Materials and Design 37 (2012) 161–165

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Materials and Design

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

Characterization of electrical conductivity of porous metal fiber sintered sheet

using four-point probe method
Wei Zhou a,b,⇑, Yong Tang b, Rong Song a, Lelun Jiang a, K.S. Hui c, K.N. Hui d
a
School of Engineering, Sun Yat-sen University, Guangzhou 510006, China
b
School of Mechanical and Automotive Engineering, South China University of Technology, Guangzhou 510640, China
c
Department of Systems Engineering and Engineering Management, City University of Hong Kong, Hong Kong
d
Department of Materials Science and Engineering, Pusan National University, Republic of Korea

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

Article history: Novel porous metal fiber sintered sheets (PMFSSs) with different porosities were fabricated by sintering
Received 18 October 2011 copper fibers. Using four-point probe method, comparative study was conducted to investigate the effects
Accepted 29 December 2011 of probe spacing, porosity, and sintering condition on the electrical conductivity of PMFSS. Our experimen-
Available online 5 January 2012
tal results showed that probe spacing plays an important role in determining the electrical conductivity.
Uniform probe spacing was adopted in order to reduce the error caused by non-uniformity of probe spac-
Keywords: ing. The measured electrical conductivity was found to decrease with increasing porosity ranging from
B. Fibers and filaments
70% to 90% for the PMFSS produced under the same sintering condition. Our experimental results were
C. Sintering
E. Electrical properties
found to agree well with the theoretical prediction by Liu’s model for the PMFSS with different porosities.
The effect of sintering condition on electrical conductivity was also investigated. It was revealed that
higher sintering temperature or longer holding time yields higher electrical conductivity of PMFSS.
Ó 2012 Elsevier Ltd. All rights reserved.

1. Introduction With the development of science and technology as well as

economy, the demand for porous metals with high porosity and
Porous metals, as a type of structural and functional materials, electrical properties is increasing. Some experimental measure-
have been developing rapidly in recent years [1,2]. Porous metal ments have been made for characterizing the electrical properties
fiber sintered sheet (PMFSS), a relatively new group of porous of porous metals. Dharmasena and Wadley [14] measured the elec-
metals have a three-dimensional reticulated structure featuring trical conductivity of open-cell aluminum foam using four-point
high porosity and large specific surface area. So far, PMFSS has probe method. The experimental results of electrical conductivity
exhibited many significant engineering applications particularly confirmed the linear dependence upon density, but the slope was
in defense and military industry, petrochemical industry, metallur- smaller than that predicted by the unit-cell model. Goodall et al.
gical machinery, automotive industry, and environmental protec- [15] characterized the electrical conductivity of replicated open-
tion for its excellent performance in filtration and separation [1], pore microcellular metal over a wide range of relative density
fluid distribution [3], energy absorption [4], biomedical device using four-point probe technique. It was found that the electrical
[5], catalytic reaction [6], and thermal management [7]. Especially, conductivity of metallic foams varied strongly with different
PMFSS has been attracting attentions as a promising electrode porosities. Liu et al. [16–18] also conducted a series of experiments
material for high efficiency batteries [8–10]. Therefore, the electri- to determine the electrical resistivity of nickel foams developed by
cal conductivity is one of the most important properties need to be electroplating on the polyether sponge sheet using a double circuit
considered. However, previous research work mainly focused on bridge. Duan et al. [19] developed a methodology to calculate the
the open-celled and close-celled metal foams [11–13]. For PMFSS apparent resistivity of metallic foam based on the pentagonal
with high porosity, limited information has been reported about dodecahedron model. The calculated evaluations based on this
the relationships between microscopic structures and electrical methodology approximately agree with the experimental results
properties. Characterizing the electrical conductivity of PMFSS is of Ni–Cr foams and Ni foams. Recently, Cuevas et al. [20] reviewed
demanding especially for its optimal performance in electrode the experimental and theoretical works about the electrical con-
applications. ductivity of metal foams. A new empirical formula was proposed
to describe the relationship between porosity and electrical con-
⇑ Corresponding author at: School of Engineering, Sun Yat-sen University, ductivity for different types of foams.
Guangzhou 510006, China. Tel./fax: +86 20 39332148. From the above reported work, it is found that the detailed
E-mail addresses: [email protected], [email protected] (W. Zhou). study of the relationships relating the porosity and sintering

0261-3069/$ - see front matter Ó 2012 Elsevier Ltd. All rights reserved.
doi:10.1016/j.matdes.2011.12.046
162 W. Zhou et al. / Materials and Design 37 (2012) 161–165

condition with the electrical conductivity of PMFSS is lacking in pressed on the testing sample surface, as shown in Fig. 2. An inline
current literature. In the present study, the PMFSS with a three- four-point probe was placed on the surface of the testing sample
dimensional reticulated structure was fabricated through the [14]. A constant current was applied through the outer current
solid-state sintering of copper fibers. Four-point probe method probes using constant current electric power (Xia Men Mingwei
was used to investigate the dependences of electrical conductivity Electricity CO., ITD, China, D-50D). The voltage drop across the
of PMFSS on the probe spacing, porosity, sintering condition. two inner voltage probes was measured with a digital voltmeter
(Agilent, USA, HP34401A). The electrical resistivity r is given by
2. Experimental procedures [14].
V 
2p I
2.1. Manufacturing process of PMFSS r¼h i ð2Þ
1
X1
þ X13  X 1 þX
1
2
1
 X 2 þX 3

As reported previously [21], the processing procedure of PMFSS

where X1, X2, and X3 are the probe spacings shown in Fig. 2. The
was divided into five steps including fiber chipping, mold-pressing,
electrical conductivity r (in units of S/m) is expressed as
sintering, cooling, and testing. First of all, the continuous copper
fibers were fabricated by cutting method with a multi-tooth tool. 1
These copper fibers were then cut into segments with length rang- r¼ ð3Þ
r
ing from 10 to 20 mm. Next, the copper fibers were randomly dis-
In order to reduce the cell size effects and characterize the over-
tributed into the packing chamber of the mold pressing equipment.
all electrical behavior, the dimension of samples was taken as
Then pressure was applied by screwing the bolt apparatus. In doing
70  40  4 mm which was several times larger than the pore size
so, a semi-finished PMFSS with the same shape of the packing
[12]. In order to eliminate the polarization effect and potential off-
chamber was obtained. Sintering was then carried out in hydrogen
set, voltage drop was measured under forward and reverse current
gas atmosphere with constant pressure of 0.3 MPa. Different sin-
directions and the average of the measured absolute values was
tering temperatures ranging from 700 °C to 1000 °C were taken.
calculated [15,22]. For the specific porosity and sintering condition,
Stage heating method was used to optimize the heating rate, which
ten specimens were prepared. Their mean value was taken as the
was kept at 300 °C/h when the temperature was below 800 °C,
electrical conductivity of PMFSS with such porosity and sintering
while reduced to 200 °C/h as the temperature was above 800 °C.
condition. All measurements were performed in ambient condition
The holding time was set as either 30 min or 60 min. When the sin-
with temperature approximately 25 °C.
tering was completed, the sample was removed from the furnace
and cooled to room temperature in air. Finally, the mold pressing
equipment was disassembled and the PMFSS was ready for electri- 3. Results and discussion
cal characterization. The appearance of PMFSS produced by above
manufacturing procedure was shown in Fig. 1. 3.1. Microscopic observations of PMFSS
Since the obtained PMFSS has a regular geometric shape, we can
calculate the average porosity using the quality–volume method Before sintering, the copper fibers were distributed randomly in
formulated by the pressing mold. The compression was then conducted to make
  contact regions among fibers.
M During sintering process, sintering joints were formed among
hð%Þ ¼ 1   100 ð1Þ
qV fibers as a result of material migration at elevated temperature.
Fiber’s metallurgy unification occurred, resulting in PMFSS with a
where V is the volume of PMFSS (cm3), M, is the mass of PMFSS (g),
three-dimensional reticulated structure [21]. Fig 3a shows the typ-
and q is the density of red copper (g/cm3).
ical three-dimensional reticulated structure of PMFSS sintered at
800 °C for 30 min. Such structure has been used as catalyst carrier
2.2. Electrical conductivity measurements
as well as heat transfer medium in the last 3 years [23,24]. From
Fig. 3b, we found that there were two types of sintering joints
Scanning electron microscopy (JSM-6380LA, Japan) was
presented in PMFSS including fiber-to-fiber surface contact and
adopted to observe the microscopic structure of PMFSS. The
crossing fiber meshing [21,25]. It was also noted that PMFSS could
measurements of electrical conductivity were performed by four-
have a wide porosity range from 60% to 98%, large pore size, and
point probe method in which four sharp probes are mechanically
interconnected pores. Moreover, it is easily to find that copper
fibers have a large number of surface microstructures after

E=70% E=80% E=90% I I

Current probe Voltage probes Current probe

Equipotential surface
Current flow line

PMFSS Sample

Fig. 1. Appearance of PMFSS with different porosities produced by the solid-state Fig. 2. Schematic diagram of four-point probe method for measuring the electrical
sintering of copper fibers. conductivity of PMFSS.
 W. Zhou et al. / Materials and Design 37 (2012) 161–165 163

(a) (c)
(b)
Fig. 3. SEM images of PMFSS produced by the solid-state sintering of copper fibers: (a) three-dimensional reticulated structure of PMFSS sintered at 800 °C for 30 min, (b)
SEM image of bonding types among fibers in the PMFSS, and (c) surface microstructures of single copper fiber after sintering at 800 °C for 30 min.

sintering at 800 °C for 30 min, as shown in Fig. 3c. When the sinter-
0.12
ing temperature was increased, a majority of the surface micro-

S/m
structures disappeared, giving rise to the smooth surface of the

6
fibers [21]. Therefore, the microscopic structures of PMFSS 0.10
depended on the sintering condition. 0.085
Average electrical conductivity 0.08

0.063
3.2. Effect of probe spacing on the electrical conductivity of PMFSS 0.055 0.056
0.06

To analyze the effect of probe spacing on electrical conductivity,

0.04
different probe spacings were adopted to measure the electrical
conductivity of PMFSS with porosity of 90% sintered at 800 °C for
30 min. In this study, four sets of probe spacing were selected 0.02
including set A (X1 = X2 = X3 = 70/3 mm), set B (X1 = X3 = 20 mm,
X2 = 30 mm), set C (X1 = 15 mm, X2 = 25 mm, X3 = 30 mm), and set
D (X1 = X2 = X3 = 15 mm). The measured electrical conductivity of A B C D
PMFSS using different probe spacings is shown in Fig. 4. It was Probe spacings
observed that set A and set D exhibited similar electrical conductiv-
Fig. 5. Average measured electrical conductivity of PMFSS using different probe
ity plots. However, set B and C showed the increase of electrical spacings.
conductivity. Thus, uniform probe spacing was adopted to measure
the electrical conductivity of PMFSS. Moreover, the electrical con-
ductivity of PMFSS was found to decrease with increasing input
90% [11,14]. Also, the approximate average values of electrical
voltage. This can be attributed to the increase of temperature
conductivity were found when the uniform probe spacing was se-
caused by higher input voltage [26]. Besides, the average values
lected. In the following section, uniform probe spacing of set A
of the measurements with different probe spacings are shown in
was taken to measure the electrical conductivity of PMFSS.
Fig. 5. It was found that the average values of electrical conductivity
were little lower than that of the metal foam with same porosity of
3.3. Effect of porosity on the electrical conductivity of PMFSS

Porosity is the most characteristic feature of porous materials.

0.12 So far, several models have been proposed to bridge the relation-
Probe spacing A
S/m

0.11 Probe spacing B ship between electrical conductivity and porosity for porous met-
Probe spacing C als, which can help to improve the design of the materials. For
6

Probe spacing D
0.10 instance, after measuring the electrical conductivity of Ni foam
produced by metal deposition techniques, Langlois and Coeuret
Electrical conductivity

0.09
[27] firstly proposed a half-empirical formula relating the electrical
0.08 conductivity and the porosity for porous material with high poros-
ity ranging from 97% to 97.8% as follows:
0.07
1h
r¼ r0 ð4Þ
0.06 4
0.05 where r and r0 are the electrical conductivity of the porous and
0.0 0.2 0.4 0.6 0.8 1.0 compact metals, respectively, and h stands for the porosity.
Eq. (4) is obtained from only a few experiments based on the
Voltage (mV)
nickel foams. Taking the differences of the specific manufacturing
Fig. 4. Measured electrical conductivity of PMFSS using different probe spacings. processes into account, the formula was revised to be [16].
164 W. Zhou et al. / Materials and Design 37 (2012) 161–165

1h by the three-dimensional reticulated structure with high porosity,

r¼K  r0 ð5Þ
4 which was of a difference in the pore shapes or the strut arrange-
where K is the coefficient dependent on manufacturing technol- ment [15,32].
ogy, or more precisely, on the specific structure of porous metals. When the corresponding experimental data of electrical con-
Other expressions correlating electrical conductivity and porosity ductivity and r0 = 5.96  107 (at 20 °C, in units of S/m) [33] was
of closed-cell foams were proposed by Huang [28–30]. The de- introduced into Eqs. (5)–(7), the mean values of K was obtained
duced expression is to calculate the theoretic values of electrical conductivity of PMFSS.
The measured values, calculated values, and relative deviations
from Eqs. (5)–(7) for the electrical conductivity of PMFSS are given
2Kð1  hÞ
r¼  r0 ð6Þ in Table 1. |Dr| is the difference between measured and calculated
2K þ h
results (i.e. |Dr| = |Calculation value  Measured value|). rE5, rE6,
As for the porous metals with high porosity, an octahedron the- rE7 are the calculated values of electrical conductivity from Eqs.
oretical model was established by Liu et al. [16,17] based on nickel (5)–(7), respectively. The relative deviations (|Dr/r|) of the electri-
foams. It showed that the model reflects well the structure of high cal conductivity can be expressed as the formal [i.e. |Dr/r| = |(Cal-
porosity materials with three-dimensional reticulated structure. culated value  Measured value)/Measured value|  100%]. |Dr5/
The correlation between electrical conductivity and porosity for r|, |Dr6/r|, |Dr7/r| are the relative deviations from Eqs. (5)–(7),
metallic foams is given by respectively.
We observed that the calculated values of electrical conductiv-
1h ity from Eq. (7) exhibited smaller difference from the measured
r¼K  r0 ð7Þ electrical conductivity in comparison to Eqs. (5) and (6) when
3½1  0:121  ð1  hÞ1=2 
the porosity was higher than 80%. However, the Eq. (7) needs to
Fig. 6 shows the measured electrical conductivity of PMFSS with be revised to exactly predict the actual electrical conductivity of
different porosities sintered at 800 °C for 30 min. For the PMFSS PMFSS. Thus, a new alternative model is expected to describe the
produced under the same sintering condition, the electrical con- relationship between porosity and electrical conductivity of PMFSS
ductivity decreased with increasing porosity range from the 70% in our future work.
to 90%. The PMFSS with 70% porosity exhibited the highest electri-
cal conductivity about 0.291  106 S/m. In contrast, the PMFSS
with 90% porosity showed the lowest electrical conductivity about 3.4. Effect of sintering condition on the electrical conductivity of PMFSS
0.055  106 S/m. For the PMFSS with low porosity, better sintering
joints among fibers fabricated by the solid-state sintering process The forming process of PMFSS can be considered as the solid-
would lead to a greater intrinsic metal conductivity [21,31]. There- state sintering process of the copper fibers in a reduction atmo-
fore, the electrical conductivity of PMFSS was increased. Further- sphere [21]. The sintering temperature and holding time are two
more, it is also found that the measured electrical conductivity of important sintering conditions in the forming process of PMFSS.
PMFSS was little lower than the metal foam with high porosity In recent years, some researchers reported that the microstructures
reported in the literatures [11,14]. These results may be caused of PMFSS were greatly affected when the sintering condition was
changed [34,35]. However, there is little information about the rela-
tionship between the sintering condition and electrical conductiv-
ity. Table 2 lists the experimental values of electrical conductivity
0.30
for the PMFSS produced with different sintering conditions. It can
S/m

be seen that the measured electrical conductivity increased with

6

0.25
increasing sintering temperature ranging from 700 °C to 1000 °C.
This may be attributed to the higher sintering temperature which
Electrical conductivity

0.20
is beneficial for atom diffusion and accelerates the sintering pro-
cess. Sintering joints then will be coarsen and the contact interfaces
0.15
among fibers is increased [35], resulting in higher electrical conduc-
tivity. However, for the higher sintering temperature, a majority of
0.10
the microstructures disappeared, leading to smooth surface of
fibers after sintering. The specific surface area of PMFSS is
0.05
decreased greatly [21].
Furthermore, when the holding time was increased from 30 min
70% 75% 80% 85% 90% to 60 min, the electrical conductivity was found to be much larger
Porosity for the PMFSS sintered at 1000 °C. For longer holding time, the sin-
tering joints between fibers are coarser [35]. Thus, the electrical
Fig. 6. Measured electrical conductivity of PMFSS with different porosities sintered conductivity was increased under the longer holding time. In addi-
at 800 °C for 30 min. tion, we also found that the measured electrical conductivity was

Table 1
Experimental results and calculated values of electrical conductivity of PMFSS using different formulae.

No. Porosity h (%) Electrical conductivity Relative deviation

r Measured (106 S/m) rE2 Eq. (5) (106 S/m) rE3 Eq. (6) (106 S/m) rE4 Eq. (7) (106 S/m) |Dr5/r| (%) |Dr6/r| (%) |Dr7/r| (%)
1 70 0.291 0.230 0.297 0.233 21.0 2.18 20.0
2 75 0.228 0.192 0.232 0.193 16.0 1.55 15.5
3 80 0.144 0.153 0.174 0.153 6.44 20.7 6.33
4 85 0.102 0.115 0.123 0.114 12.7 20.4 11.7
5 90 0.055 0.077 0.077 0.075 39.3 40.7 36.9
 W. Zhou et al. / Materials and Design 37 (2012) 161–165 165

Table 2
Measured electrical conductivity of PMFSS produced with different sintering conditions.

No. Sintering parameters Porosity (%) Dimensions of PMFSS (mm3) Electrical resistivity r (106 X m) Electrical conductivity r (106 S/m)
1 700 °C, 30 min 90 70  40  4 28.312 0.035
2 800 °C, 30 min 90 70  40  4 18.315 0.055
3 900 °C, 30 min 90 70  40  4 11.643 0.116
4 1000 °C, 30 min 90 70  40  4 5.224 0.450
5 1000 °C, 60 min 90 70  40  4 3.424 0.702

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