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To cite this article: Z. Sadeghian, M. H. Enayati & P. Beiss (2011) Characterisation of in situ
Al–TiB2 nanocomposite powder synthesised by mechanical alloying, Powder Metallurgy, 54:1,
46-49
Article views: 15
Download by: [Purdue University Libraries] Date: 06 April 2016, At: 17:12
Characterisation of in situ Al–TiB2
nanocomposite powder synthesised by
mechanical alloying
Z. Sadeghian*1,2, M. H. Enayati1 and P. Beiss2
Production of in situ Al–TiB2 nanocomposite powder was studied using mechanical alloying (MA).
Two approaches were used to obtain Al–20TiB2 (wt-%) nanocomposite powder. In the first
approach the synthesis of Al–20TiB2 (wt-%) was investigated by ball milling an elemental Al–Ti–B
powder mixture. The second approach involved a double step milling procedure to achieve an
Al–20TiB2 (wt-%) composite powder. The microstructure of as milled powder particles was
investigated by X-ray diffractometry (XRD) and scanning electron microscopy (SEM). The thermal
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behaviour of MA powders was studied by differential scanning calorimetry (DSC). From these
studies it was possible to conclude that TiB2 can be formed in situ using the second approach
without the production of undesirable phases; however, the first approach tends to form an
undesirable Al3Ti intermetallic phase in addition to the TiB2 ceramic reinforcement.
Keywords: Nanocomposite powder, Al–TiB2, Mechanical alloying, Thermal stability
3 Trace (DSC) of Al–13?8Ti–6?2B (wt-%) powder obtained a as received; b as milled for 10 h; c as milled for 20 h;
from first route d Al–90TiB2 (wt-%) powder obtained by first step plus
20 h ball milling with addition of elemental Al powder
In order to evaluate the thermal behaviour of Al– 5 Patterns (XRD) of Al–62Ti–28B (wt-%) powder mixture
13?8Ti–6?2B (wt-%) powder particles obtained by the
first route, powders were heated up to 550uC in DSC. for titanium and aluminium, which indicates that no
The DSC trace exhibited two exothermic peaks at 350 solid solution formed during ball milling.
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and 450uC and a weak peak at 190uC. These are shown Figure 5c shows that the XRD peaks of elemental Ti
in Fig. 3. In comparison with the as milled powder the and Al disappeared after 20 h of milling. It should be
XRD pattern of powder after being heated to 210uC noted that no traces of the undesirable Al3Ti inter-
suggested no structural changes had taken place metallic phase were observed on the XRD pattern. The
(Fig. 4b). Therefore, the weak peak at 190uC was disappearance of the aluminium peaks can be explained
probably caused by elimination of crystal defects. The by the high lattice strain induced in the Al lattice and by
XRD pattern of the powder taken after being heated the relatively small volume fraction of aluminium
up to 400uC (Fig. 4c) revealed a new phase which could (y13 vol.-%) in the powder. Comparison of these
not be attributed to any known phase in the Al–Ti–B results with the XRD data obtained from the first route
system. This could be a metastable phase. Heating up suggests that the lower Al content in the initial powder
to 550uC resulted in the development of Al3Ti mixture promoted the formation of TiB2 in the matrix.
(Fig. 4d). Lu et al. also observed the Al3Ti phase after Lü et al. also reported that TiB2 could not be detected
annealing ball milled Al–Ti–B powder at 450uC.15 The during the ball milling of Al–Ti–B mixtures even after a
formation enthalpies of TiB2 and Al3Ti at room milling time of 40 h.15
temperature are 2323?6 and 275?31 kJ/mol respec- After 20 h ball milling, elemental aluminium powder
tively, suggesting that the Ti–B reaction is thermo- was added to the premilled Al– 62Ti–B (wt-%) powder.
dynamically more favourable than the Al–Ti reaction. Ball milling continued for another 20 h to achieve Al–
However, the presence of the large fraction of Al in the 20TiB2 (wt-%) composition. As can be seen in Fig. 5d no
initial powder mixture seems to have limited the structural change occurred in the powder except some
interdiffusion of Ti/B and therefore the formation of broadening of XRD peaks. This was attributed to the
the TiB2. refinement of crystal size and enhancement of lattice strain.
Figure 5 shows the XRD patterns of Al–62Ti–28B Figure 6a shows a typical cross-section of a final Al–
and Al–20TiB2 (wt-%) powders obtained by the second 20TiB2 (wt-%) powder particle after a total milling time
route. After 10 h of milling, peaks of TiB2 appeared on of 40 h. The EDS analysis showed that these particles
the XRD pattern (Fig. 5b). No peak shift was observed were TiB2 phase (Fig. 6b). A fine and uniform distribu-
tion of TiB2 particles within the aluminium matrix was
achieved. Higher SEM magnification of the powder
(Fig. 7) revealed that most of the TiB2 particles have a
size ranging from several nanometres to 100 nm. Only a
few particles are in the range of 500 nm to 1 mm.
The DSC trace of powder particles after a total
milling time of 40 h (Fig. 8) showed no exothermic peak
up to 550uC. Furthermore, XRD patterns taken after
the DSC run remained unchanged when compared with
that of the as milled powder (Fig. 9b). No traces of
undesirable phases such as Al3Ti were observed from
XRD patterns after heating in DSC.
These results show that by adding the aluminium in
two stages it is possible to prevent the formation of
undesirable compounds even when exposed to high
a as milled for 40 h; b after annealing in DSC up to temperatures. The resulting Al–TiB2 nanocomposite
210uC; c up to 400uC; d up to 550uC powder is expected to have good thermal stability
4 Patterns (XRD) of Al–13?8Ti–6?2B (wt-%) powder mixture during subsequent consolidation processes.
Conclusions
a as received; b final Al–20TiB2 (wt-%) powder obtained
Al–TiB2 nanocomposite material was obtained by by second route following annealing in DSC up to 550uC
mechanical alloying of elemental powders. By reducing 9 Patterns (XRD) of Al–62Ti–28B (wt-%) powder mixture
the fraction of Al in the starting powder mixture and
using a two step milling method it was possible to
produce Al–TiB2 nanocomposite while avoiding the Acknowledgements
production of an undesirable Al3Ti intermetallic com- Sadeghian’ sincere thanks go to the Deutscher
pound. The resultant Al–TiB2 nanocomposite powder Akademischer Austauschdienst (DAAD) for supporting
exhibited good thermal stability which made it suitable the project.
for subsequent consolidation.
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