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Materials Science and Engineering A 528 (2011) 4849–4855

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Materials Science and Engineering A


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Effect of Al content on porous Ni–Al alloys


H.X. Dong a , Y.H. He a,∗ , Y. Jiang a , L. Wu a , J. Zou b,∗∗ , N.P. Xu c , B.Y. Huang a , C.T. Liu d
a
State Key Laboratory for Powder Metallurgy, Central South University, Changsha, Hunan 410083, PR China
b
Materials Engineering and Centre for Microscopy and Microanalysis, The University of Queensland, Brisbane, QLD 4072, Australia
c
Membrane Science and Technology Research Center, Nanjing University of Technology, Nanjing 210009, PR China
d
Department of Mechanical Engineering, The Hong Kong Polytechnic University, Hong Kong, China

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

Article history: Porous Ni–Al alloys with different nominal compositions ranging from Ni–10 wt.% Al to Ni–40 wt.% Al
Received 2 June 2010 were fabricated through reactive synthesis of Ni and Al elemental powders. It had been found that the
Received in revised form 30 January 2011 volume expansion, maximum pore size and permeability of porous Ni–Al alloys increased with increasing
Accepted 4 February 2011
the Al content, indicating that the nature of the pores can be manipulated through changing the Al
Available online 23 February 2011
content. In addition, detailed structural characterizations showed that the fabricated porous Ni–Al alloys
can have three crystalline phases (i.e., Ni3 Al, NiAl, and Ni2 Al3 ) when using different compositions, in good
Keywords:
agreement with the Ni–Al phase diagram. Mechanical strength tests of the fabricated porous Ni–Al alloys
Ni–Al intermetallics
Porous material
were also performed. Both of the bending strength and tensile strength of porous Ni–Al alloys were in
Mechanical properties the range of 5–80 MPa, and decreased with increasing the Al content.
Reactive synthesis © 2011 Elsevier B.V. All rights reserved.

1. Introduction ␣-Al2 O3 around their external and internal surfaces at high tem-
peratures [17,18] and since the porous Ni–Al alloys also show good
Most of the Ni–Al alloys are of great interest for more than two corrosion resistance to the acid/alkaline solution [19], the porous
decades as a potential high temperature structural material due to Ni–Al alloys may have major applications in various environments,
their outstanding engineering performances, such as low density, such as high temperature and severe rugged environment, due to
high melting point, excellent acid/alkali corrosion resistance, good their good physical and chemical properties.
oxidation resistance at elevated temperatures as well as good ther- In order to extend the potential applications of porous Ni–Al
mal conductivity [1,2]. However, the major barrier for Ni–Al alloys alloys, it is necessary to produce porous Ni–Al alloys with different
to be suitable in the structural applications is its low ductility at pore structures. Although the Al content has great influence on pore
the ambient temperature and low strength and creep resistance at structures for Al-containing porous intermetallic alloys [15,20], it
elevated temperatures [3]. is not clear how the Al content affects the pore structure in the
On the other hand, porous metals have showed their wide porous Ni–Al alloys. Furthermore, very few study on the mechanical
applications in various fields, such as seawater desalination [4], properties of porous Ni–Al alloys has been reported, which may
environmental protection [5,6], pharmaceuticals’ separation [7], limits the practical applications of the porous Ni–Al alloys.
metallurgy [8], energy storage [9] and chemical engineering In this study, porous Ni–Al alloys with different Al content were
[10,11]. Porous Ni–Al intermetallics have been produced from produced by the powder metallurgy, and the effect of the Al content
Ni + Al powder compacts by combustion synthesis [12]. However, on porous Ni–Al alloys was systematically investigated with a wide
a major difficulty of this synthesis technique is to prevent the range of the Al contents (between Ni–10.7 wt.% Al (20.6 at.% Al) and
shape alternation of the green compacts [13,14]. Recently, the Ni–40 wt.% Al (60 at.% Al)). The influence of the Al content on the
porous Ni–Al alloys with its original shape have been successfully phases and pore structures were investigated. Since bending and
fabricated through the step sintering reaction synthesis method tensile strength are the most representative processes to deform
[13,15,16]. Since porous NiAl intermetallic compounds have excel- the porous structures, the bending and tensile properties of porous
lent oxidation and corrosion resistances owing to the formation of Ni–Al alloys with 10.7–40 wt.% Al were also measured.

2. Experimental
∗ Corresponding author. Tel.: +86 731 88836144; fax: +86 731 88710855.
∗∗ Corresponding author. Tel.: +61 7 33463195; fax: +61 7 33463993. The raw materials were 99.8% purified Ni powders and 99.9%
E-mail addresses: donghx20004@163.com (H.X. Dong), yuehui@mail.csu.edu.cn purified Al powders with the average particle size of 35–40 ␮m
(Y.H. He), j.zou@uq.edu.au (J. Zou). with the nominal compositions varied from Ni–10.7 wt.% Al to

0921-5093/$ – see front matter © 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2011.02.014
4850 H.X. Dong et al. / Materials Science and Engineering A 528 (2011) 4849–4855

♦ Al ♦ ∇ Ni3Al
100 a • Ni Δ Ni2Al3
Axial expansion

Radial expansion • Δ
Δ Δ • Δ Δ
Volume expansion f) Δ Δ ♦ •♦ ♦
80 Δ
Expansion ratio / %

e)
60

Intensity
d)
40 ∇
c) ∇ ∇ ∇ ∇

20 b)

a)
0
10 15 20 25 30 35 40
0 10 20 30 40 50 60 70 80 90
Al content / wt%
2θ (°)
Fig. 1. The volume expansion of porous Ni–Al alloys as a function of Al content.

b
Ni–40 wt.% Al, in order to gain a systematic understanding of the
relationship between the fabricated pore structures and the Al con- ♣ NiAl3
tents. The Ni and Al powders were firstly blended in a cylinder mixer
for 8 h, followed by the cold die pressing (under 200 MPa) into com-
pact discs with a dimension of ∅26 mm × 2 mm. No lubricant was
added in the mixture in order to prevent the sample and environ- Intensity
ment from pollution. The green compact discs were then sintered

in a vacuum furnace with a vacuum pressure of 10−3 Pa. To pre- ♣
♣ ♣
serve the original shape of the compact discs, a slow heating rate of ♣
3 ◦ C/min was employed and the compact discs were hold at 600 ◦ C
for 4 h before heating to the final sintering temperature in order to
avoid the residual overmuch liquid Al metal (otherwise a strenuous
reaction between liquid Al and Ni may take place and may destroy
the shape of the discs, when the sintering temperature is beyond
the Al melting point) [13]. The final sintering temperature was set 10 15 20 25 30
to be 1100 ◦ C, determined by the Al–Ni binary phase diagram. The 2θ (°)
final sintering was performed for 3 h to obtain homogeneous phase
structure. For each of the measurements performed in this study, 3 Fig. 2. (A) The XRD analysis of Ni–Al alloy with different Al content sintered at
560 ◦ C: (a) 10.7 wt.%, (b) 14 wt.%, (c) 16.6 wt.%, (d) 24 wt.%, (e) 32 wt.%, (f) 40 wt.%;
discs were used to minimize the measurement errors. (B) the magnification of (f) in (A) in the diffraction angle range 10–30.
The sintered discs with different nominal compositions were
characterized by X-ray diffraction (XRD: Dmax 2500VB) to identify
the crystalline phases in the porous Ni–Al alloys. The disc dimen- expansion behaviors are similar to the volume expansion, and their
sions before and after the sintering were measured to determine maximum expansion ratios (at the Al content of 40 wt.%) are mea-
their volume expansion. The pore structure was characterized by sured to be ∼28% and ∼24%, respectively. It should be noted that,
scanning electron microscopy (SEM: JEOL JSM-7000F). The open under such huge expansion ratios, the original shape of the com-
porosity was measured by the Archimedes method [21]. The per- pact discs was still preserved. It is in a strong contrast with compact
meability and pore size were measured on a BTP-III porous material discs produced by conventional reaction synthesis [23], where the
test instrument. green compact discs always shrunk, distorted and even collapsed
Bending strength and tensile strength tests were performed extensively with increasing the Al content. Our results indicate
using an Instron Universal Testing Machine (Model LJ-3000A) that compact discs with controllable shape can be in fact obtained
under the condition with a crosshead speed of 1.0 mm/min. The through the step sintering process.
strength testing samples were cut into a shape with the dimension
of 15 mm × 3 mm × 3 mm for the mechanical tests. 3.2. Phase transformation and identification with different Al
contents
3. Results and discussion
The phase transformation during sintering varied with different
3.1. Effect of the Al content on the volume expansion sintering temperature. Fig. 2(A) shows XRD patterns taken from
compact discs sintered at 600 ◦ C with different Al contents. Several
The volume expansion during the step sintering procedure for intermediate phases, such as Ni2 Al3 , NiAl and Ni3 Al phases, co-exist
Ni–Al alloy system is one of the most remarkable phenomena with elemental Ni and Al phases in these compacts. Since 600 ◦ C
[15,22]. Fig. 1 shows the plot of measured the volume and dimen- is below the Al melting point, the formation of the intermediate
sion expansion ratios of the porous Ni–Al alloys sintered at 1100 ◦ C phases must be due to the interdiffusion and reaction of Al and Ni
for 3 h as a function of the Al content. As can be seen, the volume in solid form. These XRD data suggests that holding at 600 ◦ C for 4 h
and expansion ratios increase with increasing the Al content. At during sintering has provided sufficient time for solid diffusion and
the Al content of 40 wt.% (the maximum expansion), the volume reaction, so that the formation of intermediates becomes possible.
expansion ratio was measured to be ∼95%. The axial and radial In Fig. 2(A), it is clearly shown that, with increasing the Al content,
H.X. Dong et al. / Materials Science and Engineering A 528 (2011) 4849–4855 4851

ο
• Ni ♦ Ni3Al
a ο ο Ni2Al3
ο
ο ο ο
ο ο ο
f) ο ο ο ο ο ο

ο
e) ♦ •
Intensity

d) ♦ ο

c) ♦ ♦

b)

♦ • •
a) ♦ ♦ ♦ ο

0 10 20 30 40 50 60 70 80 90
2θ (°)

ο ο Ni2Al3
b • NiAl ∇ Ni3Al

ο ο ο Ni2Al3
d) ο ο ο ο
ο ο ο

Intensity

• •
NiAl
c) •
• •
∇ Ni3Al+NiAl
• ∇ ∇ •
b) • •

a) ∇ ∇ Ni3Al
∇ ∇

0 10 20 30 40 50 60 70 80 90
2θ (°)

Fig. 3. (A) The XRD analysis of Ni–Al alloys with different Al content sintered at
750◦ C: (a) 10.7 wt.%, (b) 14 wt.%, (c) 16.6 wt.%, (d) 24 wt.%, (e) 32 wt.%, (f) 40 wt.%;
(B) XRD patterns showing different crystalline phases formed in final sintered Ni–Al
alloys with different Al content: (a) 14 wt.%, (b) 16.6 wt.%, (c) 32 wt.%, (d) 40 wt.%.

the diffraction peak of Ni2 Al3 become stronger, indicating that the
amount of the Ni2 Al3 phase increases with increasing the Al con-
tent. To understand this phenomenon, we note that the higher the
Al contents, the larger the contacting surface area between Ni and
Al powders. In fact, the higher contacting surface area promotes
the solid interdiffusion reaction, so that more Ni2 Al3 phases can be Fig. 4. Cross-sectional structures of Ni–14 wt.% Al alloy sintered at (a) 600 ◦ C, (b)
obtained. It is of interest to note that, during sintering, generally the 750 ◦ C and (c) 1100 ◦ C.
NiAl3 phase should be the first phase to be generated from the reac-
tion between elemental Al and Ni in the Ni/Al system [24]. However,
NiAl3 only can be detected in the Ni–40 wt.% Al discs after sintered the Al diffraction peak in the compact discs is the result of extensive
at 600 ◦ C for 4 h (see Fig. 2(B)). Since the Ni2 Al3 phase is formed due reaction around Al melting point to form intermediates [23]. It is of
to the reaction between the NiAl3 phase and Ni [25], the fact that interest to note that the intensity of the Ni diffraction peak becomes
the NiAl3 phase was hardly found in our cases suggests that signif- weaker with increasing the Al content and disappears when the Al
icant reactions and subsequent phase transformations have taken content reaches to 40 wt.%. Furthermore, the same trend can be
place. In addition, the fact that no NiAl3 phase was observed in the found for the Ni3 Al phase. These evidences suggest that, when the
XRD patterns for the compact discs with the Al content lower than sintering beyond the Al melting point, severe reactions between
40 wt.% may be due to their small concentration, which is beyond remaining Al with remaining Ni and the Ni3 Al phase take place,
the XRD detectability. which eventually leads to the formation of Ni2 Al3 phase.
Fig. 3(A) illustrates the XRD patterns of compact discs sintered Fig. 3(B) is XRD patterns of compact discs finally sintered at
at 750 ◦ C (the discs were cooled when the sintering temperature 1100 ◦ C for 3 h with different Al contents. As can be seen, 3 different
reached 750 ◦ C – no holding was carried out) with different Al con- phases were found in four Al contents, namely, Ni3 Al phase found in
tents. Multiple phases, such as Ni3 Al, Ni2 Al3 and remaining Ni can the Ni–14 wt.% Al alloy, Ni3 Al and NiAl phases in the Ni–16.6 wt.%
be found in these samples. It should be noted that the Al diffraction Al alloy, NiAl phase in the Ni–24 wt.% Al and Ni–32 wt.% Al alloy
peak has disappeared, while the Ni diffraction peak persisted in and single Ni2 Al3 phase in the Ni–40 wt.% Al alloy. In addition, for
almost all the samples except Ni–40 wt.% Al. The disappearance of the cases of Ni–14 wt.% Al, Ni–24 wt.% Al and Ni–40 wt.% Al alloys,
4852 H.X. Dong et al. / Materials Science and Engineering A 528 (2011) 4849–4855

a example as it is the most classical composition in the Ni–Al alloys.


Porosity of green compacts Fig. 4 shows typical BSE images of the Ni–14 wt.% Al alloy sin-
60 porosity of sintered compacts
tered at 600, 750 and 1100 ◦ C, respectively. Fig. 4(a) shows that
porosity formed during sintering procedure
the pores (black area), Al particles (gray area), intermediate phases
50 around the Ni particles (light area) coexist in the compacts after sin-
tering at 600 ◦ C. When the sintering temperature reaches 750 ◦ C,
Open porosity / %

Al disappeared leaving pores (black area) behind (Fig. 4(b)). The


40
porosity (black area in the image) increases when the temper-
θro=0.83CAl+8.33
2
ature rises from 600 ◦ C to 750 ◦ C, indicating the consumption of
30 R =0.9642 Al plays a very important role in the formation of porosity. From
Fig. 4(b), it is clear that the intermediates (gray area) exist in the
place between the pores and remaining Ni, indicating that Al dif-
20
fuses into the Ni powders to form the intermediates. After sintering
at 1100 ◦ C for 3 h, a single phase coexists with pores, as shown in
10 Fig. 4(c).
10 15 20 25 30 35 40
Al content / wt% 3.3. Effect of the Al content on the pore structures

b 70
As shown earlier, the Al content can affect the volume expansion
3500
60 of sintered porous Ni–Al alloys dramatically, from which it is antici-
3000 Permeability / m3m-2KPa-1h-1 pated that the Al content can also have a great influence on the pore
50
Maximum pore size / μm

structure in these porous alloys. Since the pore structures are crit-
2500
40 ically important for them to be practically useful, it is important to
2000
understand the variation of the pore structures as a function of the
30
Al content. Three key parameters, such as open porosity, the max-
20 1500 imum pore size and gas permeability, are measured to determine
the pore structures of our porous Ni–Al alloys.
10 1000 Fig. 5(a) shows the variation of open porosity in compact discs
0 and porosity formed during sintering as a function of the Al content.
500
The open porosity in the compact discs decreases almost linearly
-10
0 with increasing the Al content. This is because the Al powders can
-20 be easily distorted to fill in the clearance pores in the compact discs
10 15 20 25 30 35 40
during the cold pressing. Similar to the relationship between the
Al content / wt% volume expansion and the Al content, both the open porosity in the
final sintered compact discs and porosity formed during sintering
c increase almost linearly with increasing the Al content, indicating
3500
that the pores have great dependence upon the content of Al pow-
3000 ders during the reactive sintering procedure. This is in accordance
-1 -1
Permeability / m m KPa h

Experimental data with the pore formation mechanism during the elemental pow-
2500
Linear fit der metallurgy [26]. The relationship between the open porosity
-2

2000 ( ro ) generated (Fig. 5(a)) during the sintering procedure and the
3

Al content (CAl ) can be obtained through fitting the experimental


1500
data (refer to Fig. 5(a)):
1000
R =0.97
ro = 0.83CAl + 8.33 (R2 = 0.9642) (1)
500
Since the diffusion rate of Al is significantly larger than that of Ni
0 [27], the net movement and Al consumption must be balanced by
the opposite net vacancy flux, which will result in a large number
0 500 1000 1500 2000 2500
of vacancies near the original positions of Al atoms (see Fig. 4(a)).
dm2θ / μm2 As a consequence, the pores are generated from the exhaustion of
the Al powders in the compact discs. For this reason, the high the Al
Fig. 5. Effect of Al content on the pore parameters of porous Ni–Al alloys: (a) open
porosity, (b) maximum pore size and gas permeability and (c) the relationship of
content, the higher the porosity. In this study, the maximum open
porous Ni–Al alloy parameters. porosity can be found in the porous Ni–40 wt.% Al alloys and has
been determined to be ∼55%.
Permeability and maximum pore size are the important
properties for flow-through foam applications, such as thermal
single Ni–Al phase can be achieved in each case. These phenomena applications [29], filtration [30], acoustic absorption [31], and
can be well understood through the Ni–Al binary phase diagram porous implants [32]. Accordingly, these parameters were inves-
as these compositions match with the compositions of the Ni3 Al, tigated. Fig. 5(b) shows the permeability and maximum pore size
NiAl and Ni2 Al3 phases. This result suggests that all intermediate of the porous Ni–Al alloys as a function of the Al content. It
phases formed at low sintering temperatures can be transformed shows the linear relationship between the Al content and the
into their corresponding final phases by further sintering, particular maximum pore size. Moreover, the gas permeability increases
at 1100 ◦ C for a period of 3 h. sharply with increasing the Al content over an order of mag-
To understand the morphological and compositional variations nitude (from 205 m3 m−2 KPa−1 h−1 for the Ni–16.6 wt.% Al to
of Ni–Al alloys during sintering, the back-scattered electron (BSE) 3312 m3 m−2 KPa−1 h−1 for the Ni–40 wt.% Al). Two reasons should
SEM technique is employed. Using the Ni–14 wt.% Al alloy as an be responsible to this: (1) as shown in Fig. 5(a), the proportion of
H.X. Dong et al. / Materials Science and Engineering A 528 (2011) 4849–4855 4853

Fig. 6. Typical SEM images of porous Ni–Al alloys: (a) Ni–16.6 wt % Al, (b) Ni–24 wt.% Al, (c) Ni–32 wt.% Al and (d) Ni–40 wt.% Al.

open pores increases with the Al content, which should enlarge the 3.4. Effect of the Al content on mechanical strength
pore size when pores interconnect together; and (2) the agglomer-
ation of the Al particles in compact discs when the number of the The mechanical strength is an important mechanical property
Al powders is significantly larger than that of Ni powders, resulting for porous materials. It is therefore appropriate to understand the
in the formation of larger pores. Our results are contrasted with the newly developed porous Ni–Al alloys. The bending strength and
results that the porosity and the pore size decrease with increas- tensile strength of our porous Ni–Al alloys were tested at room
ing the Al content in the porous Ni–Al alloys [28], in which the Al temperature and the result is shown in Fig. 7. As can be seen, both
powders only acts as reactants. the bending strength and tensile strength decrease with increasing
The relationship between the permeability and the other two the Al content in the compact discs. There should be two rea-
pore parameters (open porosity and maximum pore size of the sin- sons for this phenomenon. (1) The crystal phase in these nominal
tered compacts) can be described by the modified Hagen–Poiseuille compositions changes from Ni3 Al to NiAl and then to Ni2 Al3 , and
formula [18,33], which gives the intrinsic mechanical properties of these phases are different,
i.e., the ultimate tensile strength of bulk Ni3 Al and NiAl at room
2
J = Bdm  (2) temperature is 933 [34] and 200 MPa [35], respectively. (2) The
porosity and pore size increase sharply with the Al content, which
may suggest that the decreased mechanical properties must be
where J is the permeability, dm is the maximum pore size,  is the
open porosity of a given porous material, and B is a constant relating
to the properties of the permeation fluid and macroscopic dimen-
sion of the porous material. Through measuring the value of J and 75 Tensile strength
of dm2 , the constant B can be determined to be ∼1.5. Therefore we Bending strength
can determine one factor’s value based in Eq. (2) if the other two Fitting Curve
60 2
factors’ values were given. R =0.98
To understand the pore structures of our porous Ni–Al alloys
Strength / MPa

with different Al contents, Fig. 6 shows their typical SEM images. 45


As can be clearly seen, the general pore size increases with increas-
ing the Al content, which is consistent with results shown in Fig. 5. 30
It should be mentioned that the pore structures in the Ni–10.7 wt.%
Al and Ni–14 wt.% Al alloys are similar (refer to Fig. 4(c)). The pore
size and porosity of the porous Ni–10.7 wt.% Al and Ni–14 wt.% Al 15
alloys are also similar, which are obviously smaller than those of
Ni–16.6 wt.% Al alloy (as can be seen in Fig. 6(a)). Fig. 6(b)–(d) shows 0
the SEM images of the porous Ni–24 wt.% Al, Ni–32 wt.% Al and
10 15 20 25 30 35 40
Ni–40 wt.% Al alloys, respectively. The sharply increasing of the
pore size and porosity in these compact discs with high Al con- Al content / wt%
tents is mainly due to the fact that more pores were formed with Fig. 7. Bending strength and tensile strength as a function of Al content for the
increasing the Al content. porous Ni–Al alloys.
4854 H.X. Dong et al. / Materials Science and Engineering A 528 (2011) 4849–4855

Fig. 8. (a) Typical SEM micrographs of the fracture surface after tensile tests of porous Ni–40 wt.% Al; (b) the magnified views of (a).

due to the increased the pore size and the number of the pores and No. 20636020) and by the National Natural Science Founds for
[36]. Larger, open and interconnected pore structures are generally Distinguished Young Scholar (No. 50825102), “973” program (No.
much weaker than small, isolated pore structures because the for- 2009B623400), “863” program (No. 2006AA03Z511) and a Chinese
mer could induce high levels of stress concentration on the material Ministry of Education’s 111 project.
[37]. Although the mechanical properties of all porous Ni–Al alloys
vary significantly, most of their mechanical strengths are higher
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