Jurnal Rekayasa Kimia dan Lingkungan

(Journal of Chemical Engineering and Environment)

Volume 18, Number 1, Page 29 – 36, January – June 2023
ISSN 1412-5064, e-ISSN 2356-1661
https://doi.org/10.23955/rkl.v18i1.28648

Precipitation Synthesis of Cerium Oxide Nano Pigment

Iis Nurhasanah1*, Yayuk Astuti2, Pandji Triadiyaksa1

1
Department of Physics, Faculty of Science and Mathematics, Universitas Diponegoro, Semarang 50275,
Indonesia
2
Department of Chemistry, Faculty of Science and Mathematics, Universitas Diponegoro, Semarang 50275,
Indonesia
*
E-mail: [email protected]

Article History
Received: 21 October 2022; Received in Revision: 4 March 2023; Accepted: 12 March 2023

Abstract

Pigments as colorants have a wide range of industrial applications. Commonly used pigments
contain toxic elements. This study proposes cerium oxide as an alternative colorant to replace
toxic pigments. Metal doping in cerium oxide can alter the color and properties of cerium oxide.
Pure cerium oxide and iron-doped cerium oxide nanopowders were synthesized using the
precipitation method. The x-ray diffraction and scanning electron microscope analysis revealed
the formation of cubic fluorite structures of cerium oxide composed of spherical particles. The
nanopowder of pure cerium oxide is pale yellow, while iron-doped cerium oxide is brick red.
The N2 adsorption-desorption measurement showed the mesoporous nature of both cerium
oxide nanopowders. Incorporating iron into cerium oxide reduced crystallite size and increased
surface area. Moreover, UV-Vis spectroscopy analysis indicated that iron doping significantly
improves the UV absorption property and increases the bandgap energy of cerium oxide
nanopowders. The results demonstrate the cerium oxide nanopowder synthesized using
precipitation potential as a nano pigment.

Keywords: Cerium oxide, pigment, powder, precipitation, optical properties

1. Introduction metal element in the first ferric oxide (Fe 2O3)

nontoxic conventional inorganic red pigments.
Utilizing nanomaterials in a wide range of The iron incorporation into the CeO2 lattice
industrial applications has provided many changed the yellow of CeO2 to a reddish-
advantages. Nanomaterials application, such orange colour (Olegario et al., 2014).
as nanopowder, improves many pigment However, few studies have examined the
properties and produces many purposes and potential of iron-doped CeO2 nanopowder as a
functional pigments with high performance in non-toxic pigment.
their powder form. Only a few inorganic
pigments in the red to yellow range with high Various methods have been used to
performance, such as cadmium sulfoselenide, synthesize CeO2. Precipitation is a more
lead molybdate, and bismuth vanadate. suitable method for preparing nanopowder
However, pigments' toxicity and than other methods, such as the Pechini
environmental risk are severe concerns in method (Araujo et al., 2011), solid-state
developing pigments (Wu et al., 2021). reaction (Bayyapagari et al., 2018; Kumar &
Hymavathi, 2017; Oligario et al., 2014), self-
Cerium oxide (CeO2) nanopowder has a pale propagating method (Micovic et al., 2019;
yellow color and is one of the important Stojmenovic et al., 2015). These methods
inorganic pigments with high-temperature commonly require heat treatment at high
stability, high chemical resistance, and temperatures (>500oC) for a long duration,
nontoxic (Gonzaga et al., 2020). The colour which induces excessive particle growth. The
hue of CeO2 nanopowder-based pigment can present study aims to synthesize CeO2 and
be controlled by the incorporation of other CeO2:Fe nanopowders and explore their
lanthanide elements, such as praseodymium potential as environmentally friendly
(Gonzaga et al. 2020), terbium (Sulcova et al., pigments. CeO2 and CeO2:Fe nanopowders
2012), europium (Stojmenovi et al., 2015), or were synthesized using precipitation method,
transition metal elements such as zirconium followed by heat treatment at a temperature
(Joseph, et al., 2020), Nickel (Miri et al., of 500oC. Iron doping with a molar ratio of
2020), iron (Fe) (Olegario et al., 2014), and 0.05 concentration was chosen as a moderate
cobalt (Araujo et al., 2011). Iron is a transition

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doping level, which is expected to get a red The lattice parameter was calculated by using
pigment. Eq. 2.

2. Methodology √ℎ2 + 𝑘 2 + 𝑙2
𝑎= (2)
2 sin 𝜃
2.1. Materials
Remark:
Cerium nitrate hexahydrate (Ce(NO3)3.6H2O,  : the wavelength of X-ray.
 99,9%), Ferric nitrate nonahydrate
(Fe(NO3)3.9H2O,  99,9%) were purchased The morphology and composition of CeO2 and
from Sigma-Aldrich Co., Ltd. Ammonium CeO2:Fe were investigated by a scanning
hydroxide 25%, isopropanol, and ethanol electron microscope (SEM, JEOL JSM 6360)
were purchased from Merck & Co., Inc. integrated with energy-dispersive X-ray
spectroscopy (EDS). EDS was used to analyze
2.2. Synthesise of CeO2 and CeO2:Fe atomic composition in CeO2 and CeO2:Fe.
nanopowders
The N2 adsorption-desorption measurement
Pure CeO2 and CeO2:Fe nanopowders were (Quantachrome instrument) is a versatile
synthesized using the precipitation method. method to characterize porous solids and fine
The solution of Ce(NO3)2.6H2O was prepared powders. The N2 adsorption-desorption
in 42 mL of mixed isopropanol and isotherm was conducted at a temperature of
demineralized water to obtain pure CeO2 77 K to analyzee the pore size of CeO2 and
nanopowder. The ammonium hydroxide CeO2:Fe nanopowders. Then, specific surface
solution was dropped until constant pH of 10 area (SSA) and pore size were calculated
was attained. The same procedure was used using multipoint the Brunauer-Emmett-Teller
to synthesize CeO2:Fe, except by adding (BET) method and Barrett-Joyner-Halenda
Fe(NO3)3.9H2O into Ce(NO3)3.6H2O solution so (BJH) method (Thommes et al., 2015).
that the molar ratio is 0.05. The precipitation Furthermore, the SSA was used to calculate
process was carried out at room temperature. particle size using Eq. 3 (Nadjia et al., 2018).
The obtained precipitates were washed and
filtered, then dried at 100oC. The calcination 6
𝐷𝑆𝑆𝐴 = (3)
at a temperature of 500oC was subjected to  × SSA
dried precipitate for 3 hours.
Remark:
2.3. Characterization  : the theoretical density of CeO2 (g/cm3).

The structural properties of CeO2 and CeO2:Fe The optical properties of CeO2 and CeO2:Fe
nanopowders were examined using an X-ray were analyzed by UV-Vis spectrophotometer
diffractometer (PANalytical Xpert Pro). The Cu (Shimadzu 1240). The absorbance spectra of
K radiation with a wavelength of 1,5406 Å CeO2 and CeO2:Fe were measured in
was employed as an X-ray source that wavelength 200 – 800 nm. Tauc’s plot
activated at 30 mA and 40 kV. The XRD data method (Eq. 4) was utilized to determine
were recorded at 2 in the 10 to 90o with step bandgap energy.
size 0.026o. The XRD data were used to
estimate crystallite size and strain of (𝛼ℎ)𝑛 = 𝐵(ℎ − 𝐸𝑔 ) (4)
nanopowder using the size-strain-plot (SSP)
method described by Eq. 1 (Kumara et al., Remark:
2017). h : Planck constant
 : frequency
𝐾 𝜀 2 B : a constant
(𝑑ℎ𝑘𝑙 𝛽ℎ𝑘𝑙 cos 𝜃)2 = (𝑑ℎ𝑘𝑙 2 𝛽ℎ𝑘𝑙 cos 𝜃) + ( ) (1)
𝐷𝑋𝑅𝐷 2 Eg: bandgap energy
n = 2 for direct transition
Remark:  :absorption coefficient
𝛽ℎ𝑘𝑙 : full width at half of the maximum
(FWHM) of diffraction peak The absorption coefficient was evaluated from
dhkl : inter-planar spacing UV-Vis absorbance spectra using Eq. 5.
K = 3/4 for a spherical particle
 : diffraction angle 2.303 × 103 𝐴𝜌
DXRD: crystallite size = (5)
𝑙𝑐
𝜀 : the lattice strain
h, k, and l : Miller’s index Remark:
A : absorbance

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 : the density of CeO2 (g/cm3) In addition, the diffraction peaks of CeO2:Fe

l : the optical path (1 cm) possessed lower and broader intensity than
c : the suspension concentration of CeO 2 the pure CeO2 nanopowder and shifted to
nanopowder. higher 2. This result indicates that Fe3+ ions
with a smaller radius (0.645 Å) were
The refractive indices (n) of CeO2 and CeO2:Fe successfully substituted into the lattice of Ce4+
was calculated using Eq. 6 (Soni et al., 2021). ions with a larger radius of 0.97 Å. It is
supported by the calculated lattice constant of
CeO2:Fe (5.4090 Å), lower than the CeO2
𝑛2 − 1 𝐸𝑔
=1−√ (6) lattice constant (5.4208 Å). A similar result
𝑛2 + 2 20 was described for CeO2:Fe preparation by
hydrothermal (Jiang, et al., 2020) and Fe-Ce
3. Results and Discussion mixed oxide prepared by co-precipitation
method (Bao, et al., 2017). Commonly, the
3.1. Structure of CeO2 and CeO2:Fe substitution element with a radius smaller
nanopowders than CeO2 would shift the diffraction peaks of
CeO2 to higher 2 (Soni et al., 2021; Joseph
The obtained CeO2 and CeO2:Fe nanopowder et al., 2020). Since the calculated lattice
prepared by the precipitation method is shown constant of CeO2:Fe is lower than CeO2, then
in Figure 1. As can be seen, the CeO2 it is expected that the lattice experiences
nanopowder was pale yellow. The doping 5 compressive stress.
wt% iron causes the pale yellow color of CeO2
to turn to brick red. The CeO2:Fe pigments The broadening x-ray diffraction peaks are
prepared by solid-state reaction exhibited a attributed to crystallite size and microstrain in
brown to reddish-orange color (Olegario, et the crystalline material. The x-ray diffraction
al., 2014). The other previous study reported data of CeO2 and CeO2:Fe were further
that the 15 mol% mol Fe-CeO2 designed by analysed using the size strain plot (SSP)
solvothermal was light brown (Jiang, et al., method. The SSP method considered a
2020). As a result, the color of CeO2:Fe crystallite size and microstrain contribution to
depends on doping concentration and the diffraction peaks profile. The widened x-
preparation method. ray diffraction peaks reveal that CeO2 and
CeO2:Fe comprise nanometric-size
CeO2 CeO2:Fe
crystallites. This phenomenon is supported by
the determination of crystallite size using the
SSP method. Figure 2(b) shows the SSP graph
of CeO2 and CeO2:Fe nanopowders. The
experimental x-ray diffraction data (marked
with a solid circle) are located along a straight
Figure 1. Photograph of CeO2 and CeO2:Fe line of the SSP graph. The correlation
nanopowders coefficients (R2) are close to 1, implying that
experimental x-ray diffraction data fit well
The XRD patterns of CeO2 and CeO2:Fe with SSP analysis.
nanopowders are shown in Figure 2 (a). CeO2
and CeO2:Fe nanopowders had similar The average crystallite size and the lattice
patterns with many diffraction peaks at 2 : strain obtained from the slope and the
28.43, 32.95, 47.52, 56.18, 58.99, 69.29, intercept of the straight-line graph of SSP are
76.64, 78.98, and 88.46o. The observed peaks represented in Table 1. The insertion of iron
corresponded to crystal planes of (111), ions with a small radius into the cerium lattice
(200), (220), (311), (222), (400), (331), reduced the crystallite size of the CeO2
(420), and (422) for the cubic fluorite nanopowder from 6.3 to 5.3 nm. A similar
structure of cerianite (JCPDS:34-0934). The phenomenon is found in other CeO2 prepared
sharp diffraction peaks with high intensity by hydrothermal (Radovic, et al., 2013) and
confirmed the high crystallinity of CeO 2 solvothermal (Jiang et al., 2020). Meanwhile,
nanopowder. It also saw no additional iron insertion increased the strain in our CeO 2
diffraction peaks of other phases identified in from 0.01 to 0.02. The increasing strain in
CeO2 and CeO2:Fe diffraction patterns. The CeO2 can be correlated to a reduction in
result agreed with a previous report (Soni et crystallite size and a reduction in crystal
al., 2021; Jiang et al., 2020). Therefore, the regularity in the CeO2 lattice due to iron
precipitation method propers for forming CeO2 insertion. This explanation is likely attributed
and CeO2:Fe nanopowders at a temperature of to the lower diffraction peaks intensity of
500oC. CeO2:Fe than pure CeO2, as shown in figure
2(a).

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Figure 2. (a) XRD pattern and (b) SSP method of CeO2 and CeO2:Fe nanopowders

Tabel 1. The crystallite size, strain, specific surface area and particle size of CeO 2 and CeO2:Fe
nanopowder
Sample Crystallite size Strain Lattice constant BET Particle size
(nm) (Å) (nm)
CeO2 6.3 0.01 5.4208 Å 12.7
CeO2:Fe 5.3 0.02 5.4090 Å 10.6

3.2. Morphology of CeO2 and CeO2:Fe at a range temperature of 400 – 600oC for 2
nanopowders hours (Soni et al., 2021).

The SEM images of CeO2 and CeO2:Fe

nanopowders are shown in Figure 3. The SEM CeO2
images indicate that the spherical primary and
agglomerate secondary particles arrange CeO 2
and CeO2:Fe nanopowders. There was no
particle shape difference between CeO2 and
CeO2:Fe nanopowders, but weak
agglomeration appears for CeO2:Fe. The result
shows that iron doping reduces agglomeration
particles and the crystallinity of CeO 2
nanopowder. The particle size of both CeO2 in
SEM images appeared higher than the
estimated crystallite size from XRD analysis. It
can be explained due to the several crystallites
that compose the particles due to the
polycrystalline structure of CeO2. CeO2:Fe
Generally, the small-sized particle exhibits a
large surface area and high surface energy.
These characteristics lead agglomeration
tendency of particles to reduce their surface
energy. Consequently, primary particles
adhere to each other to form agglomerated
secondary particles. This phenomenon also
appears in CeO2:Fe synthesised by
hydrothermal method. The bundle structure
morphology of CeO2 and CeO2:Fe comprises
nanorod-shaped primary particles and no
effect of iron variation on CeO2 morphology
(Jiang, et al., 2020). In another study, weak Figure 3. SEM images of CeO2 and
agglomeration was found in CeO2 doping Zn CeO2:Fe nanopowders
synthesised by sol-gel method and calcination

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The incorporation of iron doping into the CeO 2 of iron into CeO2 enlarged the specific surface
lattice was investigated by EDS analysis. area of pure CeO2 nanopowder. Additionally,
According to the theoretical calculation of the particle sizes derived from BET surface-
stoichiometric CeO2 consists of 81 wt% specific area are 12.7 and 10.6 nm for CeO2
cerium and 19 wt% oxygen, whereas the and CeO2:Fe, respectively.
atomic composition of 0.05 molar rasio iron
to CeO2 equals 1.67 wt%. The atomic
composition of CeO2 and CeO2:Fe
nanopowder from EDS analysis is
summarized in Table 2. As can be seen, the
cerium and oxygen atomic composition in
CeO2 and CeO2:Fe are almost the same as the
theoretical calculation. The composition of
oxygen atom in CeO2 and CeO2:Fe, i.e., 18.59
and 18.65 wt%, are smaller than the
theoretical value of 19 wt%. The result
indicates that oxygen defect is present in both
CeO2. Moreover, the existence of the iron
atom in CeO2 was found to be 1.21 wt%. As
a consequence, the atomic composition of
cerium decreased from 81,41 wt% in pure
CeO2 to 80,14 wt% in CeO2:Fe. The atomic
composition analysis suggested that iron ions
replaced cerium ions in the CeO2 lattice.

Tabel 2. Atomic composition of CeO2 and

CeO2:Fe nanopowders
Atomic composition (wt%)
Sample
Ce O Fe
CeO2 81,41 18,59 -
CeO2:Fe 80,14 18,65 1,21

3.3. Surface area and porosity of CeO2

and CeO2:Fe nanopowders

The N2 adsorption-desorption isotherm

Figure 4. The N2 adsorption-desorption
curves, as shown in Figure 4, were analysed
Isotherm curves of (a) CeO2 and
to determine the porous properties of CeO2
(b) CeO2:Fe nanopowders
and CeO2:Fe nanopowders. According to the
hysteresis loop type of the IUPAC
Tabel 3. The BET surface area, porevolume,
(International Union of Pure and Applied
and pore radius of CeO2 and
Chemistry) classification, both CeO2
CeO2:Fe nanopowders
nanopowders belong to H3 hysteresis loop of
Sample Surface Pore Pore
type IV physisorption isotherm. The such
area volume radius
hysteresis loop is typically observed in N 2
(m2/g) (cm3/g) (nm)
adsorption by aglomerated particles. A lower
closure point shows it near 0.42 P/Po. This CeO2 65.26 0.20 2.93
explanation is supported by the SEM image CeO2:Fe 78.14 0.29 3.69
analysis that showed agglomerated particles.
Meanwhile, type IV isotherm takes place by The CeO2:Fe with a larger specific surface area
mesoporous material (Thommes et al., 2015). showed a smaller particle size than pure CeO2.
As a result, CeO2 and CeO2:Fe are composed The decreasing particle size of CeO2 due to
of mesoporous agglomerated particles. iron doping is in harmony with the estimated
crystallite size obtained from the XRD
Furthermore, the relevant type IV isotherm analysis. The decreased crystallite size of
was analysed using the BET method to find the CeO2 due to iron doping is associated with the
surface area. The BET-specific surface area of replacement of cerium ion by smaller ionic
CeO2 and CeO2:Fe nanopowders were 65.26 radii of iron without structure to be changed
and 78.14 m2/g, respectively, as depicted in leading to a smaller lattice constant as seen in
Table 3. Both CeO2 and CeO2:Fe nanopowders Table 1. The enlargement specific surface
show sizeable specific surface area. Insertion area of CeO2 by doping iron described in
precipitation synthesis of CeO2, which calcined

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at a temperature of 550oC for 5 h for hydrogen 3.4 Optical properties of CeO2 and
production application (Mansingh, et al., CeO2:Fe nanopowders
2016), as well as CeO2 synthesized
solvothermal for catalytic oxidation (Jiang et The absorption is an essential property to
al., 2020). Interestingly, the specific surface evaluate the characteristic of pigment. Figure
area of CeO2 and CeO2:Fe in this study is more 6(a) presented UV-Vis absorbance spectra of
prominent than in another previous study CeO2 and CeO2:Fe nanopowders. The
(Mansingh, et al., 2016). Nanopowder with absorption spectra showed the absorption
a large specific surface area provides peak at around 307 nm, which revealed the
advantages for paint pigment application. absorption characteristic of CeO2. The
insertion of iron significantly increased the
absorption property of CeO2. In contrast, the
shifted absorption band edge to the lower
wavelength indicates widening bandgap
energy.

Figure 5. Pore size distribution of (a) CeO2

and (b) CeO2:Fe nanopowders

In addition, pore size distribution is another

crucial aspect for the practical application of Figure 6. (a) UV Vis absorbance spectra
porous material. The BJH (Barrett-Joyner- (b) Tauc’s plot of CeO2 and
Halenda) method is appropriate for calculating CeO2:Fe nanopowders
the pore size of mesoporous materials. Figure
5 displays the BJH pore size distribution of The direct bandgap energy of CeO2 and
CeO2 and CeO2:Fe. CeO2 and CeO2:Fe show CeO2:Fe was estimated using Tauc’s
narrow pore size distribution in the 2 to 20 nm plots, as shown in Figure 6(b). The
range, indicating uniform pore size. The peak extrapolating linear part of absorption
of pore radius centred at 2.93 nm for CeO2 and spectra to h = 0 gives a bandgap
3.69 nm for CeO2:Fe nanopowders. Those energy value of 3.28 eV and 3.43 eV for
pore radii correspond with a pore volume of CeO2 and CeO2:Fe, respectively. The
0.20 cm3/g and 0.29 cm3/g, as tabulated in bandgap energies of both CeO2 are more
Table 3. The doping of iron into CeO2 significant than the bandgap energy of
increased pore size and pore volume. Thus CeO2 bulk, i.e., 3.19 eV. Others have
surface area of CeO2:Fe is higher than pure observed an increase in the bandgap
CeO2. energy of CeO2 due to iron doping (El-
Hagary et al., 2019; Bayyappagaria et

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al., 2018). The considerable bandgap Bao, H., Qian, K., Fang, J., Huang, W., 2017.
energy of both CeO2 in this study Fe-doped CeO2 solid solutions:
attributing to the quantum confinement Substituting-site doping versus
effect or blue-shift phenomenon due to interstitial-site doping, bulk doping
the nanometric particle size of CeO2 as versus surface doping. Appl. Surf. Sci.
confirmed by XRD and SSA analysis. In 414, 131–139.
contrast to the hydrothermally https://doi.org/10.1016/j.apsusc.2017.0
synthesised CeO2, the bandgap energy 4.018
of CeO2:Fe is smaller than pure CeO2 due
to the presence of the second phase of Bayyappagaria, B., Shaik, K., Nasinac, M.R.,
FeO and oxygen defect in the bandgap Inturud, O., Dugasanie, S.R., 2018.
(Radovic et al., 2013). Effect of Fe substitution on optical and
magnetic properties of CeO 2
The refractive index value is another nanoparticles. Optik. 154, 821–827.
important optical property of pigment. https://doi.org/10.1016/j.ijleo.2017.10.
The refractive index of oxide 025
semiconductors strongly correlates to
bandgap energy. The obtained bandgap El-Hagary, M., Shaabanb, E.R.,. Moustafa,
energy then uses to estimate the S.H., Gad, G.M.A. (2019) The particle
refractive index of CeO2 and CeO2:Fe size-dependent optical band gap and
nanopowders using Eq. 6. The values of magnetic properties of Fe-doped CeO2
refractive indices are 2.37 and 2.29 for nanoparticles, Solid State Sci. 91, 15–
CeO2 and CeO2:Fe, respectively. The 22.https://doi.org/10.1016/j.solidstates
obtained refractive indices values are ciences.2019.03.005
close to the refractive indices of bulk
CeO2, i.e., 2.2. The CeO2:Fe Gonzaga, L.A., Santana, V.T., Bernardi,
nanopowders with higher bandgap M.I.B., Hruby, J., Neugebauer, P.,
energy possess lower refractive indices Mesquita, A., 2020. CeO2 and CeO2:Pr
than pure CeO2 nanopowder. nanocrystalline powders prepared by the
polymeric precursor method: Yellow and
4. Conclusion red pigments with tunable color. J.
American Ceram. Soc. 103(11), 6280-
The CeO2 and CeO2:Fe nanopowder pigments 6288.
with cubic fluorite structure were obtained by https://doi.org/10.1111/jace.17339
precipitation at a calcination temperature of
500oC. The CeO2:Fe nanopowder possessed Jiang, C., Wanga, H., Wanga, Y., Xue, C.,
a smaller crystallite size, higher specific Yang, Z., Yu C., JI, H., 2020. Modifying
surface area, and more substantial absorption defect States in CeO2 by Fe doping: A
properties than pure CeO2 nanopowder. The strategy for low temperature catalytic
incorporation of iron into CeO2 shifted the oxidationof toluene with sunlight. J.
absorption edge to a lower wavelength and Hazard. Mater. 390, 122182.
changed the pigment colour from yellow to https://doi.org/10.1016/j.jhazmat.2020.
brick red. The results suggest that 122182
precipitation is useful to produce cerium oxide
nano pigment. Joseph, A., Mathew, K.P.J., Vandana, S.,
2021. Zirconium-Doped Ceria
Acknowledgement Nanoparticles as Anticorrosion Pigments
The authors acknowledge the financial support in Waterborne Epoxy−Polymer Coatings,
provided by The Ministry of Research and ACS Appl. Nano Mater. 4(1), 834-849.
Technology/National Research and Innovation https://doi.org/10.1021/acsanm.0c0316
Agency of Republic Indonesia (No. 187- 2
29/UN7.6.1/PP/2022).
Kumar, B.R., Hymavathi, B., 2017. X-ray
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