Applied Radiation and Isotopes: N.Z. Noor Azman, S.A. Siddiqui, R. Hart, I.M. Low

Applied Radiation and Isotopes 71 (2013) 6267
Contents lists available at SciVerse ScienceDirect
Applied Radiation and Isotopes

journal homepage: www.elsevier.com/locate/apradiso
Effect of particle size, ller loadings and x-ray tube voltage on the
transmitted x-ray transmission in tungsten oxideepoxy composites
N.Z. Noor Azman a,b, S.A. Siddiqui a, R. Hart c, I.M. Low a,n
a
Department of Imaging and Applied Physics, Curtin University, GPO Box U1987, Perth, WA 6845, Australia
School of Physics, Universiti Sains Malaysia, 11800 Penang, Malaysia
c
Royal Perth Hospital, East Perth, WA 6001, Australia
b
H I G H L I G H T S
c
c
c
Investigated the effect of particle size of WO3 on the x-ray attenuation ability.
Nano-sized WO3 has a better ability to attenuate lower x-ray energies (2249 kVp).
Particle size has negligible effect at the higher x-ray energy range (40120 kVp).
a r t i c l e i n f o
a b s t r a c t
Article history:
Received 19 June 2012
Received in revised form
7 September 2012
Accepted 18 September 2012
Available online 25 September 2012
The effect of particle size, ller loadings and x-ray tube voltage on the x-ray transmission in WO3-epoxy
composites has been investigated using the mammography unit and a general radiography unit. Results
indicate that nano-sized WO3 has a better ability to attenuate the x-ray beam generated by lower tube
voltages (2535 kV) when compared to micro-sized WO3 of the same ller loading. However, the effect
of particle size on x-ray transmission was negligible at the higher x-ray tube voltages (40120 kV).
Crown Copyright & 2012 Published by Elsevier Ltd. All rights reserved.
Keywords:
Micro-sized WO3-epoxy composites
Nano-sized WO3-epoxy composites
Transmission
X-ray tube voltage
Filler loading
1. Introduction
Use of nano-particles in designing advanced materials has
attracted much attraction amongst the researchers because of
superior physical and mechanical properties that can be achieved.
For instance, recent studies have shown that nano-sized ller
reinforced polymer composites provided much improvement in
chemical, physical and mechanical properties by virtue of better
dispersion of the nano-particles within the polymer matrix
(Chapman and Mulvaney, 2001; Karim et al., 2002; Ohno et al.,
2002; Schmidt and Malwitz, 2003). The main improvement of
nanoparticles as a ller assembly over conventional materials is
the maximization of the surface/volume ratio of the llers (Fabiani
et al., 2010). For example, nanoparticles improved the electrochemical capacitance of a-Ni(OH)2 in alkali solutions as compared to
Corresponding author. Tel.: 618 9266 7544; fax: 618 9266 2377.
E-mail address: j.low@curtin.edu.au (I.M. Low).
micro-sized particles of the same hydroxide due to the greater

surface/volume ratio of the nanoparticles (Jayalakshmi et al., 2006).
Additionally, this size-effect also becomes one of the virtues in
designing materials for shielding of ionizing radiations. Some
x-ray technologists believe that this effect will improve the x-ray
attenuation ability of the composite since nano-sized llers are
able to disperse more uniformly within the polymer matrix with
less agglomeration as compared to micro-sized llers (Botelho
et al., 2011; El Haber and Froyer, 2008; Steinhart, 2004). A recent
study by Botelho et al. (2011) found that nanostructured copper
oxide (CuO) is more effective in attenuation of lower x-ray beam
energy (26 and 30 kV) and no signicant variation in x-ray
attenuation at higher x-ray beam energy (60 and 102 kV).
Kunzel
and Okuno (2012) also provided similar results, which
show that the x-ray absorption is higher for a nanostructured CuO
compound compared to the microstructured counterpart for low
energy x-ray beams (25 and 30 kV) for all CuO concentrations
incorporated into polymeric resin.
In general, the attenuation of photons (x-rays/gamma-rays) is
dependent upon three factors: density, elemental composition,
0969-8043/$ - see front matter Crown Copyright & 2012 Published by Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.apradiso.2012.09.012
N.Z. Noor Azman et al. / Applied Radiation and Isotopes 71 (2013) 6267
and thickness of the absorbing material (Sprawls, 1993). Even

though lead (Pb) or lead compounds provide good x-ray shielding
properties, their usage as the shielding materials has increasingly
become a sensitive issue due to its hazardous nature. As a result,
much research has been focusing on developing new x-ray
shielding materials which are safer and easier to handle (Robert,
2005; Spinks and Wood, 1976).
The aim of this work was to develop new x-ray shielding
materials based on tungsten oxideepoxy composites with either
nano-sized or micro-sized llers. The effect of ller size on the x-ray
transmission in the diagnostic imaging energy range (25120 kV)
has been investigated. The ller size effect in x-ray shielding ability
is discussed.
2. Experimental procedure
2.1. Samples preparation
Nano-sized (o100 nm) and micro-sized ( 20 mm) tungsten
oxide (WO3) were used as ller for synthesizing WO3-epoxy
composites. The former were obtained from Sigma-Aldrich and
the latter (FR251) from Fiberglass and Resin Sales.
To prepare WO3-epoxy composite samples, WO3 powder was
added into the FR251 epoxy resin (Bisphenol-A diglycidyl ether
polymer) before the FR251 hardener (Isophoronediamine) was
mixed into it. The ratio of epoxy resin to hardener used was 2:1.
The mixing of WO3 powder in epoxy resin was done through
gentle stirring using a stirring machine at constant speed for
15 min to ensure uniform dispersion of the powder in epoxy
matrix. The well-mixed mixture was then cast in a 4 cm 6 cm
rectangular silicon rubber mold with a thickness of 7 mm and was
allowed to set overnight at room temperature. The list of
prepared samples with different weight percentages of WO3 are
shown in Table 1.
2.2. Measurement of the x-ray transmission

This work was done using two different sets of equipment.
For the lower x-ray energy range, a mammography unit (brand:
Siemens AG, model: 2403951-4G.E Health Care) was used while a
general diagnostic x-ray machine (brand: Shimadzu, model: Circlex
0.6/1.2 P364DK-100SF) was used for the higher x-ray energy range.
The initial x-ray beam intensity (Io) was determined by directly
measuring x-rays with the DIADOS diagnostic detector connected
to DIADOS diagnostic dosimeter (PTW-Freiburg, Germany) in the
absence of the sample. The dosimeter is a universal dosimeter for
measuring simultaneous dose and dose rate for radiography,
uoroscopy, mammography, dental X-ray and CT with a minimal
dose sensitivity of 8.7 10 8 milliGray (mGy) and also has a
claimed sensitive range of x-rays energy of 25 kV to 150 kV.
63
Meanwhile the transmitted x-ray beam intensity (I) was taken

with the sample placed on the detector. The distance between the xrays tube and the detector was set to 86 cm since this is the
maximum distance that can be adjusted for the mammography unit,
and the x-ray beam was well collimated to the size of the sample.
The exposure was set at 10 mAs to obtain meaningful readings
for this type of detector. The x-ray beams generated in the range of
2549 kV tube voltage was selected from mammography unit
since the machine can go only within this range for lower x-ray
energy. On the other hand, the x-ray beams generated in the range
of 40120 kV tube voltage was chosen from the general diagnostic
x-ray machine because this range is the normal range of the x-ray
tube voltage used in general diagnostic imaging purposes.
For each composite, the measurements were performed three
times. The performance of micro-sized and nano-sized WO3-epoxy
composite was compared from a log-linear scale graph of x-ray
transmission (I/Io) as a function of ller loading for each x-ray tube
voltage.
3. Results and discussion

Three different anode/lter combinations (Table 2) were used
for lower x-ray tube voltage generated from the mammography
machine, since the combination was operated by the machine
itself. The x-ray beams generated by these anode/lter combinations composed mainly of the characteristic x-ray energies of
molybdenum (17.5 keV and 19.6 keV) or rhodium (20.2 keV and
22.7 keV). For WO3 of 5 wt% and 10 wt%, the exit dose reading was
observed at 25 kV x-ray tube voltage while for 20 wt%35 wt%, the
dose reading was initiated at 30 kV x-ray tube voltage due to the
zero reading of the dosimeter at 25 kV x-ray tube voltages.
Fig. 1 clearly showed a big difference of x-ray transmission
between micro-sized WO3-epoxy composite and nano-sized
WO3-epoxy composite for x-ray beams generated for 2549 kV
tube voltages by the mammography unit at the same ller
loading. The ratio of the x-ray transmission for micro-sized
WO3-epoxy composite (Tm) to the x-ray transmission for nanosized WO3-epoxy composite (Tn) was in the range 1.33.0. The
ratio (Tm/Tn) was larger at the x-ray tube voltages 2535 kV and
was dropping as the x-ray tube voltage was increased ( Z40 kV)
as can be seen in Fig. 1. Meanwhile, the ratio (Tm/Tn) is E1.0, for
the diagnostic x-ray tube voltages range (40120 kV) generated
by the general radiography unit, which provided that Tm ETn.
Thus, the effect of WO3 particle sized reinforced epoxy composite
was negligible at the x-ray beam produced by higher x-ray tube
voltage (Fig. 2).
Table 2
Anode/lter combination operated by mammography machine.
X-ray tube
voltage (kV)
Anode/lter
combination
22
25
30
Mo/Moa
Composite by weight fraction (wt %)
35
40
Mo/Rhb
Filler (WO3)
Epoxy resin
45
49
Rh/Rhc
5
10
20
30
35
95
90
80
70
65
Table 1
List of prepared samples with different weight
fractions of ller (WO3) and epoxy resin.
a
Mo/Mo stands for molybdenum anode/
molybdenum lter.
b
Mo/Rh stands for molybdenum anode/rhodium
lter.
c
Rh/Rh stands for rhodium anode/rhodium lter.
64
Fig. 1. X-ray transmission as a function of ller loading of (a) 5 and 10 wt% of the nano-sized WO3-epoxy composite for x-ray tube voltage of 25, 35 and 49 kV generated by
mammography unit and (b) 2035 wt% of the nano-sized WO3-epoxy composite as compared to the micro-sized WO3-epoxy composite for x-ray tube voltage of 30, 35 and
49 kV generated by mammography unit.
Besides that, Fig. 3 showed that even though the x-ray tube
voltage selected from the mammography unit, and general radiography unit is same (40 kV), the value of x-ray transmission by
the nano-sized WO3 epoxy composite is lower for the x-ray
photon generated by the mammography unit. A similar result
was also obtained from micro-sized WO3 epoxy composite. This
outcome proved that the general radiography unit comprised of a
continuous spectrum of x-ray energy, which is having higher
equivalent energies as compared to the characteristic x-ray
energies produced from the mammography unit (17.522.7 keV).
Generally, photoelectric absorption dominates at lower photon
(x-ray) energy range. A photon is completely absorbed by the
atom of the material, and a photoelectron is ejected in the
process. The ejected photoelectrons may undergo single- or
multiple-scattering events with neighboring atoms, which can
alter the mass attenuation coefcient of an element relative to the
bulk material when considered over a small range of x-ray
energies together with slight uctuations in the probability of
emission of Auger electron and uorescent photons. The
probability of the photoelectric interaction is approximately

dependent on Z3/E3 where Z is the atomic number of the
absorbing material and E is the photon energy. Furthermore, the
number of W particles/gram in the nano-sized WO3-epoxy
composite is higher than that for the micro-sized WO3-epoxy
composite. Thus, the probability of an x-ray photon generated by
lower tube voltage to interact and to be absorbed may be higher
for nano-sized WO3-epoxy composite rather than micro-sized
WO3-epoxy composite.
As photon energy increases, the probability of Compton
scattering increases and hence the attenuation by the material
decreases since this interaction was weakly dependent on Z and E.
Hence, the probability of an x-ray photon generated by higher
tube voltage to interact and to be absorbed may be similar for
nano-sized and micro-sized WO3-epoxy composite.
To support our investigation on an x-ray photon generated by
lower tube voltage, we have repeated the procedure to measure
the x-ray transmission of a WO3 compact disc of the same mass
for 20 wt% (31% porosity) and 35 wt% (34% porosity) of WO3
65
Fig. 2. X-ray transmission as a function of ller loading of (a) 5 and 10 wt% and (b) 2035 wt% of the nano-sized WO3-epoxy composite as compared to the micro-sized
WO3-epoxy composite for x-ray tube voltage of 40120 kVgenerated by general radiography unit.
Fig. 3. Comparison of x-ray transmission values for all nano-sized WO3 wt% loading in the epoxy sample for operating tube voltage of 40 kV used by the mammography
unit and the general radiography unit.
66
Fig. 4. X-ray transmission for WO3 compact disc as compared to both micro-sized and nano-sized WO3-epoxy composite of the same mass of (a) 20 wt% and (b) 35 wt% of
WO3 loading in epoxy sample for x-ray tube voltage range (3049 kV) generated by mammography unit.
loading in the epoxy sample. Fig. 4 proved that the WO3 compact
disc has the lowest x-ray transmission as compared to both
micro-sized and nano-sized WO3-epoxy composites of the same
mass since WO3 particles have been compressed to be close
together (even though they have high porosity) rather than being
dispersed.
Hence, the results obtained in this work are in good agreement
with the work of Kunzel

and Okuno, (2012) which showed that
nano-sized llers are superior to micro-sized llers for attenuating
the x-ray beams generated for lower tube voltages but the effect is
the same for the x-ray beams generated for higher tube voltages.
4. Conclusions
The results of this work showed that for the same WO3 loading,
nano-sized WO3-epoxy composite has better attenuating ability
to attenuate the x-ray beams generated for lower tube voltages
(2535 kV) when compared to the micro-sized WO3-epoxy
composite. However, the role of particle size in x-ray shielding

was insignicant at the higher tube voltages range (40120 kV).
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Applied Radiation and Isotopes 71 (2013) 6267

Contents lists available at SciVerse ScienceDirect

Applied Radiation and Isotopes

micro-sized particles of the same hydroxide due to the greater

and thickness of the absorbing material (Sprawls, 1993). Even

2.2. Measurement of the x-ray transmission

Meanwhile the transmitted x-ray beam intensity (I) was taken

3. Results and discussion

Composite by weight fraction (wt %)

probability of the photoelectric interaction is approximately

with the work of Kunzel

composite. However, the role of particle size in x-ray shielding

Botelho, M.Z., Kunzel,

Schmidt, G., Malwitz, M.M., 2003. Properties of polymer-nanoparticle composites.

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