feedstock of
Ti6Al4V and the annealed Ti6Al4V commercial bar feedstock.
This observation contrasts with that obtained when using
DLFed Ti6Al4V microstructure using powder feedstock where
it was found that the {10  11} peak of the DLFed sample
shifts to the right (i.e., to a larger angle) of the annealed
Ti6Al4V [17]. The change in the lattice parameter of DLFed
Ti6Al4V powder is consistent with that reported in water
quenched material where martensite is formed [18].
Martensite in Ti6Al4V is formed when the cooling rate is
larger than about 410 8C/s [19]. In the laser processing of
Ti6Al4V wire, three times the laser power is needed to melt the
wire than is required for melting the powder. It is thus expected
that the overall temperature of the DLFed sample produced
from wire will be kept high and the cooling rate in such a
sample could be much lower than that in samples produced

from powder. It is therefore understandable that no martensite is

formed in DLFed wire Ti6Al4V samples.
3.2. Functionally graded samples
A compositionally graded thin wall sample built using laser
fabrication with Ti6Al4V wire and BurTi powder fed
simultaneously is shown in Fig. 3. The bright colour near

Fig. 3. Optical photograph showing the morphology of the compositionally

graded thin wall sample fabricated at laser power of 755 W, laser scan speed of
100 mm/min. The powder and wire feed rates are indicated in the Fig. 4. The
bright colour shows where Ti6Al4V composition dominates.

F. Wang et al. / Applied Surface Science 253 (2006) 14241430

Fig. 4. BurTi powder and Ti6Al4V wire feed rates used for the fabrication of
the compositionally graded thin wall sample shown in Fig. 2.

1427

the bottom of the sample is due to the etching response of

Ti6Al4V. The powder feed rate at a series of heights in the
sample is shown in Fig. 4. In this sample, the Ti64 wire feed rate
was kept constant and the powder feed rate of BurTi was
increased incrementally every 4 mm from 0 g/min at the sample
height of 2 mm to 18.8 g/min at the height of 38 mm.
Fig. 5 shows that equiaxed grains dominate in the entire
sample and the grain size gradually decreased with an increase
of the BurTi powder feed rate, i.e., from the bottom to top of the
sample although elongated grains were observed between 2 and
16 mm height. There is an obvious change from columnar
grains, typical of Ti64 when produced by DLF, to equiaxed
grain structure for the minimum content, 20 wt.%, of BurTi
addition investigated. The optical microstructure of the sample
produced by mixing Ti6Al4V wire and BuRTi powder is shown
in Fig. 5. The morphology obtained in the compositionally
graded sample is very different from that in laser fabricated
Ti6Al4V samples reported previously, where epitaxial growth
normally prevails [15,16]. However, the microstructure is
similar to the morphology obtained in laser fabricated BurTi

Fig. 5. Optical microstructure of FGM deposit showing that the grain size is reduced with increasing BurTi powder feed rate at a laser power of 755 W and 100 mm/
min scan speed: (a) Ti6Al4V wire, (b) 4.88 g/min BurTi powder with 0.4 g/min Ti6Al4V wire, (c) 11.36 g/min BurTi powder with 0.4 g/min Ti6Al4V wire,
(d) 16.34 g/min BurTi powder with 0.4 g/min Ti6Al4V, (e) 18.8 g/min BurTi powder with 0.4 g/min Ti6Al4V, (f) 18.8 g/min BurTi powder only.

1428

F. Wang et al. / Applied Surface Science 253 (2006) 14241430

Fig. 6. Grain size distribution obtained from different locations in the FGM deposit: (a) 2.64 g/min BurTi powder with 0.4 g/min Ti6Al4V wire, (b) 6.58 g/min
BurTi powder with 0.4 g/min Ti6Al4V wire, (c) 13.85 g/min BurTi powder with 0.4 g/min Ti6Al4V, (d) 18.8 g/min BurTi powder with 0.4 g/min Ti6Al4V, (e)
18.8 g/min BurTi powder only, (f) average grain size distribution of the FGM sample.

samples, although the grain size in 100% BurTi samples is

much smaller [20,21] than in the compositionally graded Ti64
BurTi samples in Fig. 5. Note that at the bottom of the samples
obtained in the previous work [20,21] there are about 1 mm
long elongated grains at the bottom of the BurTi sample, which
is due to a higher cooling rate near the bottom of a sample under
previous experimental condition where the laser power was
much smaller. Fig. 6 shows the grain size distribution measured
using an image analysis system obtained from at least 210
different grains in a given section of the sample. Fig. 6(f) shows
how the average grain size decreases continuously with an
average size of 175 mm at a BurTi powder feed rate of 2.64 g/
min near the bottom of the sample to 68 mm at a BurTi powder
feed rate of 18.8 g/min. This average grain size of BurTi at a
feed rate of 18.8 g/min after the Ti6Al4V wire feed interrupted
was found to be 51 mm.
Fig. 7 shows composition distributions of the main
elements measured using EDX along the height of a compositionally graded sample. From Fig. 7, it is evident that the
vanadium and chromium gradually increase and aluminium
and titanium gradually decrease with increase of the BurTi
powder feed rate as expected from the compositions of the

two alloys. The level of alloying elements at which the grain

structure changes from columnar to equiaxed can be estimated from this graph since this change occurs at about a build
height of 10 mm (cf. Fig. 5(b)). The V content is about 10%,

Fig. 7. EDX measurements of the composition of a DLFed sample along the

height of the FGM thin wall. These measured compositions can be used to
assess the efficiency of the incorporation of powder during laser fabrication
since the actual feed rate of powder and wire are known.

F. Wang et al. / Applied Surface Science 253 (2006) 14241430

1429

Fig. 8. X-ray diffraction (XRD) spectrum at different positions of FGM thin wall sample made by DLF with BurTi powder and Ti64 wire at the following feed rates:
(a) 2.64 g/min BurTi powder with 0.4 g/min Ti6Al4V wire, (b) 6.58 g/min BurTi powder with 0.4 g/min Ti6Al4V wire, (c) 18.8 g/min BurTi powder only, (d)
compare (c) with (a and b) and (e) the shift of 2u of b(1 1 0) and the change of lattice parameter a.

the Al content about 2.5% and the Cr content about 2% and it

is clear that the change to an equiaxed grain structure is
associated with a significant changes from the composition of
Ti64. This implies that about 10% of the powder is
incorporated into the build.
In order to assess whether there were any changes of crystal
structure in the compositionally graded sample, produced by
varying the powder feed rate, typical X-ray diffraction results
are shown in Fig. 8. It is evident that the lattice parameter of
compositionally graded material decreases gradually with
increasing the amount of BurTi. The sudden reduction of the
lattice parameter toward the top of the sample is attributed to
the fact that the top is 100% BurTi.
The results of X-ray diffraction has also shown that there is
no new phase formed from mixing BurTi and Ti6Al4V within
the range of mixing ratios studied here although the Bragg
angle (and corresponding interplanar spacing) of b phase
changes with the change of composition or mixing ratio.

From previous work [16], it has been found that during laser
fabrication Ti64 tends to grow on the previous layer and
nucleation in the newly deposited layer occurs only under some
specific conditions whereas in laser fabricated BurTi nucleation
normally takes place in every layer of the deposition. It is
perhaps surprising that a small amount of BurTi would change
the solidification mechanism completely in the Ti6Al4V from
epitaxial growth and thus a columnar microstructure, to
nucleation dominating in the deposition so that equiaxed grains
form. However, it should be noted that the minimum amount
of BurTi used in these experiments corresponds to a significant
change in alloy composition.
4. General discussion
The results presented in this paper have shown that the use
of wire as one of the feedstock material is a practical way
forward for the manufacture of functionally graded alloys. The

1430

F. Wang et al. / Applied Surface Science 253 (2006) 14241430

fact that only about 10% of the BurTi powder that was fed into
the laser was incorporated into the build emphasises the waste
of powder that would occur if two powders were used. If wire is
used it should be possible to re-use most of the unused powder.
The complex interplay between alloy composition, cooling
rate and thermal cycles makes it very difficult to predict the
microstructure of alloys prepared in this way. Further work is
underway in which detailed thermal histories will be measured
experimentally and used to validate modelling of the process so
that thermal histories over a wide range of conditions can be
predicted. This should allow the development of microstructures and the formation of equilibrium and non-equilibrium
phases to be understood so that properties of functionally
graded materials can be controlled.
5. Conclusions
1. When wire feedstock is used for laser fabrication, the power
requirements to produce fully dense samples are increased
above that when using powder. This higher power leads to
higher temperatures and slower cooling so that in contrast to
powder samples no martensite is formed.
2. Simultaneous feed of powder and wire allows successful
production of functionally graded samples.
3. The changes in microstructure observed along the lengths of
functionally graded samples are similar to those expected
from the imposed changes in composition, although the
change from the columnar grains in pure Ti6Al4V when
DLFed to equiaxed grains shows that addition of the BurTi
alloy to Ti6Al4V changes the way in which solidification
occurs at relatively low concentrations.
Acknowledgements
The authors would like to acknowledge the financial support
of this work by EPSRC, grant no.: GR/S02365/01. Thanks are
also due to Prof. M.H. Loretto for useful discussions.
References
[1] M. Koizumi, FGM activities in Japan, Compos. Part B: Eng. 28 (1997) 14.
[2] Y. Watanabe, T. Nakamura, Microstructures and wear resistances of
hybrid Al-(Al3Ti + Al3Ni) FGMs fabricated by a centrifugal method,
Intermetallics 9 (2001) 3343.

[3] H. Guo, K.A. Khor, Y.C. Boey, X. Miao, Laminated and functionally
graded hydroxyapatite/yttria stabilized tetragonal zirconia composites
fabricated by spark plasma sintering, Biomaterials 24 (2003) 667675.
[4] J.F. Groves, H.N.G. Wadley, Functionally graded materials synthesis via
low vacuum directed vapor deposition, Composites Part B 28B (1997) 57
69.
[5] Y.-M. Lim, Y.-J. Park, Y.-H. Yun, K.-S. Hwang, Functionally graded Ti/
HAP coatings on Ti6Al4V obtained by chemical solution deposition,
Ceram. Int. 28 (2002) 3741.
[6] E.M. Heian, J.C. Gibeling, Z.A. Munir, Synthesis and characterization of
Nb5Si3/Nb functionally graded composites, Mater. Sci. Eng. A368 (2004)
168174.
[7] M.L. Griffith, L.D. Harwell, J.A. Romero, M.E. Schlienger, C.L. Atwood,
J.E. Smugeresky, Multi-material processing by LENSTM, in: Proceedings
of the Solid Freeform Fabrication Symposium, Austin, TX, 1997.
[8] W. Ul Haq Syed, A.J. Pinkerton, L. Li, A comparative study of wire
feeding and powder feeding in direct diode laser deposition for rapid
prototyping, Appl. Surf. Sci 247 (2005) 268276.
[9] W. Ul Haq Syed, A.J. Pinkerton, L. Li, Effects of wire feeding direction
and location in multiple layer diode laser direct metal deposition, Appl.
Surf. Sci 248 (2005) 518524.
[10] J. Liang, Direct laser fabrication of titanium alloy powders, Ph.D. thesis,
University of Birmingham, UK, 2005.
[11] K.I. Schwendner, R Banerjee, P.C. Collins, C.A. Brice, H.L. Fraser, Direct
laser deposition of alloys from elemental powder blends, Scr. Mater. 45
(2001) 11231129.
[12] R. Banerjee, P.C. Collins, A. Genc, H.L. Fraser, Direct laser deposition of
in situ Ti-/6Al-/4V-TiB composites, Mater. Sci. Eng. A358 (2003) 343
349.
[13] S. Das, T.P. Fuesting, G. Danyo, L.E. Brown, J.J. Beaman, D.L. Bourell,
Direct laser fabrication of superalloy cermet abrasive turbine blade tips,
Mater. Des. 21 (2000) 6373.
[14] W. Liu, J.N. DuPont, Fabrication of functionally graded TiC/Ti composites by laser engineered net shaping, Scr. Mater. 48 (2003) 13371342.
[15] X. Wu, J. Mei, Near net shape manufacturing of components using direct
laser fabrication technology, J. Mater. Process. Technol. 135 (2003) 266
270.
[16] X. Wu, J. Liang, J. Mei, C. Mitchell, P.S. Goodwin, W. Voice, Microstructures of laser-deposited Ti6Al4V, Mater. Des. 25 (2004) 137144.
[17] L. Qian, J. Mei, J. Liang, X. Wu, Influence of position and laser power on
thermal history and microstructure of direct laser fabricated Ti6Al4V
samples, Mater. Sci. Technol. 21 (2005) 597605.
[18] L. Zeng, T.R. Bieler, Effects of working, heat treatment, and aging on
microstructural evolution and crystallographic texture of a, a0 , a00 and b
phases in Ti6Al4V wire, Mater. Sci. Eng. A 392 (2005) 403414.
[19] T. Ahmed, H.J. Rack, Phase transformations during cooling in a + b
titanium alloys, Mater. Sci. Eng. A 243 (1998) 206211.
[20] X. Wu, R. Sharman, J. Mei, W. Voice, Microstructure and properties of a
laser fabricated burn-resistant Ti alloy, Mater. Des. 25 (2004) 103109.
[21] X. Wu, R. Sharman, J. Mei, W. Voice, Direct laser fabrication and
microstructure of a burn-resistance Ti alloy, Mater. Des. 23 (2002)
239247.