In this work, the influence of climate and weather
factors and natural exposure time at Dong Hoi
(Quang Binh) on UV-Vis spectra, the change of
color, and electric properties of HDPE/m-CaCO3
composites were investigated. The UV-Vis spectra
showed the formation of carbonyl groups and vinyl
groups in HDPE macromolecules of the composites
by their photo-degradation. The surface of the
composites was lightened continuously, the L* and
E* values were increased with increasing natural
exposure time. There was significant loss in both
redness and yellowness of the composites. In the
summer, the composites were affected by solar
radiation more strongly, so the yellowness was
decreased significantly. The dielectric constant,
dielectric loss of the composites were increased and
their electrical breakdown voltage was reduced with
increasing natural exposure time
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Vietnam Journal of Chemistry, International Edition, 55(4): 417-423, 2017
DOI: 10.15625/2525-2321.2017-00483
417
Study on change of color and some properties of high density
polyethylene/organo-modified calcium carbonate composites exposed
naturally at Dong Hoi - Quang Binh
Le Duc Minh
1
, Nguyen Thuy Chinh
2
, Nguyen Vu Giang
2
, Tong Cam Le
1
,
Dau Thi Kim Quyen
1
, Le Duc Giang
3
, Thai Hoang
2*
1
Faculty of Pedagogy Natural Sciences, Ha Tinh University, 447 26/3 street, Ha Tinh, Vietnam
2
Institute for Tropical Technology, Vietnam Academy of Science and Technology
3
Faculty of Chemistry, Vinh University
Received 22 January 2017; Accepted for publication 28 August 2017
Abstract
This paper presents the study on the UV-Vis spectra, change of color and some properties of high density
polyethylene/organo-modified calcium carbonate (HDPE/m-CaCO3) composites exposed naturally in Dong Hoi district,
Quang Binh province (Vietnam). From June 2014 to June 2016, the samples of HDPE/m-CaCO3 composites were
tested naturally on outdoor shelves at Dong Hoi sea atmosphere region (at Dong Hoi, Quang Binh). The change of UV-
VIS spectra, color and some properties of the HDPE/m-CaCO3 composites depend on geographic, weather and climatic
factors (solar radiation, temperature, humidity, etc.). In the UV-VIS spectra, the band at 265 nm showed the formation
of the carbonyl groups such as ketone, lactone carbonyl and aliphatic ester which were occurred in photo-degradation
process of HDPE/m-CaCO3 composites. The results of color change indicated the surface of the samples of HDPE/m-
CaCO3 composites was lightened continuously with increasing natural exposure time and increased in total color
difference value and significant loss in both redness and yellowness. a*, b* values and electrical breakdown of
HDPE/m-CaCO3 composites were decreased while their l*, E, dielectric constant and dielectric loss were increased
with rising natural exposure time. Dielectric constant of HDPE/m-CaCO3 composites was in the range of 1.75 to 2.1
and dielectric loss of HDPE/m-CaCO3 composites went up from 1.7 to 3.2 for 0 to 24 months. The electrical breakdown
of HDPE/m-CaCO3 composites reduced due to the decrease in the relative crystalline degree of the samples caused by
the scission photo-degradation of HDPE macromolecules in HDPE/m-CaCO3 composites for natural exposure time.
Keywords. HDPE/CaCO3 composites, photo-degradation, natural exposure, color change, electric properties, UV-
Vis spectroscopy.
1. INTRODUCTION
High-density polyethylene (HDPE) is currently
the most widely used commercial polymer due to its
superior mechanical and physical properties.
However, its toughness, weather resistance,
processability, and environmental stress cracking
resistance are not good enough, which have thus
limited its application in many high-technology
fields. One measure to improve its properties is
reinforcement with some fillers [1]. Inexpensive
inorganic substances such as calcium carbonate
(CaCO3), mica, wollastonite, glass fiber, glass beads,
jute, and silica (SiO2) are widely used as fillers to
improve mechanical and thermal properties of
polymers in the plastic industry. In recent years
micro-size fillers have attracted great interest, both
in industry and in academia because they often
exhibit remarkable improvement in properties of
materials [2].
HDPE filled with mineral particles also
improves dimensional stability, opacity, and barrier
properties. CaCO3 is the largest volume mineral
used in the polymer industry because of its low cost
and abundance. It is available globally in a variety of
particle shapes, purities, and sizes (macro, micro,
and nano). However, because of its higher polar
nature and higher surface areas, CaCO3 is difficult to
disperse and stabilize in a polymer matrix. Poor
dispersion and adhesion of filler lead to a composite
with poor final physical properties [3, 4]. Therefore,
organo-modification of surface of CaCO3 can help to
improve the interaction and dispersion of CaCO3
into the polymer matrix [5-7].
VJC, 55(4), 2017 Thai Hoang et al.
418
The study on the degradability of linear
polyolefins under natural exposure testing was
reported by Telmo Ojeda [8]. This study showed that
in less than one year of testing, the mechanical
properties of all samples decreased virtually to zero,
as a consequence of severe oxidative degradation,
that resulted in substantial reduction in molar mass
accompanied by a significant increase in content of
carbonyl groups. Rui Yang et al. have studied the
natural photo-oxidation of HDPE composites, with
several inorganic fillers. They concluded that some
inorganic fillers such as CaCO3 and wollastonite,
can stabilize HDPE. The surfaces of the composites
after natural exposure testing became rough and with
cracks. A seriously damaged surface did not
definitely correspond to a great oxidation degree.
The remaining volatile oxidation products of the
photo-oxidized composites were proven to be mostly
a series of n-alkanes [9]. The study on the effect of
natural exposure testing on tensile properties of
kenaf reinforced HDPE composites was reported by
A.H. Umar [10]. Due to better stiffness, Young
modulus of HDPE composites is much higher than
neat HDPE. The micro-cracking on the surface of
HDPE composites can be observed after 200 hours
of testing.
Recently, we have studied the degradation and
stability of HDPE/m-CaCO3 composites under
natural weather condition on outdoor shelves in
Dong Hoi sea atmosphere region (Quang Binh
province) to evaluate the change of their
morphology and properties. In the Fourier
Transform Infrared spectra of the exposed samples,
the absorption peak around 1735 cm
-1
characterizes
the stretching vibration of carbonyl group formed
during natural exposure. The tensile strength and
elongation at break of HDPE/m-CaCO3 composites
were reduced significantly while their Young
modulus, the number of cracks and size of cracks
on the surface of the samples were increased with
increasing natural exposure time. The melting
enthalpy, relative crystalline degree of HDPE/m-
CaCO3 composites were slightly increased during
the first 9 months of natural exposure while their
melting temperature and initial degradation
temperature were decreased [11].
This study reports the results of change in UV-
Vis spectra, color, electrical properties of HDPE/m-
CaCO3 composites exposed naturally in Dong Hoi,
Quang Binh. Here, we chose Dong Hoi, Quang Binh
to investigate the change in properties and
morphology of HDPE/m-CaCO3 because Dong Hoi
has not only the sea climate but also draconic
climate. This is typical climate at the sea atmosphere
region in the north – middle provinces. The
influence of natural exposure time and weather
factors on the above changes HDPE/m-CaCO3
composites were evaluated and discussed.
2. EXPERIMENTAL
2.1. Materials
The materials used in this work were a HDPE
(Daelim, Korea) with melting flow index,
kg16.2/C1900
MFI of 1.20 g.min
-1
, and its density of
0.937 g.cm
-3
; CaCO3 powder with density of 2.7
g.cm
-3
(Minh Duc Chemical Stockshare Co.) was
modified by 0.5 wt.% of stearic acid in solid state
using high intermixer (SHR-100A, Shanghai China)
for 90 minutes at 60-65
o
C and mixing speed of 750-
800 rpm.
2.2. Preparation of HDPE/m-CaCO3 composites
The HDPE/m-CaCO3 (wt./wt.) composites were
prepared by melt-mixing in a Haake internal mixer
at 160
o
C for 5 minutes at Institute for Tropical
Technology (ITT), Vietnam Academy of Science
and Technology (VAST). Immediately after melt-
mixing, the HDPE/m-CaCO3 composites were
pressed by hydraulic heat press machine at a
temperature of 160
o
C and the pressure of 5 MPa to
form sheets with thickness from 1 to 1.2 mm.
2.3. Natural exposure of HDPE/m-CaCO3
composites
The samples of HDPE/m-CaCO3 composites were
exposed starting from June 2014 to June 2016 on
outdoor testing shelves at the Natural Weathering
Station of the Institute for Tropical Technology in
Dong Hoi sea atmosphere region (Quang Binh,
Vietnam). Inclining angle of the shelf in comparison
with the ground was 45 degree as typically shown in
Figure 1, and total exposure time of the samples was
24 months.
Figure 1: View of outdoor exposure testing shelves
at Dong Hoi sea atmosphere region
VJC, 55(4), 2017 Study on change of color and some
419
After every three months, the samples were
withdrawn and stored under standard conditions
before determining their properties and morphology.
The abbreviate samples were M0, M3, M6, M9,
M12, M15, M18, M21, M24 corresponding to 3, 6,
9, 12, 15, 18, 21, 24 months of natural expose,
respectively.
2.4. Characterizations
2.4.1. UV-Vis analysis
UV-Vis spectra of HDPE/m-CaCO3 composites
were recorded on a CINTRA 40 (USA) UV-Vis
GBC scanning spectrophotometer in the range 200-
500 nm at ITT, VAST.
2.4.2. Color measurements
The color parameters of HDPE/m-CaCO3
composites were determined by a ColourTec PCM
(PSM
TM
, United State) according to ASTM D2244-
89 standard. The total color difference ( E) of the
samples was calculated using the following
equations.
2 2 2
* * *E L a b
Where, L
*
= L
*
– L0; a
*
= a
*
– a0; b
*
= b
*
– b0;
And L
*
is a measurement of brightness ( L
*
> 0
for light, L
*
< 0 for dark); a
*
is a measurement of
redness or greenness ( a
*
> 0 for red, a
*
< 0 for
green); b
*
is a measurement of yellowness or
blueness ( b
*
> 0 for yellow, b
*
< 0 for blue); L
*
,
a
*
and b
*
are the color parameters of the natural
exposed sample; L0, a0 and b0 are the color
parameters of the unexposed sample. For each
sample, the color parameters were measured at ten
different positions of the sample to obtain the
average value. The above measurements were
performed at ITT, VAST.
2.4.3. Electric properties
The dielectric parameters of HDPE/m-CaCO3
composites (dielectric constant - ’ and dielectric
loss - tan ) were measured at 1 kHz by TR-10C
machine (Ando, Japan) according to ASTM D150
standard. The volume resistivity and surface
resistivity were conducted on TR 8491 machine
(Takeda, Japan) according to ASTM D257. The
electrical breakdown was carried out on Til-Aii 70-
417 machine (Russia) according to ASTM D149-64
standard. The above experiments were performed
at 25
o
C and humidity about 60 % at ITT, VAST.
3. RESULTS AND DISCUSSION
3.1. UV-Vis spectra
The UV-Vis spectra of HDPE/m-CaCO3 composites
according to natural exposure time at Dong Hoi
(Quang Binh) were presented in figure 2. The UV-
Vis spectra showed an increase of the absorption
intensity of HDPE in the composites between 200
and 300 nm wavenumber. In the UV-Vis spectrum
of initial sample (M0 sample), there was one very
strong absorption band at 226 nm. The absorption at
226 nm must be associated with the π – π* transition
of the ethylenic group of the α,β-unsaturated
carbonyl of impurity chromophores of the enone
type in photo-oxidation degraded HDPE. The
presence of these chromophores had been identified
in the previous studies results [11]. For the exposed
samples, the UV-Vis spectra also had the absorption
band at 226 nm. Interestingly, the formation of a
very broad absorption centred at 265 nm
characterized for the carbonyl groups in HDPE when
increasing natural exposure time. The results from
the UV-Vis spectra indicated the formation of the
carbonyl groups such as ketone, lactone carbonyl
and aliphatic ester which were occurring in photo-
degradation process of HDPE/m-CaCO3 composites.
Figure 2: UV-Vis spectra of HDPE/m-CaCO3
composites according to natural exposure time
The chain scission of the HDPE in the
composites matrix by photo-oxidative degradation of
the polymer via Norrish 1 and 2 reactions. If
degradation of the carbonyl groups proceeds
according to the Norrish 1 reaction, the formed free
radicals can attack the polyolefin (scheme 1) [12],
which may lead to termination via crosslinking or
chain scission. If the degradation proceeds according
to the Norrish 2 reaction, carbonyl groups and
terminal vinyl groups are produced (scheme 2) and
chain scission occurs [12]. The ketones, carboxylic
VJC, 55(4), 2017 Thai Hoang et al.
420
acids, and vinyl groups are the three major
functional groups that accumulate with the photo-
degradation of HDPE macromolecules in HDPE/m-
CaCO3 composites [13]. The formation of carbonyl
groups and vinyl groups can be remarks of HDPE
chain scission.
HDPE CH2 CH CH2
O2, PE
CH2 C CH2
O
H
OH
CH2 C CH2
O
H
OH
CH2 C CH2
O
h
CH2 C
O
+ CH2
h
h
CH2 C
O
CH2 + CO;
Scheme 1: Norrish Type 1 reaction for the
photo-degradation of HDPE [12]
HDPE CH2 CH2 CH CH2 CH2
O2, PE
CH2 CH2 C CH2 CH2
O
H
OH
CH2 CH2 C CH2 CH2
O
h
CH2 C CH3
O
CH +
h CH2 CH2 C CH2 CH2
O
H
OH
h
Scheme 2: Norrish Type 2 reaction for the
photo-degradation of HDPE [12]
3.2. Color change
The change of surface color of HDPE/m-CaCO3
composites depends on their structure and
composition (the chemical composition change leads
to the changes in electric, thermal, and color
properties) [14]. The change in values for three color
parameters ( L
*
, a
*
and b
*
) as well as the total
color change ( E) of the composites as a function of
natural exposure time was displayed in table 1 and
figure 3.
Figure 3: The a
*
, b
*
, L
*
and E value of
HDPE/m-CaCO3 composites according to natural
exposure time
The surface of the samples of HDPE/m-CaCO3
composites was lightened continuously, the L
*
and
E values were increased with increasing natural
exposure time. The changes in E
values for the
samples were found to be consistent with the change
in L
*
values. The results of color change indicated
that the surface of the samples of HDPE /m-CaCO3
composites was faded continuously with increasing
natural exposure time expressed by a constant
increase in L
*
value and significant loss in both
redness and yellowness. This phenomenon may be
due to the change in morphology and existence of
double bonds, chromophore groups and
heterogeneous structures inside the HDPE
macromolecules during photodegradation HDPE/m-
CaCO3 composites. These groups affect the visible
light absorbability, leading to the variation in visual
color of the composites.
The b
*
value of HDPE/m-CaCO3 composites
was decreased significantly with natural exposure
time. This decrease indicated a loss in yellowness.
Two distinguished periods of lightness decrease: one
between the third and ninth months (from September
2014 to March 2015) and another between the
fifteenth and twenty-first months (from September
2015 to March 2016). After 3 and 9 months of
natural exposure testing, the b
*
values of HDPE/m-
CaCO3 composites were 0.86 and 0.26, respectively.
Similarly, when natural exposure time was reached
up to 15 and 21 months, the b
*
of HDPE/m-CaCO3
composites were -1.8 and -2.08, respectively. The
winter and spring months were characterized by
gradual increase of rainfall and decrease of solar
radiation (table 2). The significant decrease of the
b
*
value was observed for the samples exposed
from 9 to 15 months and from 21 to 24 months.
After 9 and 15 months of natural exposure testing,
the b
*
of HDPE/m-CaCO3 composites were 0.26
and -1.80, respectively. When natural exposure time
was reached up to 21 and 24 months, the b
*
of
HDPE/m-CaCO3 composites are -2.08 and -2.85,
respectively (table 1). In the summer, the average
temperature/month and average sunny hours/month
are higher, thus the samples have been affected by
solar radiation more strongly. This caused the faster
photo-degradation of HDPE/m-CaCO3 composites,
thus, their b
*
values were decreased significantly.
The average temperature, the relative humidity,
the total rainfall and total hours of sunlight at Dong
Hoi (Quang Binh) in the period from 2014-2016
were demonstrated in table 2. It is clearly seen that,
from ninth to fifteenth months and from twenty-first
to twenty-fourth months of natural exposure, the
highest temperature is from 27.2 to 38.6
o
C and 35.2
to 36.5
o
C, total sunlight hours were quite high, 1208
and 493 hours, respectively. The high intensity of
VJC, 55(4), 2017 Study on change of color and some
421
solar radiation could make a significant contribution
to the photodegradation in amorphous part of
HDPE/m-CaCO3 composites.
Table 1: The change of a
*
, b
*
, L
*
and E
*
value of HDPE/m-CaCO3
composites according to natural exposure time
Samples M3 M6 M9 M12 M15 M18 M21 M24
a
*
3.27 2.63 2.33 2.05 1.71 1.41 1.21 1.11
b
*
0.86 0.59 0.26 -0.86 -1.80 -1.96 -2.08 -2.85
L
*
2.99 3.31 3.77 5.27 7.22 7.62 7.98 9.24
E 4.03 4.26 4.44 5.71 7.64 8.00 8.33 9.73
Table 2: Climate and weather database at Dong Hoi (Quang Binh) from June 2014 to June 2016
Times
Ttb
(
o
C)
Tx
(
o
C)
R
(mm)
Rx
(mm)
Utb
(%)
E
(mm)
S
(h)
St
(d)
CC
(d)
2014
June 30.9 39 78 41 67 163 191 22 0
July 30.1 37.5 85 31 71 137 220 12 0
August 29.6 38.5 132 60 72 134 176 11 0
September 29.6 38.5 132 60 72 134 176 11 0
October 25.6 32 605 189 87 57 129 0 0
November 24.2 30 344 160 88 48 106 0 0
December 19.2 25.8 160 48 82 70 35 0 0
2015
January 18.8 25 84 42 84 55 130 0 0
February 20.7 27.2 40 9 91 28 64 0 0
March 24.2 36.7 32 24 90 39 100 0 0
April 25.6 41 206 133 85 72 173 8 0
May 31 40.5 9 6 70 176 298 18 0
June 30.9 39.5 73 36 69 153 290 22 0
July 29.1 39.3 88 15 72 136 106 9 0
August 29.6 38.6 36 19 76 114 241 8 0
September 28.8 38.6 567 194 81 93 204 6 0
October 25.8 32.8 95 36 81 79 170 0 0
November 25.5 31 339 68 86 49 143 0 0
December 21.2 29.2 79 47 85 55 75 0 0
2016
January 19.8 27.3 70 44 89 35 48 0 0
February 17.6 35.2 8 4 80 70 82 1 0
March 20.6 28.5 16 4 89 36 80 0 0
April 25.7 40 53 36 87 53 169 3 0
May 28.4 36.5 75 38 80 92 244 3 0
June 31.0 38.5 119 63 70 117 260 13 0
Ttb, Tx: Average and highest temperature; R, Rx: Rainy total and highest rainy quantity in day;
Utb: Average humidity; e: Steam quantity; S: Sunny hours; St: Storm; CC: Day numbers have drizzle.
3.4. Electric properties
3.4.1. Dielectric parameters
The frequency dependence of dielectric constant of
HDPE/m-CaCO3 composites according to natural
exposure time was shown in figure 4a. It can be seen
that the effective dielectric constant of the M0
sample was very weakly dependent on frequency,
which is the typical characteristic of non-polar
VJC, 55(4), 2017 Thai Hoang et al.
422
polymers. The M0 sample contained non- dipolar
units and there were not frequency characteristics in
the range of 100-10
6
Hz. For the exposed samples,
the interfacial polarization can cause an increase of
dielectric constant when compared with the M0
sample. When the chains of HDPE in HDPE/m-
CaCO3 composites were scissed, the free volumes
could be decreased and may cause the increase of
dielectric constant. Additionally, it was caused by
the formation of the carbonyl groups such as ketone,
lactone carbonyl and aliphatic ester occurring in
photo-degradation process of HDPE/m-CaCO3
composites. When increasing natural exposure time,
the charge carriers in composites were increased.
This contributed to the rise of dielectric constant of
the samples.
The dielectric loss of HDPE/m-CaCO3
composites was increased with increasing natural
exposure time and frequency because a higher
frequency voltage can yield higher electrical
conductivity as shown in figure 4b. Unlike the
dependence of dielectric constant, an unclear
correlation of dielectric loss which can be stated (the
dielectric loss of the samples can increase or
decrease when increasing natural exposure time) and
immobility of charge carriers in the samples. There
were two competitive factors that affect the
dielectric loss of the samples such as hindrance in
charge transport and the incorporation of charge.
The incorporation of large volume fraction of
interfaces and polymer chain entanglement which in
turn cause immobility of charge carriers or reduction
in electrical conductivity, and thus causing a
reduction of dielectric loss. On the other hand, the
agglomeration of volume fraction can also result in
an apparent reduction of interface area of the
samples. Therefore, the effect of immobility of
charge carriers on reduction in electrical
conductivity is far less important than the influence
of charge carriers, which causes an increase of
dielectric loss of the samples.
3.4.2. Electrical breakdown voltage
The electrical breakdown voltage data of HDPE/m-
CaCO3 composites were performed in table 3. The
value of electrical breakdown voltage of the samples
was decreased gradually with increasing natural
exposure time. This observation is of vital
importance for engineering application because the
dielectric rupture always occurs at the weakest
points. In other words, the real dielectric strength of
the samples is determined by the weakest part of
their insulation.
Figure 4: Frequency dependence of dielectric
constant (a) and dielectric loss (b) of HDPE/m-
CaCO3 composites according to natural exposure
time
Firstly, when increasing natural exposure time,
the relative crystalline degree of the samples was
reduced. This can be explained by the scission
photo-degradation of HDPE macromolecules in
HDPE/m-CaCO3 composites leading to decrease
crystalline regions of HDPE/m-CaCO3 composites
as shown in previous research [11]. In the result, the
intrinsic strength of the samples was decreased.
Secondly, the mobility of charges in the HDPE/m-
CaCO3 composite insulation is much higher with
increasing natural exposure time. Therefore, the
charges are wider distributed in the HDPE/m-CaCO3
composites and the screening effect is less
pronounced. The above reasons make decrease of
the electrical breakdown voltage of the composites
according to natural exposure time (table 3).
Table 3: Electrical breakdown voltage data of HDPE/m-CaCO3
composites according to natural exposure time
Samples M0 M3 M6 M9 M12 M15 M18 M21 M24
E (kV/mm) 24.17 21.89 21.55 18.33 17.54 17.04 16.46 15.68 14.39
VJC, 55(4), 2017 Study on change of color and some
423
4. CONCLUSIONS
In this work, the influence of climate and weather
factors and natural exposure time at Dong Hoi
(Quang Binh) on UV-Vis spectra, the change of
color, and electric properties of HDPE/m-CaCO3
composites were investigated. The UV-Vis spectra
showed the formation of carbonyl groups and vinyl
groups in HDPE macromolecules of the composites
by their photo-degradation. The surface of the
composites was lightened continuously, the L* and
E* values were increased with increasing natural
exposure time. There was significant loss in both
redness and yellowness of the composites. In the
summer, the composites were affected by solar
radiation more strongly, so the yellowness was
decreased significantly. The dielectric constant,
dielectric loss of the composites were increased and
their electrical breakdown voltage was reduced with
increasing natural exposure time.
Acknowledgement. The authors thank Vietnam
Academy of Science and Technology for supporting
this research and National Center of Hydro-
Meteorological Service for providing the weather
and climate data.
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1589-1594 (2009).
Corresponding author: Thai Hoang
Institute for Tropical Technology
Vietnam Academy of Science and Technology
No. 18, Hoang Quoc Viet Road, Cau Giay Dist., Ha Noi
E-mail: hoangth@itt.vast.vn.
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