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Color Research Application - 2021 - Nikam - Assessment of The Factors Affecting The Weathering Properties of Pigment
Color Research Application - 2021 - Nikam - Assessment of The Factors Affecting The Weathering Properties of Pigment
DOI: 10.1002/col.22671
RESEARCH ARTICLE
KEYWORDS
artificial weathering, color fading, organic pigments, pigment dispersion
Color Res Appl. 2021;46:1313–1320. wileyonlinelibrary.com/journal/col © 2021 Wiley Periodicals LLC. 1313
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1314 NIKAM ET AL.
function of binders is to hold the pigments, extenders etc. added and mixed at low speed of 500 rpm for
intact with the surface.4 Pigments provide color and optical 10 minutes on the dispermat. The powder ingredients
properties (opacity, reflectance) to the paint film.5 The pig- pigment, extender followed by rheology additive were
ments are also more susceptible to the heat. Exposure of the added, the mixture was mixed well for 10 minutes at
pigment to the heat results into the change in the crystal 800 rpm. Grinding was performed for 30 minutes at
structure which then leads to the fading of shade.6 Gener- 3000 rpm. The chilling (by circulation of cool water)
ally, the pigment or pigment particle surface is modified was provided during grinding stage to maintain tempera-
with functional moieties to enhance the performance prop- ture of mixer between 8 C to 25 C.
erties of the pigments.7 Inorganic pigments have low
chroma and tinting strength but they have good hiding
power, excellent lightfastness, and chemical resistance, 2.3 | QUV/ATLAS panel preparation and
whereas organic pigments have bright color, and the paint application
weather fastness is inferior compared to the inorganic
pigments.8,9 Among the various chemistries of organic The preparation of the primer for panel application
pigments, monoazo yellow pigments possess inferior started with 100 mL of water-based primer (acrylic emul-
weather fastness and chemical resistance.10,11 However, sion based, pigment volume concentration [PVC] 70%,
there were efforts to improve the storage stability, and parti- and coverage 30-33 m2/L) in a 200 mL metal container.
cle size stability of Pigment Yellow 74 (PY 74) by controlling This was diluted at 1:1 with water, and was mixed well
the crystal structure parameters.12 Besides that, the other using gyro shaker for 5 minutes.
parameters such as deviations in the quality of pigments For the prepation of the exterior paint for panel appli-
among the different manufacturers, surface preparation, cation, 100 mL of acrylic emulsion exterior paint (PVC
etc. will also lead to fading of the color. Generally artificial 40%, and coverage 16-18 m2/L) and 10 mL of pre-
weathering (UV chambers from Q-Labs [QUV], and pared PY 74 colorant were placed in a 200 mL metal con-
weather-O-meter from ATLAS) tests are performed to these tainer; then mixed well using gyro shaker for 5 minutes.
pigment dispersions to understand their performances. This paint was diluted at 1:0.4 with water and mixed well
Here in this article, pigment dispersion of monoazo for 3 minutes with a spatula.
yellow pigment (PY 74) was prepared using PY 74 from Fiber cement panels of dimension 150 mm × 75 mm
different manufacturers. The effect of various factors for QUV, and 145 mm × 65 mm for ATLAS were used in
such as temperature during dispersion process, alkalinity the study. The fiber cement panels were cleaned thor-
of the QUV and ATLAS panels, and surface preparation oughly under running tap to clean the dirt from the sur-
of QUV and ATLAS test panels on the fading of the color- face. These panels were then allowed to dry overnight at
ants is studied. room temperature. A single coat of primer was applied
by brush on these panels, and allowed to dry for 4 hours
at room temperature. This was followed by two coats
2 | EXPERIME N TAL METH OD (applied by brush) of acrylic emulsion exterior paint with
an interval of 8 hours between two coats. Then panels
2.1 | Materials were allowed to cure at room temperature for 7 days
before subjecting them to the ATLAS and QUV
The PY 74 from three different manufacturers, calcium chambers.
carbonate as extender, attapulgite as thickener,
ethoxylate of fatty oil ester, fatty acid modified emulsifier,
and soya lecithin as wetting and dispersing agents, bio- 2.4 | Characterization
cides, defoamer as additives, and DM water are used in
the study. All the raw materials are of commercial grade Infrared (IR) spectroscopy: Infrared spectra are recorded
and used as received; manufacturers details are not given using IR spectrometer from PerkinElmer. The samples
to avoid product promotion. for IR spectroscopy were prepared by grinding pigment
and KBr using mortar and pestle, and then made pellet
by using pellet die.
2.2 | Pigment dispersion Particle size: Mastersizer 2000 from Malvern instru-
ment, which operates on static light scattering principle,
Pigment dispersions were prepared in 1 L stainless steel- was used to record the particle size distribution. The sample
jacketed vessel using high speed disperser (Dispermat- was prepared by dispersing 0.5 g of pigment in 10 mL of 1%
VMA-Getzmann, Germany). Liquid ingredients were sodium lauryl sulphate solution by sonication for 1 minute.
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NIKAM ET AL. 1315
Scanning electron microscopy: Field-emission scan- scanning electron microscopy and energy dispersive X-
ning electron microscopy and energy-dispersive X-ray ray analysis. IR spectra for these three different manu-
(FESEM and EDX) analysis of the PY 74 pigment from facturers are shown in Figure 1 (IR spectra are split in
different manufacturers were carried out using Jeol to two regions for better clarity). There is no signifi-
7100F. The dispersion was prepared by sonicating the cant difference in IR spectral features except spectral
pigment in water at 33 kHz for 5 minutes using a features near 1650 cm−1 which are the characteristics
sonicator from Telsonic Ultrasonics, and then a drop of of olefinic group observed.
the dispersion was placed on double-sided tape pasted on Particle size distributions for pigments received from
stub, and was allowed to dry. Platinum sputter coating three different manufacturers are shown in Figure 2. Par-
for 30 seconds at 20 mA was given to the samples. ticle size distribution near 200 nm is quite similar among
Spectrophotometer (Gretag Macbeth Color-Eye these three pigments. However, the difference in particle
7000A and software Propallete 3.3) was used to record size distribution can be observed between 1 and 90 μm.
the color differences of the panels. QUV-accelerated The morphology and elemental analysis were per-
weathering test machine from Q-Lab USA (Operational formed for the PY74 pigments. Scanning electron micro-
conditions—Condensation at 45 C, and UV at 50 C, scopic images and EDX spectrum are shown in Figure 3.
Irradiance—0.55 watts/m2/nm, UV radiation source— SEM image of PS2 shows that, the particles are uniform
UVB 313 EL), and ATLAS chamber (operational in shape, and EDX analysis shows only carbon and oxy-
conditions—6500 W water cooled Xenon Arc burner, gen elements arising from pigment particles. Whereas
humidity of 60%-80%, black panel temperature of 63 C,
irradiance of 0.5 watts/m2/nm, 100 minutes of dry
cycle with continuous radiation followed by 15 minutes
of water spray under the continuous radiation)
were used.
The panels were taken out at regular intervals for
recording the color difference using spectrophotometer,
the water droplets on the panels were wiped out gently
using tissue paper, and the panels were allowed to cool
down to room temperature before recording the color dif-
ference. The coloristic values were recorded and stored in
the spectrophotometer.
3 | R ES U L T S A N D D I S C U S S I O N
F I G U R E 1 Infrared spectra
of Pigment Yellow (PY 74)
pigment from three different
manufacturers PS1, PS2, and
PS3 at figure print to bending
vibrations (A), and stretching
vibrations (B)
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1316 NIKAM ET AL.
F I G U R E 3 Scanning electron microscopy and energy-dispersive X-ray (EDX) analysis of PS1, PS2, and PS3. EDX spectra are given for
2 difference spots for PS1 and PS2 to differentiate the pigment and plate-like structures. No plate-like structures found for PS2
SEM images of PS1 and PS3 shows plate-like structures oxygen arising from pigment particles, and the plate-like
in addition to regular uniform particles. EDX analysis of structures contained mostly aluminum, and silicon might
regular uniform particles are mostly of carbon and be from extender/additives. The main difference between
15206378, 2021, 6, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/col.22671 by Egyptian National Sti. Network (Enstinet), Wiley Online Library on [05/02/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License
NIKAM ET AL. 1317
qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
PS1 and PS3 is that, the size and abundance of plate-like
ΔE ab = ðL2 −L1Þ2 + ða2 −a1Þ2 + ðb2 −b1Þ2 ð1Þ
structures in PS3 is much higher than in PS1.
Pigments from different manufacturers PS1, PS2, and
PS3 were used to prepare pigment dispersions using the sim- where ΔE*ab is the color difference, L (Lightness), a (red-
ilar formulation. Initial colorimetric values L, a, b, and the ness/greenness), and b (yellowness/blueness) are stan-
ΔE*ab (the color difference of reference and experimental dard CIE coordinates. Throughout this article ΔE refers
QUV panels, here in this case, the initial readings of QUV to the CIELAB color difference, which is given by Equa-
panels before placing them in the ATLAS and QUV cham- tion (1).
bers are taken as the reference) of panels were recorded Experiments were conducted to rule out the variation
using spectrophotometer according to the Equation (1).13 in QUV chambers or malfunctioning and set parameters.
These initial readings are stored in the computer and used Pigment dispersion from pigment PS3 was used in the
in subsequent measurements to find the color difference of panel preparation and then the panels were exposed in
the panels exposed to QUV. The panels were prepared and four separate QUV chambers. As shown in Figure 4, no
exposed in duplicate, and the given results are the average of significant difference in ΔE was observed as a function of
two different panels with an experimental deviation <5%. exposure time of 1000 hours.
The QUV-exposed panels were taken out at the time interval The influence of primers and the base paint (clear
of 100, 250, 500, 750, 850, 1000 hours, and the coloristic of base/zero TiO2 base) of different batches on the color dif-
these panels were recorded. ference during the ATLAS and QUV exposure was stud-
ied. Primers of different batches were used while
preparing the panels keeping the pigment dispersion
from PS 3, clear base 1 the same. The influence of the
primer of different batch on the color difference even
after 1000 hours of ATLAS and QUV exposure is very
minimal as shown in Figure 5. Then the panels were pre-
pared with the paints of two different clear bases keeping
the pigment dispersion from PS 3, primer 1 same. Varia-
tion in color difference during the weatherability test for
these panels is shown in Figure 6. There is a slight differ-
ence in ΔE observed as shown in Figure 6B. However,
the difference is less than 1 unit and visually also there
was not much difference found. Since there was no sig-
nificant difference in different lots of primers and clear
bases, no change in color difference/fading was observed.
Since the panels are made up of cement reinforced
with cellulose fibers, the quality of panels may contribute
to the variation in the color difference. The panels of two
different lots were immersed overnight in DM water of
F I G U R E 4 The performance of different QUV chambers for pH 6.8. The panels were removed from the water, and
variation in color difference of pigment dispersion the pH of water was recorded. The pH of water where
F I G U R E 6 Influence of base paint of different batches on F I G U R E 8 Variation of color difference (ΔE) of PY74 from
variation in color difference different manufacturers as a function of exposure time
F I G U R E 9 Images of the ATLAS and QUV panels coated with paint based on pigment dispersion prepared using three different
pigment manufacturers
F I G U R E 1 0 Effect of with cooling and without cooling water F I G U R E 1 2 Difference in color (ΔE) observed for panels of all
circulation during the grinding process on variation in color better and poor factors studied
difference at ATLAS and QUV exposures
reason for PS3 to show superior weather fastness might be
due to the presence of large and high amount of plate-like
particles contained aluminum and silicon as characterized
by SEM and EDX which are shown in Figure 3.
The above observations were tested by combining the
set of better and set of poor performance parameters
studied individually. Set of best factors includes pigment
manufacturer (PS 3), with cooling water circulation dur-
ing the pigment dispersion, along with clear base paint
(Base 1), primer 1, panel lot 1, and set of poor factors
include pigment manufacturer (PS 1), no cooling water
circulation during the pigment dispersion, along with
F I G U R E 1 1 Images of the ATLAS and QUV exposed panels of
clear base paint 1, primer 1 and panel lot 1. Though some
pigment dispersion prepared with and without cooling water
circulation
of the parameters such as clear base, primer, and
ATLAS/QUV panels did not show difference in ΔE when
studied individually, however, when combined these
The major contributors for the difference in ATLAS with pigment of different manufacturer, and the higher
and QUV performance or the color fading are found to be dispersion processing temperature resulted the difference
the quality of pigments sourced from different manufac- in the ΔE as shown in Figure 12.
turers that may arise due to difference in surface treat-
ment, crystal structures, morphology of the particles, and
the temperature during processing of the dispersion. How- 4 | CONCLUSION
ever, IR spectral features and particle size distribution data
did not show any correlation with color difference This article reveals various factors governing the color/
observed. The oil absorption (43-48 g/100 g) and bulk den- shade fading of dispersion of PY 74. The PY 74 pigment
sity (0.24-0.31 g/cm3) of PY74 from three different manu- from different manufacturers was used to prepare the dis-
facturers are not significantly different. The probable persions and the paint was subjected to ATLAS and QUV
15206378, 2021, 6, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/col.22671 by Egyptian National Sti. Network (Enstinet), Wiley Online Library on [05/02/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License
1320 NIKAM ET AL.
weathering test to analyze various factors on color or [12] Hoshino, R, Nagasato, S, Takayama, M, Inoue, S,
shade fading. Among the factors studied, PY 74 from pig- Matsuzaki, S, CI Pigment Yellow 74 (Insoluble Azo Pigment),
ment manufacturers 1 and 2, and/or the higher tempera- and Coloring Composition Using Same. US Patent
20140335358A1, 2014.
ture during the grinding resulted higher color difference.
[13] CIElab, Colorimetry, CIE Pub. No. 15.2 Commission Inter-
ATLAS and QUV panels applied with paint based on Pig- nationale de l'Eclairage, Austria 1986 ISBN:3-900-734-00-3
ment manufacturer 3, and/or the cooling water circulation [14] Lomax SQ. The application of x-ray powder diffraction for the
during pigment dispersion resulted better color retention analysis of synthetic organic pigments. Part 1: dry pigments.
and hence a significantly lower ΔE. There was no contri- J Coat Technol Res. 2010;7:331-346.
bution of primers, and base paint of different batches, [15] Herbst W. Dispersion of organic pigments with modern disper-
ATLAS/QUV panels of different lots, and various QUV sion equipment. Pigm Resin Technol. 1974;3:12-25.
chambers on color/shade fading. These findings will help
in identifying the effect of grinding temperature, and also
AUTHOR BIOGRAPHIES
the approaches for pigment testing for weatherability.