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j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 1 9 5 ( 2 0 0 8 ) 321–326

journal homepage: www.elsevier.com/locate/jmatprotec

Direct laser fabrication of Ti6Al4V/TiB

F. Wang ∗ , J. Mei, Xinhua Wu


IRC in Materials, The University of Birmingham, Edgbaston B15 2TT, UK

a r t i c l e i n f o a b s t r a c t

Article history: Ti6Al4V/TiB discontinuously reinforced composites have been fabricated using direct laser
Received 14 August 2006 fabrication by injection of pre-mixed powders of TiB2 and Ti6Al4V. The microstructures have
Received in revised form 8 May 2007 been characterised by scanning electron microscopy and transmission electron microscopy
Accepted 12 May 2007 and by X-ray diffraction which show that TiB is formed during laser fabrication. The room
temperature tensile properties, including Young’s modulus of the composites, have been
measured and their tribological properties assessed using a sliding wear test. It has been
Keywords: found that the modulus, the yield and ultimate strength of Ti6Al4V are increased by the
Direct laser fabrication TiB and that the ductility is decreased. The wear resistance is significantly improved by the
Composite material borides. Post-heat treatment or HIPping improve the ductility.
TiB reinforced titanium alloys © 2007 Elsevier B.V. All rights reserved.

feeding two kinds of different powder and functionally graded


1. Introduction samples can be made by continuously changing the powder
feed rate of one or both powders.
Titanium-TiB reinforced composites have been extensively
In a recent paper Genç et al. (Genç et al., 2006) and Baner-
studied during the last few decades, because they com-
jee et al. (Banerjee et al., 2003, 2005) have discussed in detail
bine the high stiffness and strength of the boride with the
the structure of the TiB precipitates formed in laser-deposited
toughness and damage tolerance of titanium alloy matrix
Ti6Al4V–TiB composites. The mechanical properties of powder
giving increased high-temperature strength, good creep per-
metallurgy-route Ti6Al4V–TiB, which contained either ran-
formance, fatigue resistance and wear resistance. A variety
domly oriented or aligned TiB reinforcements, have been
of methods have been developed to manufacture discontin-
studied (Gorsse and Miracle, 2003b). Ocelik et al. (Ocelik et
uous composites, such as casting, powder metallurgy and
al., 2005) showed that TiB2 /Ti6Al4V layers prepared by laser
SHS (self-propagation high-temperature synthesis) technolo-
cladding show excellent wear resistance. In the present study,
gies (Gorsse et al., 1998; Gorsse and Miracle, 2003a; Zhang et
DLF has been used to manufacture discontinuously reinforced
al., 1999; Geng et al., 2003). Surface engineering has also been
composite samples by feeding pre-mixed TiB2 and Ti6Al4V
used to improve the surface properties of titanium alloys by
powder into the laser molten pool. The microstructure,
using high-energy laser or electron beams to incorporate TiB
mechanical and wear properties of the composite samples
and TiB + TiC or TiN in the surface of titanium alloys (Yun et
have been studied.
al., 2004, 2005).
During direct laser fabrication (DLF), powder is fed at a con-
trolled rate into the molten pool irradiated by the laser where 2. Experimental procedures
individual particles are melted as the movement of the laser
follows the path defined by a CAD file of a component. With The materials used in this work are TiB2 powder (>99.5%
this technology composites can be made by simultaneously purity) with particle size ranging from 5 to 50 ␮m and Ti6Al4V


Corresponding author. Tel.: +44 121 414 7892; fax: +44 121 414 7890.
E-mail address: F.wang@bham.ac.uk (F. Wang).
0924-0136/$ – see front matter © 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.jmatprotec.2007.05.024
322 j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 1 9 5 ( 2 0 0 8 ) 321–326

Fig. 1 – Secondary electron scanning micrograph of TiB2 powder and its X-ray diffraction pattern which shows diffraction
maxima corresponding only to TiB2 .

powder with particle size less than 300 ␮m. The TiB2 powder is manufactured from DLFed plates. The samples containing
too fine to be individually delivered by the powder feed system 10 wt.% TiB2 broke during machining and no tensile samples
and it was therefore pre-mixed with Ti6Al4V powder, using could be made from this composition (this work was car-
5 wt.% TiB2 and 10 wt.% TiB2 . These correspond to 1.55 wt.% ried out by an outside contractor). Some of those plates were
and 3.1 wt.% boron. A hot rolled Ti6Al4V plate of 20 mm thick thermally stress relieved by heat treating for 2 h at 600 ◦ C in
was used as a substrate, which was ground with 320 grit SiC an argon atmosphere; others were hot isostatically pressed
paper, and then degreased with acetone and ethanol before (HIPped) for 4 h at 930 ◦ C and a pressure of 103 MPa. Vickers
being used. microhardness tests were carried out using a 100 g load.
The fabrication process is carried out in an atmosphere-
controlled glove box with the oxygen kept below 5 ppm. A
ROFIN SINAR TRIAGON 1750 W CO2 laser was used which is 3. Results
operated at 1148 W CW laser, with a 12.5 cm lens, +37 mm
defocus, and 150 mm/min scan speed. A TWIN 10-COMPACT Fig. 1 shows the particle size of TiB2 powder and the X-ray
powder feeder system is used to deliver the pre-mixed pow- diffraction pattern and it is clear that all diffraction maxima
ders with a powder feed rate is 6.58 g/min via the argon are from TiB2 .
carrier gas rate at 4 L/min. The composite samples which were
produced are 4 mm × 25 mm × 50 mm. The samples were cut, 3.1. Microstructural observations on DLFed samples
mounted, ground, polished and etched, for optical, SEM and
TEM examination or for testing. Preliminary experiments were carried out in order to define
The composites were characterised using a JEOL 7000F the optimum laser processing conditions for the production of
scanning electron microscope (SEM) coupled with an Oxford homogeneous fully melted samples. Some partly melted TiB2
X-ray EDX system and PHILIPS CM-20 transmission electron
microscope (TEM). A PHILIPS Xpert diffractometer, with Cu K␣
radiation was used to obtain diffraction data.
Tribological properties were assessed using a pin-on-disc
tribometer. During pin-on-disc experiments, samples with
and without TiB reinforcement were rotated against a station-
ary hardened bearing steel ball of 6 mm diameter at a speed of
66 rpm (0.031 m/s). The nominal diameter of the wear track is
9 mm and the normal contact load was 10 N. The sliding dis-
tance used was 1000 m and tests wear conducted in air without
lubrication. The samples were 20 mm × 20 mm × 2 mm thick.
Wear resistance property is determined by measuring the
cross-section of the wear tracks with a stylus profilometer.
While the stylus is moving across the wear track, the vertical
and horizontal positions of the stylus are recorded and later
processed by Microsoft Excel so that a 2D profile of the wear
track is obtained. Wear volume loss is obtained by integrat-
ing the area across the wear scar profile, and multiplying by
the circumferential length of the track. Four measurements
are performed for each wear track and average values are Fig. 2 – Scanning electron micrograph taken using
reported. backscattered electrons from sample with 10 wt.% TiB2
Room temperature tensile specimens from the samples using 755 W laser power; shows unmelted boride and
prepared from pre-mixed powder containing 5 wt.% TiB2 were Ti6Al4V particles.
j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 1 9 5 ( 2 0 0 8 ) 321–326 323

Fig. 3 – Scanning electron micrograph taken using backscattered electrons from samples of Ti6Al4V composites containing
(a) 5 wt.% TiB2 and (b) 10 wt.% TiB2 .

particles and Ti6Al4V powders are found in the composites


where the laser power was 755 W, as shown in Fig. 2.
When the power is increased to 1148 W, in conjunction
with a scan speed of 150 mm/min and 6.58 g/min powder feed
rate, homogeneous samples are produced as illustrated in
Fig. 3. These micrographs show that needle-like borides are
distributed uniformly in the Ti6Al4V matrix for the samples
with both 5 and 10 wt.% TiB2 addition. The composite consists
of equiaxed and platelet ␣-phase and intergranular ␤-phase
rather than Widmanstatten lath-like characteristic of Ti6Al4V.
With increasing volume of boride the width and length of
borides become wider and longer (Fig. 3(b)).
Fig. 4 is bright-field TEM micrograph of a 10 wt.% TiB2
sample with the electron diffraction pattern from the boride
particle inset. This pattern shows that the borides are TiB,
rather than TiB2 . This would be expected since at this laser Fig. 5 – X-ray diffraction pattern of the Ti6Al4V/TiB
composite.

power the TiB2 is either melted by the laser or it dissolves in


the molten Ti6Al4V when it will precipitate as TiB.
X-ray diffraction was used to confirm the crystal structure
of the borides and as can be seen in Fig. 5 all the diffraction
maxima, other than those from the Ti6Al4V, correspond to TiB
(cf. Fig. 1).
Some samples were HIPped after laser fabrication and the
microstructure of a HIPped sample is shown in Fig. 6. There is
no obvious change of TiB however equiaxed ␣-phase in DLFed
Ti6Al4V/TiB matrix become coarse as judged by comparing
this image with Fig. 3(a).

3.2. Mechanical property assessment

Fig. 7 shows the tensile stress–strain curves obtained at room


temperature for DLFed Ti6Al4V and TiB/Ti6Al4V composites,
which prepared from pre-mixed powder containing 5 wt.%
TiB2 , after the different treatments indicated on the figure. The
strength of HIPped or annealed Ti6Al4V (the two lower curves)
Fig. 4 – 200 kV many beam bright-field TEM micrograph is lower than that of the HIPped or annealed Ti6Al4V/TiB sam-
from a sample of Ti6Al4V with 10 wt.% TiB2 showing TiB ples. The ductility is however better for the Ti6Al4V samples.
selected area diffraction pattern. The tensile data is summarised in Table 1.
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Table 1 – Mechanical property of Ti6Al4V/TiB composites


Sample Annealed HIPped

YS0.2 (MPa) UTS (MPa) ı (%) E-modulus YS0.2 (MPa) UTS (MPa) ı (%) E-modulus
(GPa) (GPa)

As DLFed Ti6Al4V 853 938 11.5 97 829 900 16 95


DLFed TiB/Ti6Al4V 1050 1094 6.6 138 958 1040 10.3 122

Fig. 7 – Tensile stress–strain curves of DLFed Ti6Al4V with


and without TiB reinforcement before and after heat
Fig. 6 – Scanning electron micrograph of sample of treating or HIPping.
Ti6Al4V/TiB manufactured using 5 wt.% TiB2 , after HIPping
at 930 ◦ C/100 MPa/4 h.
dimples but Ti6Al4V/TiB (Fig. 8(b)) contains both cleavage and
dimples and exhibits a mixed mode of brittle fracture and
ductile fracture.
Table 2 – Microhardness values of the Ti6Al4V with and
without TiB
3.3. Wear tests
Sample Vickers microhardness

Ti6Al4V 340 Fig. 9 is the summary of pin-on-disk wear test results. It


Ti6Al4V + 5 wt.% TiB2 560 can be seen that the sliding wear property of Ti6Al4V has
Ti6Al4V + 10 wt.% TiB2 750 been dramatically improved by adding TiB. The volume loss
of DLFed Ti6Al4V is 0.35 mm3 while the volume loss of DLFed
The microhardness values of the various samples are Ti6Al4V/TiB made using 5 wt.% TiB2 is 0.14 mm3 and the vol-
shown in Table 2. ume loss of DLFed Ti6Al4V/TiB made using 10 wt.% TiB2 is
SEM micrographs of the fracture surfaces for DLFed Ti6Al4V 0.008 mm3 .
and Ti6Al4V/TiB composite are shown in Fig. 8. The fracture The worn surfaces of DLFed Ti6Al4V and DLFed Ti6Al4V/TiB
surface of DLFed Ti6Al4V (Fig. 8(a)) mainly consists of the fine are shown in Fig. 10. It was found that noticeable debris and

Fig. 8 – SEM fractographs of (a) DLFed Ti6Al4V and (b) Ti6Al4V/TiB composite after tensile testing at room temperature.
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a contributory factor to this improved balance of proper-


ties.
The pin-on-disc experiments have shown that at the start
of sliding, the Ti6Al4V disc and the hardened bearing steel ball
contact directly and sliding through two-body wear mecha-
nism and that strong adhesion occurs between the Fe and
the Ti6Al4V which generated wear debris. This debris changes
the wear mechanism from two-body to three-body. Further
adhesion between materials attached on the hardened bear-
ing steel ball and Ti6Al4V would generate more debris from
the Ti6Al4V surface and hardened bearing steel ball surface.
The combined action of strong adhesion, abrasion and severe
plastic deformation leads to the very high and continuously
increased material loss of the Ti6Al4V.
In the case of the TiB-containing samples the worn sur-
Fig. 9 – Wear volume loss of DLFed Ti6Al4V without or with
face is dominated by micro-grooving which indicates that the
TiB reinforcement sliding distance 1000 m, and contact
wear is by three-body abrasion which is steel ball, Ti6Al4V/TiB
loads 10 N.
composite and the TiB particles pulled out during sliding pro-
cess. The wear rate is so small because the hardness has been
significantly increased by the TiB.
plough grooves occur on the worn DLFed Ti6Al4V, indicating
that the wear occurred by a combined mechanism of adhesion,
abrasion and plastic deformation. 5. Conclusions
Fig. 10(b) shows the worn surface of DLFed Ti6Al4V/TiB. It
is very different from the DLFed Ti6Al4V. There is no adhe- (1) Discontinuously reinforced Ti6Al4V/TiB composites have
sion observed because the hardness of the composite has been been successfully fabricated using direct laser fabrication
dramatically increased by adding TiB. by injection of pre-mixed powders of TiB2 and Ti6Al4V. The
composites are free of pores and cracks and the distribu-
tion of the boride is reasonably uniform.
4. Discussion (2) The Ti6Al4V/TiB composite made using 5 wt.%TiB2 main-
tains reasonable ductility coupled with slight increases in
The DLF work has shown that with the correct choice of pro-
yield strength, ultimate strength, Young’s modulus hard-
cessing parameters it is straightforward to obtain fully dense
ness and wear resistance. The properties of the DLFed
microstructures, the properties of which are only slightly
Ti6Al4V/TiB composite are slightly changed by HIPping.
changed by HIPping. The results presented in this work show
(3) The wear of the Ti6Al4V occurs by a combined mechanism
that addition of boron to produce a composite material can
of adhesion, abrasion and plastic deformation while the
lead to improvements in yield and ultimate strength, while
wear of the Ti6Al4V/TiB composite is dominated by micro-
retaining reasonable ductility and that these properties are
grooving.
coupled with increased hardness and improved wear resis-
tance. This is a significantly better balance of properties than
were obtained in similar experiments using TiC reinforcement Acknowledgements
where improved wear resistance required a very high vol-
ume fraction of TiC at which composition the ductility was The authors would like to acknowledge the financial support
zero (Wang et al., 2007). The obvious microstructural refine- of this work by EPSRC, grant no: GR/S02365/01. Thanks are also
ment associated with the presence of boron is presumably due to Prof. M.H. Loretto for useful discussion.

Fig. 10 – Wear morphologies taken by SEM using backscatter electrons (a) from a Ti6Al4V sample. (b) Ti6Al4V/TiB sample.
326 j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 1 9 5 ( 2 0 0 8 ) 321–326

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