Authors Accepted Manuscript

Magnetic properties of polymer matrix composites

with embedded ferrite particles
Ana Paula Pereira Fulco, Jos Daniel Diniz Melo,
Carlos Alberto Paskocimas, Suzana Nbrega de
Medeiros, Fernando Luis de Araujo Machado,
Alexandre Ricalde Rodrigues
www.elsevier.com

PII:
DOI:
Reference:

S0963-8695(15)00112-7
http://dx.doi.org/10.1016/j.ndteint.2015.10.002
JNDT1720

To appear in: NDT and E International

Received date: 1 July 2015
Revised date: 14 September 2015
Accepted date: 1 October 2015
Cite this article as: Ana Paula Pereira Fulco, Jos Daniel Diniz Melo, Carlos
Alberto Paskocimas, Suzana Nbrega de Medeiros, Fernando Luis de Araujo
Machado and Alexandre Ricalde Rodrigues, Magnetic properties of polymer
matrix composites with embedded ferrite particles, NDT and E International,
http://dx.doi.org/10.1016/j.ndteint.2015.10.002
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Magnetic properties of polymer matrix composites with embedded ferrite particles

Ana Paula Pereira FulcoI,*; Jos Daniel Diniz MeloI; Carlos Alberto PaskocimasI;
Suzana Nbrega de MedeirosII; Fernando Luis de Araujo MachadoIII; Alexandre
Ricalde RodriguesIII

Department of Materials Engineering, Federal University of Rio Grande do Norte -

UFRN, Natal, RN, Brazil

II

Department of Physics, Federal University of Rio Grande do Norte - UFRN, Natal,

RN, Brazil
III

Department of Physics, Federal University of Pernambuco - UFPE, Recife, PE, Brazil

* e-mail address: anapfulco@yahoo.com.br

ABSTRACT
Polymeric composite materials offer advantages for many applications because of a
combination of properties, which includes high specific mechanical strength and elastic
modulus and corrosion resistance. However, the non-magnetic nature of these materials
impedes the use of nondestructive evaluation (NDE) techniques using magnetic sensors.
In this work, glass fiber-reinforced epoxy magnetic composites were produced with the
addition of 10 wt.% of cobalt or barium ferrite particles. Circular plates with notches of
1, 5 and 10 mm in diameter were produced and characterized using magnetic flux
leakage (MFL) technique. The effect of particle size on the magnetic properties of the
composites was also investigated for the barium ferrite. The results indicated a good
correlation between the measured magnetic signals and the presence of notches.
Smaller average particle sizes hindered the identification of the smallest notch.
1

However, it resulted in better signal-to-noise ratio for the intermediate and larger size
notches.
Keywords: polymer-matrix composites (PMCs); magnetic markers; non-destructive
testing; ferrites.

1. Introduction
Polymer composite materials offer a combination of properties that makes them
advantageous for many applications. These properties include low density, high
mechanical strength and elastic modulus and corrosion resistance. Due to these unique
characteristics, these materials are widely used in applications such as aeronautical and
aerospace structures, sporting goods and various industrial applications.
Polymer composites are increasingly recognized as an enabling technology to
meet specific and ever-increasing demanding requirements of the oil and gas industry.
As corrosion poses major challenges for conventional steel pipes, the inherent corrosion
resistance of polymer composites combined with their superior mechanical properties
and low density has made them the natural choice of material [1-4]. Currently, many
types of fiber-reinforced polymer materials are used in oilfields. While fiberglass has
been the typical reinforcement, the predominant resins are polyester, vinyl ester and
epoxy [1].
Damage in composite structures are known to affect their mechanical properties
and functionality. In some cases, damage progression may ultimately lead to structural
failure with potential consequences that include damage to property or the environment
and even loss of human life. While some surface damages may be easily detected

during routine inspections, internal damages that are often undetectable by simple visual
inspection can cause significant reductions in strength and stability of the structure.
Therefore, approaches for the detection of internal damages in polymer composite
materials are of great interest. The use of nondestructive evaluation (NDE) techniques
allows assessing the structural integrity of the component without damaging the
materials. Typical nondestructive testing (NDT) techniques currently used to examine
polymer composite materials include ultrasound, thermography, shearography and x-ray
computed tomography (XR - CT) [5-7].
Shearography has been used to assess damages, including the detection of
delamination, with various types of excitation such as temperature, vacuum and internal
pressure [6]. Thermography is a highly sensitive technique to detect delamination, but
there are limitations to measurements on thick laminates [6]. X-ray computed
tomography (X-ray CT) provides high-resolution images and full 3D reconstruction of
the assessed part and can detect defects such as voids, cracks, inclusions, dry fibers and
delamination. In this case, the specimens to be tested may be thicker than those
evaluated by thermography due to low x-ray attenuation of polymer composites.
Ultrasound have been widely used for the inspection of metallic parts [7].

In

composites, ultrasonic inspection can detect damages such as delamination, providing

reliable information on relatively thick parts.
Magnetic Flux Leakage (MFL) testing is a widely used, non-destructive testing
(NDT) method for the detection of corrosion, pitting, cracks and wall losses in steel
structures, including steel pipelines [8]. However, this technique is not suitable for
polymer composites because the material cannot be magnetized. Thus, pipelines made
with conventional polymer composites do not allow structural integrity assessment
through nondestructive techniques (NDT) using instrumented pigs (pipeline inspection
3

gauge), which operate with magnetic sensors.

This is a major limitation of these

materials in this type of application.

The addition of magnetic particles to polymer matrix composites offers great
potential for the inspection of these materials using NDT that are sensitive to changes in
magnetic field. Ferrites are ceramic magnetic materials with spontaneous magnetic
induction [9], which can be used in a wide variety of technological applications. These
materials are therefore natural candidates to be added to polymer composites.
The aim of this work was to develop polymer composites with the addition of
ferrites as magnetic markers to allow the application of damage detection techniques
using magnetic flux leakage and to study the influence of particle size on the magnetic
properties of the material.

2. Experimental
2.1. Preparation and characterization of the ferrite particles
Cobalt ferrite particles were synthesized by the Pechini method. Stoichiometric
amounts

of

citric

acid

(C6H8O7,

99%

purity),

nitrate

cobalt

hexahydrate

(Co(NO3)2.6H2O, 99% purity) and iron nitrate nonahydrate (Fe(NO3)39H2O, 99%

purity) were dissolved in ethylene glycol (C2H6O2, 99 % purity) under magnetic stirring.
Three moles of ethylene glycol per mole of metal ions were used for the synthesis. The
gel was dried in a muffle furnace (Marconi, model MA385) to the primary calcination at
temperature of 350C for 3 h with a heating rate of 3C/min and static oxidizing
atmosphere to eliminate the organic material.

This resulted in an expanded resin

(spongy and dark colored product). The product was then milled to form fine and

homogeneous cobalt ferrite powders. Subsequently, the powders were calcined at 800C
for 6 h in a muffle furnace using a heating rate of 10C/min.
Commercially available barium hexaferrite produced by Fermag Ltda Brazil
was milled to reduce particle size using a high-energy attritor mill at room temperature.
The milling process was conducted using zirconia balls in wet medium (isopropyl
alcohol) for 12 h and 20 h. The process was interrupted for 30 min, at every 3 h, to
minimize heating. The different milling times were used to allow the evaluation of
effect of particle size on the magnetic properties of the composites.
The crystalline structure of the ferrites was analyzed by X-ray diffraction (XRD)
using a XRD -7000 Shimadzu diffractometer with CuK radiation source. Crystallite
sizes were obtained with Scherrer's equation [10]. The Rietveld method was used to
refine the XRD data [11] using the MAUD (Materials Analysis Using Diffraction)
program [12]. Ferrite particles were also observed by field emission scanning electron
microscopy FEG SEM (FEI Inspect F50) operating at an acceleration voltage of 20 kV.
Based on the FEG SEM images, average particle size and size distribution were
estimated using a minimum of 15 particles in a typical sample. Magnetic measurements
were performed at room temperature using a vibrating sample magnetometer (VSM).

2.2. Fabrication and characterization of the composite plates

Circular plates of 250 mm in diameter (Figure 1) were manufactured by hand
layup for magnetic characterization. The materials used were: fiberglass 0/90 biaxial
knitted fabric type KT C1000 SE 1500 (975 g/m2) from Owens Corning, epoxy resin
type AIRSTONE 780E from Dow Chemical Company and ferrite particles. The epoxy
resin was mixed with ferrite particles using a mix ratio in parts by weight (pbw) of
5

90:10 (resin:particles). Composite materials with magnetic particles fillers have been
reported in the literature with particle contents up to 60 wt.% [13,14,15]. In this work,
the particle content was limited to 10 wt.% in order to maintain the low viscosity of the
epoxy, which is an important advantage in thermoset polymer composite
manufacturing.

Higher particle content have also been reported to reduce some

mechanical properties of polymer composites, such as tensile strength. The evaluation

of mechanical properties was not included in the scope of this work.
A mechanical mixer (Marconi MA147) with speed of 1500 rpm was used to
disperse the ferrite particles in the polymer matrix over a period of 15 min. Then, the
fiberglass fabric was impregnated with epoxy resin combined with ferrite particles and
three layers were laid-up at [0/45/0], respectively, on a flat tool previously prepared
with mold release agent. This staking sequence results in laminates with fibers at 0,
90, 45, and -45 which are commonly used in structural applications.
The laminate was then vacuum bagged and cured at about 25 C. Circular
notches were drilled on the composite plates using drill bits of 1, 5 and 10 mm,
respectively, for subsequent magnetic characterization. The sizes of the notches
considered in this work are of the same order of magnitude as those typically produced
by corrosion found in both internal and external surfaces of metallic pipes carrying
crude oil. Overall, four circular plates were produced according to the type of ferrite
added: cobalt ferrite, barium ferrite as received, barium ferrite milled for 12h and
barium ferrite milled for 20h.

Figure 1 Polymer matrix composite plates with notches. Stickers on each side
of the notches limits the region analyzed on the magnetic measurements.

Field emission scanning electron microscopy images of the composite plates

with magnetic particles were obtained using an FEI Inspect F50 to evaluate particle
dispersion.
Variations in magnetic field on the four polymer matrix composite plates were
measured using a custom-made apparatus (Figure 2). The plates were first mounted on
a stepper motor in which it was possible to control the speed and direction of spin. A
magnet and a Hall sensor were kept fixed near the rotating plate to measure the vertical
component of the magnetic field. The Hall sensor with three pins and a sensitivity of 5
mV was connected to a nanovoltmeter and a current source.

Nanovoltmeter

Circular plate

Hall sensor

Current source

Stepper motor

Figure 2 Custom-made apparatus for the magnetic measurements.

The Hall sensor detected the magnetic field produced by the magnetized
composite plate along with distortions produced in the field by the notches. There are at
least two reasons for the measured variations in magnetic flux lines at the notches. First,
as observed in stainless steel, the flux lines are more concentrated at the notches
because of the reduction in thickness that, in turn, increases locally the magnetic field
and saturates the local magnetization. Secondly, a smaller component of the magnetic
field produced by the magnetic particles is detected at the notch area due to the
increased sensor-to-surface distance. Data were acquired via a LabView-based
computer controlled data acquisition system using a GPIB interface. In order to verify
the repeatability of the measurements, the direction of rotation of the circular plates was
reversed over the limits of each notch using the stepper motor controller. Symmetrical
curves about the turning point indicate a clear correlation of the notch with the
deformation of the magnetic field lines over the region.
8

3. Results and Discussion

Figure 3 shows the X-ray diffraction pattern for the cobalt ferrite after heat
treatment at 800 C for 6 h. Peaks related to the CoFe2O4 phase confirm the cobalt
structure (22-1086). However, the additional peaks observed suggest the presence of
other phases on the cobalt ferrite structure. In this case, the peaks correspond to the
following impurities: hematite (Fe2O3) and cobalt oxide (Co3O4), with JCPDS ICDD
file numbers of (87-1165) and (80-1335), respectively, as determined using the X'Pert
software.

5000

CoFe2O4
Fe2O3
Co3O4

Intensity (CPS)

4000

3000

2000

1000

0
10

20

30

40

50

60

70

80

Figure 3 X-ray diffraction pattern of the cobalt ferrite.

Figure 4 shows X-ray diffraction patterns of barium ferrites as received and

after milling for 12 h and 20 h. Peaks of BaFe12O19 are observed in all patterns (070276).

A diffraction peak at 2 = 24.07 corresponding to a Fe2O3 phase (03-0800) was

also observed on X-ray diffraction patterns of the milled samples. The appearance of
this phase can be explained by contamination and broken bonds between Fe atoms
during the milling process. Furthermore, the diffraction peak broadening observed in
the milled samples indicates fragmentation of the material and refinement of crystallite
size to the nanometer range, as result of the milling process. Similar observation has
been reported in the literature [16].

Intensity (CPS)

1200
1000
800
600
400
200
0
500
400
300
200
100
0
800
700
600
500
400
300
200
100
0
10

BaFe12O19

Fe2O3

(a)

20

40

60

80

(b)

20

40

60

80

(c)

20

30

40

50

60

70

80

Figure 4 X-ray Diffraction pattern of barium ferrite samples: (a) without milling, (b)
milled for 12 h and (c) milled for 20 h.

Average particle size and crystallite size of ferrite particles are shown in Table 1.

10

Table 1 Particle size and crystallite size of ferrite particles.

Oxides

Average crystalline size (nm)

Particle size (nm)

CoFe2O4

256.53

340

BaFe12O19 (without milling)

181.76

750

BaFe12O19 (12 hours)

24.49

670

BaFe12O19 (20 hours)

18.58

400

According to the data presented in Table 1, the milling process was effective in
reducing the particle size of BaFe12O19 ferrites from an average of 750 nm to 670 nm,
after 12 h, and to 400 nm after 20 h milling time. For CoFe2O4, the average estimated
particle size was 340 nm.
For BaFe12O19 samples, it was observed that the milling process reduced the
average crystallite size to the nanometer range, in agreement to results previously
reported in literature [16]. Therefore, there was a reduction from 181.76 nm (starting
BaFe12O19) to 18.58 nm (20 h milling time).

The most significant reduction in

crystallite size was during the first 12 h of milling time when the average crystallite was
reduced from 181.76 nm to 24.49 nm. The average crystallite size measurements agree
with the results of the X-ray diffraction peaks for the BaFe12O19 samples for which
sharper peaks imply larger crystallite size.
For CoFe2O4, the crystallite size determined was 256.53 nm. The literature
reports crystallite size for cobalt ferrite [17] when synthesized by another method at
11

temperature of 800C/6h, obtaining crystallite size of 102.32 nm. This larger average
crystallite size is due to the effect of diffusion, which occurs between ions at high
temperatures, since this favors the coalescence of grains, forming larger crystals.
Although Scherrer equation is known to be applicable to crystallite sizes below 200 nm,
the value measured is an indication that the crystallite size of the CoFe2O4 produced is
larger than that obtained by a different synthesis method published in the literature [17].
FEG SEM micrographs of the ferrites are shown in Figure 5. For the CoFe2O4
sample, the material obtained is composed of coarse clusters and of finely divided
particles (Figure 5 a). This can be attributed to the characteristic of the carbonized
material, which has been first disaggregated in a mortar, yielding particles with a broad
distribution of cluster sizes and that preserves the size distribution after calcination.
Thus, clusters with estimated sizes ranging from 10 m to 2 m associated with
particles of sizes ranging from 1 m to 300 nm were observed. The estimated average
particle size in this case was 340 nm.
For the BaFe12O19 sample before milling (Figure 5 b), the micrograph indicates
that the original barium ferrite is composed by clusters of tightly bound smaller
particles. These clusters were found to have an average size of about 13 m consisting
of particles of about 750 nm in size.

These characteristics are related to the

manufacturing process of these ferrites which were obtained by solid state reaction
using high heat treatment temperatures, typically above 1200 C. This process results in
the formation of the desired phase, as well as powder sintering.
After the milling process, clusters of finer particle sizes are obtained, as shown
in Figure 5 a) and b). The powder showed average particle size of about 670 nm and
400 nm, after milling for 12 h and 20 h, respectively. This suggests that the milling

12

process was effective in breaking the clusters and reducing the particle size of the
original material. However, the presence of some particles with angular shape and
average size of around 2.30 m was verified. These particles are remaining fragments
of the original unmilled particles.

a)

b)

c)

d)

Figure 5 FEG SEM micrographs of the ferrite particles: a) CoFe2O4, b) BaFe12O19

(without milling), c) BaFe12O19 (12 h), d) BaFe12O19 (20 h).

13

Figure 6 shows the magnetization curves recorded at room temperature (27 C)

with maximum field of 1.8T for CoFe2O4 and BaFe12O19 samples.

The highest

saturation magnetization value, 76 J/T-kg, was obtained for the unmilled BaFe12O19
sample. In this case, the largest particle size (Figure 5 b) favored the formation of
magnetic fields of greater magnitude.

Larger particles result in a larger area of

magnetic domain, which favors increased magnetization. Therefore, the milling process
of the ferrites resulted in lower saturation magnetization.
It was also observed that the milling process of barium ferrites resulted in the
formation of hematite phase, as previously discussed and shown in Figure 4. The
formation of this phase was explained by contamination of the milling system
(polyamide 66 - Technyl ball and support) or broken bonds between Fe atoms during
the milling process. The presence of hematite may have influenced the saturation
magnetization measurements.
For BaFe12O19 sample (before milling), the coercivity value was 0.25T. After
the milling process for 12 h and 20 h, this value was reduced to approximately 0.19T.
This can be explained by the fact that a smaller coercivity implies in a smaller saturation
field and easier magnetization of the material.

This effect was confirmed by the

characterization of these materials by MFL.

14

80
60
40

M (J/T-kg)

20
0
-20
CoFe2O4

-40

BaFe12O19 - no grinding
BaFe12O19 - 12 hours

-60

BaFe12O19 - 20 hours
-80

-2000

-1500

-1000

-500

500

1000

1500

2000

H (T)

Figure 6 Graphic representation of the magnetization as a function of the magnetic field

for CoFe2O4, BaFe12O19 (no milling), BaFe12O19 (12 h) and BaFe12O19 (20 h).

Figure 7 shows FEG SEM micrographs of the polymer matrix composites with
the addition of ferrite particles. Clusters of about 4.0 m were observed in composites
with BaFe12O19 (unmilled) and CoFe2O4 ferrites, as shown in Figure 7 a) and b),
respectively. In figure 7 c), which corresponds to the composite with BaFe12O19 (milled
for 20 h), it can be observed that the milling process favored not only the reduction of
particle size but also their dispersion in the polymeric matrix. Uniform dispersion of the
magnetic particles on the composite is essential for damage detection since areas
without magnetic particles may produce a false indication of damage.

15

a)

b)

c)

Figure 7 FEG SEM micrographs of the polymer matrix composite with the addition of
the following particles: a) BaFe12O19 (unmilled), b) CoFe2O4, c) BaFe12O19 (milled for
20 h).
Figures 8, 9 and 10 show variation in magnetic field (mT) measured
perpendicular to the plane of the circular plates versus distance (mm) for circular
notches of 1 mm, 5 mm and 10 mm in diameter, respectively, as previously shown in
Figure 2. The curves of magnetic field variation (Figures 8 to 10) clearly indicate the
presence of notches on the circular plates. The beginning and end of each notch marked
with arrows in Figures 8 to 10 match the notch diameter on the circular plates, thereby
confirming that the field signal obtained is characteristic of each notch.

The
16

repeatability of the measured signals was assessed using measurements in clockwise

and counterclockwise directions and the position of inversion in the rotation direction is
indicated in Figures 8 to 10 using dotted lines. It was also observed in these figures that
the signals measured on circular plates with barium ferrite (before milling) and with
cobalt ferrite are very well defined, providing curves indicative of the beginning and
end of the notch. For circular plates with addition of barium ferrite milled for 12 h and
20 h, the variation of magnetic signal over the notch area was detected only for notches
of 5 mm and 10 mm (Figures 9 and 10).

CoFe2O4
BaFe12O19 (no grinding)

BaFe12O19 (12 hours)

BaFe12O19 (20 hours)

H (mT)

0
5

10

15

20

25

30

d (mm)

Figure 8 Magnetic field curves (mT) versus distance measured in composite plates
with CoFe2O4, BaFe12O19 (no milling), BaFe12O19 (12 h) and BaFe12O19 (20 h) at the
1mm notch. Arrows indicate the beginning and end of each notch.

17

H (mT)

CoFe2O4

BaFe12O19 (no grinding)

BaFe12O19 (12 hours)
BaFe12O19 (20 hours)

-2

10

15

20

25

30

d (mm)

Figure 9 Magnetic field curves (mT) versus distance measured in composite plates with
CoFe2O4, BaFe12O19 (no milling), BaFe12O19 (12 h) and BaFe12O19 (20 h) at the 5 mm
notch. Arrows indicate the beginning and end of each notch.

The curves of variation in magnetic field presented in Figure 8 show no change

in magnetic signal over the notch area for composites with the addition of barium ferrite
milled for 12 to 20 h. Thus, the milling of magnetic particles did not favor the detection
of smaller notches (1 mm). For notches of 5 and 10 mm (Figures 9 and 10), the
beginning and end of the notches can be clearly identified by the arrows on all four
polymer composite plates.
For all measurements (Figures 8 to 10) there was a greater variation in magnetic
signal over the notches for composite plates with cobalt ferrite and barium ferrite
18

without milling. This can be explained by the higher magnetization of these samples
which results in higher equipotential lines and consequently greater magnetic flux
leakage, thereby contributing to higher resolution in detecting the notch, as evidenced
by the hysteresis curves of these materials (Figure 6). However, the curves presented in
Figures 9 and 10 indicate that the smallest particle size allowed producing smoother
magnetic curves with fewer discontinuities.

This can also be related to a more

homogeneous particle distribution within the polymer matrix. Moreover, the magnetic
field curves of composites with barium ferrite of smaller particles showed peaks only
over the regions of the notches, which did not occur for barium ferrites without milling
or for cobalt ferrites, i.e., it allowed better signal-to-noise ratio.

CoFe2O4
BaFe12O19 (no grinding)

BaFe12O19 (12 hours)

BaFe12O19 (20 hours)

H (mT)

0
5

10

15

20

25

30

35

d (mm)

Figure 10 Magnetic field curves (mT) versus distance measured in composite plates
with CoFe2O4, BaFe12O19 (no milling), BaFe12O19 (12 h) and BaFe12O19 (20 h) at the 10
mm notch. Arrows indicate the beginning and end of each notch.
19

4. Conclusions
In this study, fiberglass reinforced polymer matrix composite circular plates with
the addition of ferrites (10 wt.%) were produced for magnetic characterization using
magnetic flux leakage (MFL) technique. Barium ferrites were added to the composites
with different particle sizes: without milling and milled in a high-energy mill for 12h
and 20h.

In addition, composite plates were manufactures with cobalt ferrites

synthesized by the Pechini method and the results were compared with those obtained
with barium ferrite. Circular notches of 1, 5 and 10 mm in diameter were introduced on
the composite plates to investigate the potential use of the magnetic characterization
technique for the identification of defects and damages in polymer composites.
According to the results obtained, changes in the magnetic signal of samples
with 10 wt.% of cobalt ferrite were reproducible and characteristic for all notch sizes
studied. For composites with barium ferrite, 5 and 10 mm notches were detected with
all particle sizes analyzed, and the magnetic signal showed good correlation with the
location and size of the notches. However, the notch of 1 mm was detected only for
larger particle sizes (micrometric clusters formed by particles of approximately 0.75
m). For composite plates with barium ferrite milled for 12 and 20 h, 1 mm notch did
not produce a significant variation in the magnetic field, suggesting that the milling of
particles did not favor the detection of smaller notches. Nevertheless, the smaller
particle size allowed producing smoother magnetic curves with variations only over the
notch regions and therefore a better signal-to-noise ratio. Moreover, smaller variation in
the baseline is expected with narrower particle size distribution and better particle
dispersion in the polymer matrix. The overall results indicate that the proposed
technique has great potential for the detection of defects and damages in polymer matrix
composites by using non-destructive magnetic testing.
20

Acknowledgments
This study was supported by the National Council for Scientific and
Technological Development (CNPq-BRAZIL) through the Petrobras Technology
Award (5th Edition). Special thanks to FERMAG Ltda for the donation of the barium
ferrites.
References
[1] HOSSAIN ME (2011) The current and future trends of composite materials: an
experimental

study.

Journal

of

Composite

Materials

45:2133-2144.

doi:

10.1177/0021998311401066
[2] YANG C (2000) Design and analysis of composite pipe joints under tensile loading.
Journal of Composite Materials 34:332-349. doi: 10.1177/002199830003400404
[3] PERREUX D, SURI C (1997) A study of the coupling between the phenomena of
water absorption and damage in glass/epoxy composite pipes. Composites Science and
Technology 57:1403-1413. doi: 10.1016/S0266-3538(97)00076-6
[4] FROST SR, CERVENKA A (1994) Glass fiber-reinforced epoxy matrix filamentwound pipes for use in the oil industry. Composites Manufacturing. 5:73-81. doi:
10.1016/0956-7143(94)90058-2
[5] HUANG YD, FROYEN L, WEVERS M (2001) Quality control and non-destructive
test in metal matrix composites. Journal of Nondestructive Evaluation, v. 20:113-132.
doi: 10.1023/A:1013503005743
[6] AMENABAR I, MENDIKUTE A, LPEZ-ARRAIZA A, LIZARANZU M,
AURREKOETXEA J (2011) Comparison and analysis of non-destructive testing
techniques suitable for delamination inspection in wind turbine blades. Composites: Part
B 42:1298-1305. doi: 10.1016/j.compositesb.2011.01.025
[7] BAYRAKTAR E, ANTOLOVICH SD, BATHIAS C (2008) New developments in
non-destructive controls of the composite materials and applications in manufacturing
engineering.

Journal

of

Materials

Processing

Technology

206:30-44.

doi:

10.1016/j.jmatprotec.2007.12.001
21

[8] GLORIA NBS, AREIZA MCL, MIRANDA IVJ, REBELLO JMA (2009)
Development of a magnetic sensor for detection and sizing of internal pipeline corrosion
defects. NDT & E International 42:669-677. doi: 10.1016/j.ndteint.2009.06.009
[9] SUGIMOTO M (1999) The Past, Present, and Future of Ferrites. Journal of the
American Ceramic Society 82:269-280. doi: 10.1111/j.1551-2916.1999.tb20058
[10] B.E. WARREN: X-Ray diffraction. London: Dover Publications, 1990
[11] JCPDS-ICDD Card, International Centre for Diffraction Data, Newtown
Square,PA, 2002
[12] L. Lutterotti, Total pattern fitting for the combined size-strain-stress-texture
determination in thin film diffraction, Nuclear Inst. and Methods in Physics Research,
B, 268, 334-340, 2010.
[13] MOU'AD A. TARAWNEH, SAHRIM HAJI AHMAD, YU LI JIUN, RADWAN
DWEIRI, IBRAHIM N. HASSAN (2014) Morphology and Mechanical Properties of
NiZn Ferrite/Thermoplastic Natural Rubber Composite. Advanced Materials Research.
308-312. doi: 10.4028/www.scientific.net/AMR.925.308
[14] ASIRI, A. M., HUSSEIN, M. A., ABU-ZIED, B. M. AND HERMAS, A.-E. A.
(2014), Enhanced coating properties of Ni-La-ferrites/epoxy resin nanocomposites.
Polym Compos. doi: 10.1002/pc.23095
[15] ANGELOS CHRISTOPOULOS, EVANGELOS HRISTOFOROU AND GEORGE
TSAMASPHYROS (2012). Strain sensing capabilities of iron/epoxy composites. Smart
Materials and Structures 21 085030,. doi:10.1088/0964-1726/21/8/085030
[16] V. SEPELAK et. al. (2014) The mechanically induced structural disorder in barium
hexaferrite, BaFe12O19, and its impact on magnetism. Faraday Discussions. 170:121135. doi: 10.1039/c3fd00137g
[17] BRICEO S, BRAMER-ESCAMILLA W, DELGADO GE, PLAZA E,
PALACIOS J, CAIZALES E (2012) Effects of synthesis variable on the magnetic
properties of CoFe2O4 nanoparticles. Journal of Magnetism and Magnetic Materials, v.
324:2926-2931. doi: 10.1016/j.jmmm.2012.04.051

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Graphical abstract

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Highlights

The potential of magnetic flux leakage testing for NDE of polymer composites
with embedded ferrite particles was assessed.
Changes in magnetic signals were reproducible and showed good correlation
with location and size of notches in the material.
Smaller ferrite particles did not favor the detection of smaller notches, but
resulted in better signal-to-noise ratio.

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