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Composites Part B 77 (2015) 268e277

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Composites Part B
journal homepage: www.elsevier.com/locate/compositesb

Experimental analyses of SFRP material under static and fatigue


loading by means of thermographic and DIC techniques
V. Crupi, E. Guglielmino, G. Risitano*, F. Tavilla
 degli Studi di Messina, Dipartimento di Ingegneria Elettronica, Chimica e Ingegneria Industriale, Contrada Di Dio (S. Agata), 98166 Messina, Italy
Universita

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

Article history: The mechanical properties of injection moulded short glass fibre-reinforced polyamide composites was
Received 3 April 2014 investigated using experimental techniques. The Digital Image Correlation technique was applied during
Received in revised form the tensile tests in order to obtain the stressestrain curves and to identify the fracture location at the
3 February 2015
early stages of the tests. Moreover, the thermographic technique was used during the static tests in order
Accepted 16 March 2015
to identify the fracture zone and also during the fatigue tests, carried out at different frequencies, to
Available online 23 March 2015
study the temperature evolution of the specimen. A theoretical model was developed to analyze the
temperature evolution during the fatigue test and the effect of the test frequency. The aim of this study is
Keywords:
B. Fatigue
the application of the Thermographic Method for the fatigue assessment of short glass fibre-reinforced
B. Mechanical properties polyamide composites.
D. Mechanical testing © 2015 Elsevier Ltd. All rights reserved.

1. Introduction Tensile tests were performed by Godara and Raabe [5] using
digital image correlation (DIC) for resolving the mechanical
Today, lightweight and low cost components can be obtained behaviour and spatial distribution of the plastic microstrains in an
with short fibre reinforced plastics. The recyclable nature of these epoxy resin reinforced with 35 wt% short borosilicate glass fibres.
materials by comparison to thermoset matrixes composites is also With the growing interest in lightweight structures, the short
clearly appealing. Restricted a few years ago to automotive appli- fibres reinforced plastics (SFRP) are being used increasingly in load-
cations with limited mechanical requirements, these materials, bearing applications, where the components experience cyclic
filled with glass fibres up to 50% in mass, are now used for struc- loads, so they are prone to fatigue failure in service. Thus, there is an
tural components [1e3]. increasing attention on the design of SFRP components against
Polyamide-6,6 is known for its balance of strength, modulus and fatigue and a more detailed knowledge of their fatigue behavior is
chemical resistance. Both polyamide-6,6 and short E-glass fibre needed. The fatigue mechanisms in short glass fibre reinforced
reinforced polyamide-6,6 composite have many potential applica- polyamide 6 were presented by Horst and Spoormaker [6]. The
tions, such as stressed functional automotive parts (fuel injection fatigue tests of SFRP material are even more time consuming than
rails, steering column switches), safety parts in sports and leisure the tests required for metallic materials because the viscous ma-
(snowboard bindings) and other commercial products where creep terial exhibits a high heat build-up at high frequencies [3,7].
resistance, stiffness, resistance to dynamic fatigue are demanded in Jegou et al. [8] applied a heat build-up protocol on a short fibre
addition to weight saving. reinforced plastic, used for structural automotive applications
The design of short fibre reinforced plastic components for (PA66GF50), and predicted the fatigue properties from the tem-
structural applications requires an accurate knowledge of the perature measurements. A first approach, based on the tempera-
several factors affecting the tensile properties and the fatigue life- ture measurements, was proposed, providing a good correlation to
time. The tensile strength and toughness/impact energy of short the fatigue data obtained according to the classic procedure.
fibre reinforced polymer composites would depend on a number of Esmaeillou et al. [9] performed tensionetension fatigue tests on
factors such as fibre length, interfacial adhesion and properties of SFRP composites at different applied maximum stress and analyzed
components [4]. the specimens at both microscopic and macroscopic scale. The
temperature was measured during cyclic loading using an infrared
camera and also the progressive loss of stiffness was evaluated
* Corresponding author. Tel.: þ39 347 3209239.
E-mail address: giacomo.risitano@unime.it (G. Risitano).

http://dx.doi.org/10.1016/j.compositesb.2015.03.052
1359-8368/© 2015 Elsevier Ltd. All rights reserved.
V. Crupi et al. / Composites Part B 77 (2015) 268e277 269

Nomenclature d phase shift [rad]


ε strain
c specific heat capacity at constant pressure [kJ/(kg K)] ε0 strain amplitude
f frequency [Hz] εf strain failure
t time [s] r density [kg/m3]
tand loss factor s stress [MPa]
D fibre diameter [mm] s1,s2,s3 principal stresses [MPa]
E* complex modulus of elasticity [MPa] smax maximum stress [MPa]
E0 storage modulus of elasticity [MPa] smin minimum stress [MPa]
E00 loss modulus of elasticity [MPa] s0 stress amplitude [MPa]
K slope of DTIeN curve [K] sR tensile strength [MPa]
Km thermoelastic coefficient [MPa1] u angular velocity [rad/s]
L fibre length [mm] Dt* characteristic time increment [s]
N number of cycles DTs_exp experimental temperature increment during static test
Nas asymptotic number of cycles [K]
N* characteristic number of cycles for composite materials DTs_th theoretical temperature increment during static test
R stress ratio [K]
T surface temperature [K] DTd temperature increment during fatigue test [K]
W total work [J] DTas asymptotic temperature increment during fatigue test
Wt thermal work [J] [K]
a thermal linear expansion coefficient [K1] DT* characteristic temperature increment during fatigue
b absorbed energy ratio test of composite materials [K]

during the tests. Moreover, the effects of the frequency and of the and also the authors have a strong background in this filed. They
mean stress on the fatigue strength were evaluated. applied the TM for the fatigue assessment of steels in low cycle [25]
In Ref. [10], Noda et al. studied the fatigue behaviour of short high cycle [26], and very high cycle [27] fatigue regimes and also for
glass-fibre reinforced nylon 66 under stress controlled fatigue tests the fatigue analysis of metallic mechanical components [16].
on the basis of the nonlinear dynamic viscoelasticity measure- This study is the first step of a research aimed at applying the TM
ments. In order to analyze the effect of nonlinear viscoelasticity on for the fatigue assessment of composite materials, obviously taking
the fatigue behavior, quantitative measurements of nonlinear into account that the composites have different and more complex
viscoelasticity, based on Fourier analysis, were carried out. fatigue mechanisms respect to metallic materials.
Sonsino et al. [3] investigated the fatigue strength behaviour of a A review of the scientific results in literature, related to the
short-glass-fibre reinforced polyamide PA66GF35. The authors application of the thermographic techniques to composite mate-
emphasize the importance of monitoring the surface temperature rials have been presented by Vergani et al. [28].
during fatigue testing for this kind of materials. Moreover, they note De Monte et al. [29] investigated the influence of temperature,
that the surface temperature, reached by the specimen during a thickness and fibre orientation on the off-axis behaviour of
fatigue test, must not exceed the value of 35  C in order to obtain PA66GF35 under cyclic loading.
reliable values and not influenced by the possible structural The same material was considered in this study. Tensile tests
changes of the material. were carried out on specimens using a hydraulic testing machine
Handa et al. [11] investigated the temperature evolution of the and DIC and IR Camera have been used during all tests. Stress vs
specimens in PA66GF33 during fatigue tests, carried out at different strain curves and temperature evolution associated to the applied
values of load ratio and test frequency (in the range between 5 and tensile stress were determined. The trend of the surface tempera-
50 Hz). They proposed a model which correlates the stabilization of ture of the specimen during fatigue tests was analyzed at different
the surface temperature with the parameters E0 (storage modulus), test frequencies. The stress range, applied during the fatigue tests,
E00 (loss modulus) and tand (loss factor). was maintained at a constant level below the fatigue limit in order
An energy-based approach was proposed by Meneghetti and to obtain an indication on the amount of energy, which is generated
Quaresimin [12] to analyse the fatigue strength of plain and only by internal material damping.
notched specimens made of a short fibre-reinforced plastic weak-
ened by rounded notches. 2. Static tests
Full-field measurement techniques were applied in Refs. [13,14]
for the damage investigation of composites. 2.1. Material and methods
The traditional methods of fatigue assessment of metallic and
composite materials are extremely time consuming. In order to The material used in this study is a commercial polyamide-6,6
overcome the above-mentioned problems, an innovative approach containing 35 wt% glass-fibres, designed as PA66GF35. Table 1
for fatigue assessment of materials and structures has been pro- shows the mechanical and physical properties of the material;
posed in Ref. [15]: the Thermographic Method (TM). The Thermo- the values are extracted from the manufacturer's datasheet. The
graphic Method, based on thermographic analyses, allows the rapid specimens were made by injection moulding. Granulated com-
determination of the high-cycle fatigue limit [15] and the SeN mercial materials were held in a drying furnace at 60  C ÷ 80  C for
curve [16] of materials, mechanical components and structural 24 h prior to injection. For all blends, the injection parameters were
details, using a very limited number of tests. There are a lot of pa- maintained constant. Dog bone specimens (Fig. 1) were injection
pers [17e24] in literature, which confirm that the TM has been moulded (type 1A of the ISO 527-2:1993 standard) with processing
already used successfully to predict the fatigue strength of metals, conditions based on ISO 294-1:1996 and ISO 1873-2:2007. The
270 V. Crupi et al. / Composites Part B 77 (2015) 268e277

Table 1
Mechanical and physical properties of PA66GF35 according to the manufacturer's datasheet.

Fibre diameter Fibre length Density Specific heat capacity Thermal linear expansion coefficient Tensile strength Elastic modulus Failure strain

D [mm] L [mm] r [kg/m3] c [kJ/(kg K)] a [1/K] sR [MPa] E [MPa] εf [%]

10 280 1410 1,670 2,50E-05 150 ÷ 210 8700 ÷ 11400 3÷4

specimens were machined out from injection-moulded plates at


orientation angle of 0 . Fibres have a nominal diameter of 10 mm Table 2
Parameters used for DIC analysis.
and an average length of approximately 280 mm.
The static tests were carried out using a servo-hydraulic load Project parameters: Facet
machine at a crosshead rate equal to 2 mm/min with constant Facet shape rectangular
Facet size 12 pixels
relative humidity and temperature. The tensile tests were carried
Facet step 10 pixels
out on 10 specimens using a hydraulic testing machine (MTS 810) Project parameters: Strain
and the DIC technique, which uses a mathematical correlation to Computation size 3
analyse digital images of samples subjected to mechanical strain, Validity quote 55%
Strain computation method Total
has been used during all tests. ARAMIS 3D 2M LT system was used
Stage parameters
to analyze the strain pattern of the specimen surface. Two cameras Accuracy 0.04 pixels
with a resolution of 1600 x 1200 pixel were used. The system ac- Iteration limit Enabled
curacy for the strain measurement is about 104, while the higher Residual gray scale level 20 levels
acquisition frequency is 12 Hz. The main parameters related to the Intersection deviation 0.3
Recording image sequence
characteristics of the facet, the method of calculation and the mode
Simple measuring mode 1 image/s
of acquisition of images are reported in Table 2.
In a second time, the authors have focused their attention on the
influence of the setting parameters by performing an analysis of the
For linear isotropic homogeneous material and in adiabatic
optimization of the post-processing phase. At the conclusion of this
condition, the variation of temperature during the phase I of the
study it was found that it is possible to optimize the analysis using
static test is proportional to the variation of the sum of the principal
higher values for the “facet size” (larger facets) and lower values for
stresses [30]:
the “facet step” (increasing the overlapping area). The study
focused on the shape of the facet. The result was that the rectan-
a
gular shape is the optimal choice. DTs ¼  T $ðs þ s2 þ s3 Þ (1)
Moreover, during tensile tests, an IR camera FLIR SC® 3000 was r$c 0 1
used and the specimens were coated with black paint.
for uniaxial stress state, it follows:

2.2. Theory/calculation a
DTs ¼  T $s ¼ Km T0 $s1 (2)
r$c 0 1
As reported in Ref. [28], there are many studies in literature on
the thermal response of composites during static tests. During where Km is the thermoelastic coefficient.
static tests of common engineering metals, the temperature evo- Clienti et al. [31] for the first time correlated the first deviation
lution on the specimen surface, detected by means of an infrared from linearity, which corresponds to the end of the phase I, to the
camera, is characterized by three phases: an initial approximately fatigue limit of plastic materials. As reported in Ref. [32] “the end of
linear decrease due to the thermoelastic effect (phase I), then the the thermoelastic phase could be related, also for composites, to a
temperature deviates from linearity until a minimum (phase II) and stress value sD, which can identify the initiation of a different kind
a very high further temperature increment until the failure (phase of damage”. This was observed for basalt [32] and glass [33] fibre
III). A typical DTeN curve, obtained by a constant-amplitude fatigue reinforced composites. The SEM analyses on glass-fibre reinforced
test, is shown in Fig. 2. specimens, tested at various load levels, and the measurements of

Fig. 1. Representation of specimen with dimensions in mm.


V. Crupi et al. / Composites Part B 77 (2015) 268e277 271

the fracture zone. For all stage point, the evolution of strain is
constant and gives a good prediction of the failure zone.
During some tensile tests, the temperature of the specimen
surface was detected by means of an IR camera. Fig. 4 shows the
pattern of the applied stress and the experimental temperature
increment DTS_exp, detected by means of the themocamera, during a
tensile test and some infrared images of the specimen. Comparing
the images obtained by thermographic (Fig. 4) and DIC (Fig. 3)
techniques, it is clearly evident that the infrared analysis gives less
accurate results for the prediction of the fracture zone than those
obtained by means of DIC technique. After a nonlinear initial part of
the DTS_expet curve, probably due to the stabilization of the grips of
the testing machine, an approximately linear trend is clearly visible
in the curve and its slope corresponds to the thermoelastic coeffi-
cient Km of eq. (2). A linear regression of this part of the DTS_expet
curve, relative to the phase I, was performed in order to include the
maximum number of thermal data, which allows to get the highest
correlation coefficient (R2 ¼ 0.9618). In the same graph it is re-
ported the theoretical temperature increment DTS_th, obtained
Fig. 2. Theoretical trends of stress and temperature during a static tensile test. applying eq. (1). The values of the parameters (density r, specific
heat capacity at constant pressure c and linear expansion coeffi-
cient a), used for eq. (1), are reported in Table 1. For the investigated
stiffness reduction in interrupted static tests, characterized by two
material, the DTS_expet curve has a different trend respect to the
loadingeunloading cycles, confirmed that the defects do not
linear trend of the theoretical DTS_thet curve when the applied
propagate and the global temperature trend during tensile static
stress is about 55 MPa as shown in Fig. 4.
tests is about linear until the applied stress in lower than sD [34].
Sonsino et al. [3] obtained by experimental tests that the value
of fatigue strength at Nf ¼ 1E6 cycles (R ¼ 1) for PA66GF35 (the
2.3. Results & discussion same material investigated in this study) is 55 MPa. A similar result
of fatigue strength at Nf ¼ 1E6 cycles (R ¼ 1) was obtained by De
Since the DIC technique is able to estimate the displacement Monte et al. [29] for PA66GF35 specimens with thickness t ¼ 3 mm.
field in each region of the specimen, it was applied during the
tensile tests in order to obtain the stressestrain curves and to
detect the failure zone at the early stages of the tests. Fig. 3 shows 3. Fatigue tests
an application of DIC technique during a tensile test. In the figure,
some images, obtained by DIC analysis during the tests, are showed 3.1. Material and methods
along with the stress versus strain curve in order to highlight the
evolution of strain in the fracture zone. Analysing Fig. 3, it can be The specimens, investigated under fatigue loading, have the
noted that even at low strain (about 0.4%) it's possible to identify same geometry (Fig. 1) of those used for the static tests and are

Fig. 3. Stressestrain curve and DIC images for a static tensile test.
272 V. Crupi et al. / Composites Part B 77 (2015) 268e277

Fig. 4. (a) Experimental trends of stress and temperature and IR images during a static tensile test; (b) Temperature evolution versus applied stress levels during a static tensile test.

made from the same material by injection moulding as reported in internal material damping due to the viscoelastic nature of the
paragraph 2.1. material itself.
The trend of the surface temperature of the specimen was For fatigue tests, the following parameters were used:
analyzed at five different test frequencies (1,3,6,9 and 12 Hz). The maximum stress smax ¼ 20 MPa; load ratio R ¼ 1; test frequency
stress range, applied during the tests, was maintained at a constant f ¼ 1,3,6,9 and 12 Hz.
level (20 MPa) below the fatigue limit [3] in order to obtain an As previously mentioned, the specimens were coated with black
indication on the energy amount, which is generated only by paint and during the test the surface temperature of the specimen
V. Crupi et al. / Composites Part B 77 (2015) 268e277 273

was monitored with an IR camera. When the surface temperature


of the specimen got to the stabilization, the test was stopped. s0 eiðutþdÞ  *  id
E* ¼ ¼ E e (5)
ε0 eiut
The complex modulus can be split up into a real component E0
3.2. Theory/calculation and the imaginary component E00 :
00
During HCF tests of common engineering metals, the tempera- E* ¼ E0 þ jE (6)
ture evolution on the specimen surface, detected by means of an
infrared camera, is characterized by three phases when the spec- The ratio between E0 and E00 gives the loss factor:
imen is cyclically loaded above its fatigue limit: an initial rapid
E0
increment (phase I), a plateau region (phase II), then a very high tan d ¼ 00 (7)
further temperature increment until the failure (phase III). The E
same trend was observed for metals by Crupi et al. in LCF [25] and The integration of stress over strain of one loading cycle gives
VHCF [27] regimes. the total work W:
For that concerns the SFRP composite materials, the tempera- Z
ture evolution during the fatigue tests is different [11]; after an W¼ sdε (8)
initial linear increment (phase I), there is another linear increment
with lower slope (phase II). The theoretical DTdeN curves, obtained
for steel and SFRP composite during constant-amplitude fatigue which finally leads to a relation between the total work on the time
tests, are shown in Fig. 5. The intersection between the two linear and loss factor expressed by:
trend gives the values of cycle number and temperature increment,
vW
defined in Fig. 5 as N* and DT*, which is not exactly an asymptotic ¼ p$f $s0 $ε0 $sin d (9)
vt
temperature increment.
Following the work of Chandra et al. [35], the main mechanisms Rittel et al. [36] had showed that only a part of the absorbed
that produce damping effects in SFRP are: the viscoelastic nature of energy W converts to thermal energy Wt. This part of absorbed
the polymer matrix, damping due to interphase effects between energy is expressed by the factor b:
fibre and matrix, damping due to damage and thermoelastic 
damping. The total work W being absorbed by the material during vWt vW
b¼ (10)
one cycle can be determined from the hysteresis in the stresse- vt vt
strain curve.
Under adiabatic condition, the thermal energy rate causes the
Damping causes a part of the mechanical work to be irreversibly
material to heat up with the temperature rate:
absorbed by the material during a fatigue test (loading and
unloading process). This finally heats up the material, which can be vT 1 vWt
measured by infrared thermography or other system instruments. ¼ (11)
vt r$c vt
Under sinusoidal loading, the stress s and the strain ε (they are
functions of the time) can be written as: where r is the density and c the specific heat capacity of the
material.
s ¼ s0 eiðutþdÞ (3) Thus, the relationship between temperature and frequency is:

vT p
ε ¼ ε0 eiut (4) ¼b f $s0 $ε0 $sin d (12)
vt r$c
where s0 and ε0 are the stress and strain amplitudes, u is the being the number of fatigue cycles N related to frequency f and
angular velocity, d is the phase shift and t is the time. time t:
The complex modulus E* is the ratio between s and ε:
vT p
¼b $s $ε $sin d (13)
vN r$c 0 0
Then, a new parameter K can be introduced:

p
K¼b s $ε $sin d (14)
r$c 0 0
According to the definition of the parameters N* and DT*, shown
in Fig. 5, it follows:

DT* ¼ K$N* (15)

3.3. Results & discussion

According to the developed model, the characteristic thermal


parameter is DT*. Fig. 6 shows the experimental and theoretical
DTdeN curves necessary to define the values of N* and DT*. The
temperature trend of test performed at 1 Hz is not reported because
Fig. 5. Theoretical DTdeN curves for steel and SFRP composite during a fatigue test. the value of DTd is very low. The theoretical curves were computed
274 V. Crupi et al. / Composites Part B 77 (2015) 268e277

Fig. 6. Experimental and theoretical DTdeN curves during the fatigue tests.

Table 4
for each test by means of a linear interpolation of the data relative
Theoretical and experimental values of K [K].
to the two phases of the DTdeN curves (Fig. 5), obtaining the values
of N* and DT* and the slope K. Moreover, a theoretical value of the Theoretical value Experimental value

slope K was calculated using eq. (14). The values of the parameters f ¼ 3 Hz f ¼ 6 Hz f ¼ 9 Hz f ¼ 12 Hz
(density r, specific heat capacity at constant pressure c and absor- 0.00060 0.00058 0.00065 0.00065 0.00065
bed energy factor b), used for eq. (15), are reported in Tables 1 and 3 Deviation [%] 4.7% 7.9% 7.4% 8.1%
[11]. Table 4 shows the comparison between the theoretical and
experimental values of K. A good achievement was obtained with a
percentage deviation lower than 8%. The results confirm that, as In Ref. [37], Crupi developed a theoretical model able to describe
show in Fig. 6, the slope K is almost the same for all the tests carried the temperature evolution during the phase I and phase II of the
out at different frequencies. Table 5 reports the values of N* and DT*. fatigue life:
The value of DT* increases with increasing the test frequency. Fig. 7
shows the correlation between DT* values and the corresponding f  
DTd ¼ DTas $ 1  e t
N
(16)
values; as show in equation (12) and in Ref. [7], DT* is related to the
test frequency f by means of a linear relationship. These results
confirm the validity of the theoretical model applied to SFRP ma- where t is a constant; if N is t then DTd is 0.63 DTas and if N is 4t
Dt * ¼N * , then DTd is 0.98 DTas. The model was applied successfully to steels
terials. Moreover, the values of time f
required to reach the
in Ref. [37]. In order to apply eq. (16) on SFRP materials, the pa-
temperature increment DT* for each test, are reported in Table 5. It rameters N* and DT* were considered instead of Nas and DTas and it
is interesting to note that Dt* has an almost constant value for all was necessary to find the correct convergence criterion as a func-
the tests performed at different frequencies but at the same envi- tion of the relationship between N* and t parameters. Fig. 8 shows
ronmental testing conditions. the experimental DTdeN curve and other five curves, obtained

Table 3
Mechanical properties of PA66GF35 [11].

Absorbed energy ratio b [/] Storage modulus of elasticity E0 [MPa] Loss modulus of elasticity E00 [MPa] Loss factor tand [/]

0.15 5000 340 0.068


V. Crupi et al. / Composites Part B 77 (2015) 268e277 275

Table 5
Characteristic values considered in the theoretical approach.

Test frequency Characteristic temperature increment Characteristic number of cycles Characteristic time increment

f [Hz] DT* [ C] N* [/] Dt* ¼ N*/f [s]


3 0.55 1000 333
6 1.20 2000 333
9 2.10 3000 333
12 2.50 4000 333

Fig. 7. Correlation between the temperature increment DT* and the frequency f with some IR images.

considering different values of the ratio between N* and t. By the Combining and developing the equation (16) with equation (15),
analysis of the results, it was found that the best convergence cri- it follows:
terion is obtained when t ¼ 1.5,N*. Applying this criterion for all
tests (Fig. 9), a good agreement between the experimental data and  
DTd ¼ K$N * $ 1  e t
N
(17)
the theoretical model proposed by Crupi [37] is obtained.
Considering eq. (15) and t ¼ 1.5,N*, the equation (17) can be
written as:

p  
 N
DTd ¼ b s0 $ε0 $sin d$N * $ 1  e 1;5$N* (18)
r$c
Considering Dt* a constant value for all frequencies:

N* ¼ Dt * $f (19)

the equation (18) can be written as:

 
p  N
DTd ¼ b s0 $ε0 $sin d$Dt * $f $ 1  e 1:5$Dt $f (20)
r$c

which describes the temperature evolution during the fatigue life


of the investigated SFRP materials as a function of the material's
properties (b, r, c, sin d), of the load condition (s0, ε0, f) and char-
Fig. 8. Experimental data and DTdeN curves, predicted considering different values of acteristic time increment Dt*. The temperature evolution of a
the ratio between N* and t. PA66GF35 composite, subjected to different fatigue loading
276 V. Crupi et al. / Composites Part B 77 (2015) 268e277

Fig. 9. Experimental data and DTdeN curves, predicted using the theoretical model proposed by Crupi [37].

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