j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 1 ; 1 1 : 1 1 2 e1 2 0

Available online at www.sciencedirect.com

journal homepage: www.elsevier.com/locate/jmrt

Original Article

Structural, optical and photocatalytic properties of

cuboid ZnO particles

H. Vahdat Vasei, S.M. Masoudpanah*

School of Metallurgy & Materials Engineering, Iran University of Science and Technology (IUST), Tehran, Iran

article info abstract

Article history: Zinc oxide (ZnO) powders were prepared by solution combustion method using trime-
Received 4 September 2020 thyloctylammonium bromide (OTAB) and a mixture of OTAB and citric acid as fuel. Single
Accepted 3 January 2021 phase ZnO powders with wurtzite structure were directly formed at high fuel contents
Available online 9 January 2021 (4
1). The porous microstructure of combusted ZnO powders by mixed fuels had the
specific surface area in the range of 73e416 m2/g in which increased with the increase of
Keywords: amount of fuels. The ZnO powders synthesized by single OTAB fuel were composed of the
Zinc oxide compacted agglomeration particles with cuboid-like morphology. The optical and photo-
Solution combustion synthesis catalytic properties of ZnO powders were determined as a function of fuel type and con-
OTAB tents by diffuse reflectance spectroscopy and photoluminescence spectroscopy
Mixed fuel techniques. The ZnO powders obtained by OTAB-citric acid mixed fuel at 4 ¼ 1.5 showed
Photocatalytic activity the highest adsorption (53%) and photodegradation (95%) efficiency of MB dyes during
90 min under ultraviolet (UV) light irradiation.
© 2021 The Author(s). Published by Elsevier B.V. This is an open access article under the CC
BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

Zinc oxide (ZnO) as an ultraviolet photocatalyst has received

1. Introduction
Recently, the International Water Management Institute
(IWMI) and the Food and Agriculture Organization of the
United Nations (FAO) have reported that the pollution of water
has increased in developed and developing countries, leading
to the undermining of the economic growth and the threat-
ening the physical and environmental health of a large
number of people [1]. Several physical and chemical methods
such as adsorption, ion exchange, separation, and advanced
oxidation processes (AOPs) have been applied for water
treatments [2e4]. Among them, the AOPs are interesting
candidates owing to the complete color removal, harmfulness
byproducts, efficient in low concentration, and low cost [2].
significant attention due to its wide band gap energy (3.37 eV),
large excitation binding energy (60 meV), excellent chemical
stability, and low cost [2e4]. The various chemical routes such
as hydrothermal [5], solvothermal [6], solegel [7], precipitation
[8], thermal decomposition [9], solid state [10], solution com-
bustion synthesis (SCS) [11] have been used to synthesize the
nanostructured ZnO powders.
SCS as a simple, inexpensive, and time/energy-efficient
route have been used for the rapid production of nano-
structured materials in large scale [12,13]. Furthermore, the
SCS is also compatible with circular economy concept because
of its eco-friendly characteristics [14,15]. The SCS based on a
self-sustained exothermic reactions between metal

* Corresponding author.
E-mail address: masoodpanah@iust.ac.ir (S.M. Masoudpanah).
https://doi.org/10.1016/j.jmrt.2021.01.003
2238-7854/© 2021 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 1 ; 1 1 : 1 1 2 e1 2 0 113

precursors (e.g. nitrates, carbonates, and sulfates) as oxidants

(101)
and organic materials (e.g. urea, glycine and citric acid, etc.) as

(100)
(002)

(110)

(103)

(112)
fuels. Actually, the SCS consists of three main steps; the dis-

(102)
solving of precursors in water as solvent, the gelation of pre- ϕ=1.5
cursor solution by evaporation of solvent, and the ignition of

Intensity (arb. units)

dried gel by heating up on a hot plate or furnace [15e17]. The
SCSed products show many favorable features such as high ϕ=1
specific surface area, porous microstructure, defective crystal
structure for application as catalysts [12,16].
In this work, the ZnO powders were synthesized by solu- ϕ=0.75
tion combustion synthesis using trimethyloctylammonium
bromide (OTAB) as fuel following our previous works
[11,18,19]. OTAB as a C8-tailed cationic surfactant belongs to φ=0.5

the trimethylammonium bromide (CnTAB) family. Further-

20 30 40 50 60 70
more, the OTAB fuel was combined with the citric acid as 2 theta (°)
auxiliary fuel for further control over on the structural,
microstructural, optical, and photocatalytic properties of ZnO Fig. 1 e XRD patterns of the as-combusted ZnO powders by
powders. using various amounts of single OTAB fuel.

[21,22]. The particle size and shape of ZnO powders were

2. Experimental procedures observed by a Vega II field emission scanning electron mi-
croscope (TESCAN, Czech Republic) and transmission electron
2.1. Materials microscopy (Philips CM200). The TEM samples were prepared
by ultrasonically dispersion of powders in ethanol/water so-
Zinc nitrate (Zn(NO3)2) and citric acid (C6H8O7) were purchased lution for 15 min. The specific surface area and pore size dis-
from Merck company, while the OTAB surfactant ([(C8H17) tribution of combusted ZnO powders were measured from N2
N(CH3)3]Br) was purchased from SigmaeAldrich Co. adsorptionedesorption isotherms on a PHS-1020 (PHSCHIN,
China) instrument. The powders were firstly degassed at
2.2. Synthesis 250  C for 5 h. The specific surface areas and pore volume were
calculated from the BrunauereEmmetteTeller (BET) equation
Required amounts of zinc nitrate as oxidant and OTAB and and BarretteJoynereHalenda (BJH) method, respectively [23].
citric acid as fuel were dissolved in distilled in water under The band gap energy and crystal defects were measured from
magnetic stirring. The amounts of fuels were calculated ac- UVeVis diffuse reflectance spectra (Shimadzu UVeVis-52550)
cording to the following reaction [12,16,20]: and photoluminescence (PL) spectra (Hitachi F-7000 Fluores-
  cence). The excitation wavelength was 325 nm.
104 5
Zn NO3 2 þ C11H26BrN þ ð4  1ÞO2 / ZnO
70 2
1104 1304 54 54 2.4. Photocatalytic experiments
þ CO2 þ H2O þ N2 þ Br2 (1)
70 70 70 70
The photocatalytic performance of the powders was tested on
 
1 104 104 methylene blue (MB) dye under irradiation of two UV lamps
ZnðNO3Þ2 þ C11H26BrN þ C6H8O7
2 70 18 (Philips, 8W). The amount of ZnO catalyst was 0.1 g and the
5 15454 12854 initial concentration of MB solution was 15 mg/L. In order to
þ ð4  1ÞO2 / ZnO þ CO2 þ H2O
2 630 630
 
1 54 54
þ 1 þ N2 þ Br2 (2)
2 70 140

which the 4 values as fuel to oxidant ratio were set as 0.5,

0.75 and 1.5. After homogenization, the precursor solution
was evaporated at 80  C. The dried gel was ignited by further
heating up to 250  C on a hot plate. The combusted powders
were hand-crushed by a pestle.

2.3. Characterization

Phase, structure, lattice parameters and crystallite size were

extracted by refining the XRD patterns which were recorded
by a PANalytical X-ray diffractometer (CuKa ¼ 1.5414
A) in-
strument. The XRD patterns were structurally analyzed for
calculating the lattice parameters and crystallite size by
Fig. 2 e XRD patterns of the as-combusted ZnO powders by
Rietveld refinement method using HighScore Xpert software
using various amounts of OTAB-citric acid mixed fuels.
114 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 1 ; 1 1 : 1 1 2 e1 2 0

band gap energy

Table 1 e Lattice parameters (±0.0002 A), 3. Results and discussion
(±0.01 eV) and photodegradation rate constant (±0.001
min¡1) of the as-combusted ZnO powders as a function of
3.1. Structural analysis
f values.
F

a¼b (A) c (

A) Eg (eV) k (min1) XRD patterns of the ZnO powders synthesized by single OTAB
OTAB fuel and OTAB-citric acid mixed fuels are presented in Figs. 1
0.5 3.2534 5.2092 3.08 0.001 and 2, respectively. Table 1 summarizes the lattice parameters
0.75 3.2533 5.2118 3.12 0.002
versus fuel contents. All diffraction peaks of (100) (002) (101)
1 3.2505 5.2010 3.11 0.001
(102) (110) (103) and (112) indicate the hexagonal wurtzite
1.5 3.2556 5.2136 3.13 0.002
OTAB þ Citric acid structure of ZnO with space group P63mc (PDF2#00-036-1451).
0.5 3.2533 5.2117 3.14 0.01 The powders synthesized by single OTAB fuel are composed of
0.75 3.2518 5.2094 3.17 0.02 the ZnO and impurity Zn(BrO3)2.6H2O phases in which the
1 3.2539 5.2024 3.14 0.02 impurity phases disappear with the increase of fuel amount
1.5 3.2535 5.2111 3.20 0.03 [20,24]. For the mixed fuels, the citric acid molecules chelate
the Zn2þ cations which hindered the precipitation of
Zn(BrO3)2.6H2O phase. The zinc citrate species are thermally
decomposed to the ZnO particles during combustion reaction.
establish the adsorption/desorption equilibrium, the suspen- Furthermore, the lattice parameters of powders are near to
sion was stirred in the dark for 60 min. Then the UV lamps the bulk ZnO values (a ¼ b ¼ 3.2542
A and c ¼ 5.2066

A), con-
were turned on. At each 30 min interval times, the concen- firming the wurtzite crystal structure [25].
tration of residual MB dye in the irradiated solution was
recorded on PG Instruments Ltd T80-UV/Vis spectrophotom- 3.2. Morphological observations
eter. For higher accuracy, the ZnO catalysts were separated by
centrifugation at 4000 rpm for 20 min. SEM images of the ZnO powders versus fuel type and amount
are shown in Figs. 3 and 4. The single OTAB fuel results in a

Fig. 3 e Low magnification SEM micrographs of the as-combusted ZnO powders by single OTAB fuel at (a) f ¼ 0.5, (b)
f ¼ 0.75, and (c) f ¼ 1.5 and by using mixture of OTAB and citric acid fuels at (d) f ¼ 0.5, (e) f ¼ 0.75 and (f) f ¼ 1.5.
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 1 ; 1 1 : 1 1 2 e1 2 0 115

Fig. 4 e High magnification SEM micrographs of the as-combusted ZnO powders by single OTAB fuel at (a) f ¼ 0.5, (b)
f ¼ 0.75, and (c) f ¼ 1.5 and by using mixture of OTAB and citric acid fuels at (d) f ¼ 0.5, (e) f ¼ 0.75 and (f) f ¼ 1.5.

mixture of cubic-like and quasi-spherical particles which are
compactly agglomerated. With the increase of fuel contents,
the cubic-like particles were disappeared and replaced by
spherical particles. The morphology of ZnO powders depends
on the physicochemical properties of the dried gel and
amount of released gases and heat during the combustion
reaction and the [12]. The cubic-like particles were formed at
low fuel contents because of the precipitation of Zn(BrO3)2.6-
H2O phase during gelation process. The cubic morphology of
Zn(BrO3)2.6H2O precipitate was transferred to the final prod-
ucts [26]. The released gas leads to the porous and foamy
microstructure, while the released heat is benefitted for the
particle sintering and growth [18]. Accordingly, the higher
porosity of the OTAB-citric acid fuel is attributable to the
higher liberated gaseous products. Furthermore, the sintered
microstructure by single OTAB fuel shows that the released
heat has a more dominant factor in its microstructure.
Furthermore, the particle size increases from ~50 to ~250 nm
for the mixed fuels on account of the increase of adiabatic
combustion temperature from 2000 to 2500 K with the in-
crease of the 4 values [23].
TEM images of the as-combusted ZnO powders by single
OTAB fuel and OTAB-citric acid mixed fuels at 4 ¼ 1.5 are
compared in Fig. 5. The cubic-like particles (~300e450 nm) and
quasi-spherical particles can be observed for the single OTAB
fuel, while there are only spherical particles (~65 nm) for the
mixed fuels. Furthermore, the high magnification TEM image
show that the cubic-like particles are formed by self-
assembling of a large amount of nanoparticles. Although the
surfactant molecules burn during the combustion process, but
the surfactants can self-assemble the precipitates during
gelation process.
3.3. Textural analysis
The efficiency of heterogeneous catalysts mainly depends on
the textural properties including specific surface area and
porosity of materials. N2 adsorptionedesorption isotherms
and pore size distribution plots of the ZnO powders are shown
in Fig. 6. The isotherms of the combusted ZnO powders are IV
type with H3 hysteresis according to IUPAC classification. The
H3 hysteresis is related to the brittle agglomeration of parti-
cles with 3D pore network [27]. As the amount of fuel in-
creases, the specific surface area increases from 35 to 108 m2/g
and from 72 to 416 m2/g for single OTAB fuel and OTAB-citric
acid mixed fuels, respectively, because of the increase of
amount of gaseous products which disintegrate the large
particles into ones. The released heat is responsible for
116 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 1 ; 1 1 : 1 1 2 e1 2 0
Fig. 5 e TEM images of the ZnO powders synthesized by (a and b) single OTAB fuel and (c and d) mixture of OTAB and citric
acid fuels at f ¼ 1.5.
particle sintering and growth, leading to the decrease of spe-
cific surface area [12]. Accordingly, the higher specific surface
area of mixed fuels than that of single fuel can be attributed to
the liberation of higher amount of gaseous products by the
mixed fuel [28]. The role of combustion gases can be
confirmed by the higher pore volume for the mixed fuels in
comparison with the single fuel (Table 2). The pores are also
distributed in the micropore range (1e2 nm). Table 3 compares
the specific surface areas of ZnO powders synthesized by
various methods. The highest specific surface areas of ZnO
powders obtained by OTAB-citric mixed fuels can be attrib-
uted to the synergetic effect of OTAB and citric acid molecules
on the reduction of surface tension of precursor solution and
the increase of combustion rate [29].
3.4. DRS study
UVeVis diffuse reflectance spectroscopy (Fig. 7) was used to
determine the optical properties of the combusted ZnO
powders versus fuel type and amounts. The maximum ab-
sorption edge for all various 4 values was in the UV region
because of intrinsic band structure of ZnO [30]. The optical
band gap energy can be calculated by Tauc’s equation as fol-
lows [18]:


2
ðahnÞ ¼ A hn e Eg (3)
which a, and hn are the coefficient of absorption and the
photon energy in eV, respectively. The A is material constant.
For determining the band gap energy, a straight line was
tanged on the (ahn)2 curve vs. hn which the straight line was
extrapolated to zero (as shown in the inset of Fig. 7) which are
summarized in Table 1. The values of band gap energy in-
crease from 3.08 to 3.20 eV by the increase of fuel content
because of the different native defects concentrations [31e33].
The values of band gap energy by OTAB fuel are lower than
mixed fuel, regardless of fuel content which can be related to
the purity, crystallinity, particle size and shape of ZnO pow-
ders [34].
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 1 ; 1 1 : 1 1 2 e1 2 0 117

300 extended Zn interstitial, and antisite defects, respectively

8 (a)
7 0.5 [36,37]. The UV emission is located at 394 and 395 nm for the
dVp/drp (cm3/(g-nm)
250 6 0.75 single OTAB fuel and OTAB-citric acid mixed fuels, respec-
5 1
tively. The ZnO samples synthesized by mixture of OTAB and
Va/cm3(STP) g-1

200 4 1.5
3 citric acid fuels shows the violet band emission because of the
2 surface zinc vacancy [38]. Furthermore, the weak broad red
150
1
0 emission at around 606 nm is detectable for the OTAB samples
100 0 10 20 30 caused by the crystal defects originated from their lower
Pore diameter (nm)
crystallinity. The blue emissions at 442 and 459 nm are
50 attributed to transition between the vacancies of oxygen and
interstitial oxygen. The oxygen vacancies are responsible for
0
0 0.2 0.4 0.6 0.8 1 the weak blue-green emission at 484 nm [39e42]. However,
Relative pressure, p/p0 the higher combustion temperature of the mixed fuels results
in the higher crystallinity and the absence of visible
1000
60 emissions.
900 (b)
50 0.5
dVp/drp (cm3/(g-nm)

800 0.75
40 1 3.6. Photocatalytic and adsorption study
700 1.5
Va/cm3(STP) g-1

30
600
20 The as-combusted ZnO powders were used for the photo-
500 10 degradation of MB dye solution under UV light irradiation. The
400 0 degradation efficiency is calculated by using the following
300 0 5 10 15 20
Pore diameter (nm) equation [43]:
200
 
100 C0  C
Degradationð%Þ ¼  100 (4)
0 C0
0 0.2 0.4 0.6 0.8 1
Relative pressure, p/p0

Fig. 6 e Adsorption (filled symbols) and desorption (open

symbols) isotherms and pore size distribution of the as- (a)
combusted ZnO powders by using (a) single OTAB fuel and
(b) the mixture of OTAB and citric acid fuels. ( h )2
Absorbance (arb. u.)

Table 2 e Dependence of the BET specific surface area

(±0.1 m2/g) and pore volume (±0.01 cm3/g) on the fuel/
oxidant molar ratio (f). 2.9 3 3.1 3.2 3.3
h (eV)
Fuel f SBET (m2/g) Pore volume (cm3/g)
OTAB 0.5 35.0 0.17 0.5
0.75
0.75 54.2 0.23 1
1 108 0.52 1.5
1.5 36.3 0.20
OTAB þ citric acid
200 300 400 500 600 700 800
0.5 72.7 0.43 Wavelength (nm)
0.75 362.8 1.85
1 350 1.66
(b)
1.5 415.8 1.97
Absorbance (arb. u.)

( h )2

3.5. Photoluminescence (PL) study

By considering the role of native defects on either improve- 3 3.1 3.2 3.3
ment or worsening of photocatalytic activity, the PL spec- h (eV)
0.5
troscopy (Fig. 8) was employed to study the native defects of 0.75
ZnO powders [35]. Typically, the PL spectra of ZnO consist of 1
1.5
two main emissions; UV and visible emissions in which the
UV emission is related to the free excitons recombination in 200 300 400 500 600 700 800
bond structure, while the visible emissions are dependent on Wavelength (nm)
the crystal defects and/or impurities level [33]. The visible
Fig. 7 e UVeVis diffuse reflectance spectra of the as-
region consists of various emissions such as blue (~460 nm),
combusted ZnO powders using (a) single OTAB fuel and (b)
green (~540 nm), and red (~630 nm) due to the Zn vacancy,
the mixture of OTAB and citric acid fuels.
118 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 1 ; 1 1 : 1 1 2 e1 2 0

Table 3 e Comparison of the BET specific surface area (±0.1 m2/g) of the as-combusted ZnO powders with the other reported
results.
Synthesis method Specific Surface Area (m2/g) condition References
Solution combustion 350 Fuel: OTAB þ Citric acid, f ¼ 1 [19]
Solution combustion 205 Fuel: DTAB þ Citric acid, f ¼ 1 [19]
Solution combustion 202 Fuel: SDS þ Citric acid, f ¼ 1 [49]
Exo-templating 202 Template: CMK-1 [50]
Exo-templating 192 Template: PAN-CMK-3 [50]
Solvothermal 186 e [51]
Thermolysis 153 e [52]
Solution combustion 122 Fuel: SDS þ Citric acid, f ¼ 1.5 [49]
Solution combustion 416 Fuel: OTAB þ Citric acid, f ¼ 1.5 This work
Solution combustion 363 Fuel: OTAB þ Citric acid, f ¼ 0.75

800 the mixture of OTAB and citric acid fuels show the higher
(a) 0.5
700
0.75 efficiency of 84%, 97% and 100% at the same fuel contents.
1
1.5 The photocatalytic process is based on the generation
PL Intensity (arb. u.)

600
of photo-induced electronehole pairs in the semi-
500 conductor under UV/visible irradiation, leading to the
400 formation of highly active species such as O-2 and HOO/
$OH by reacting of electronehole pairs with O2, OH and
300
H2O species. The dye molecules adsorbed on the surface
200 of photocatalyst are mineralized to CO2 and H2O species
100 by photogenerated oxidant agents [44]. Therefore, photo-
catalytic activity is related to the adsorption capability
0
350 400 450 500 550 600 650 700 and optical properties which are dependent on the specific
Wavelength (nm)

800
0.5 1
(b) (a)
700 0.75
1
PL Intensity (arb. u.)

600 1.5 0.8

500

400 0.6
C/C0

300
0.4 Dark UV
200

100 0.5
0.2 0.75
0 1
350 400 450 500 550 600 650 700 1.5
Wavelength (nm)
0
-60 -30 0 30 60 90 120 150 180
Fig. 8 e PL spectra of the as-combusted ZnO powders using Time (min)
(a) single OTAB fuel and (b) the mixture of OTAB and citric 1
(b)
acid fuels.
0.8
where C0 and C are the initial and instant concentrations,
respectively. The photodegradation rate of MB dyes can be 0.6
Dark UV
C/C0

fitted by the pseudo-first kinetics as follows:

  0.4
C
Ln ¼  kt (5)
C0
0.2 0.5
The values of k (min1) as rate constant calculated by 0.75
  1
C 1.5
plotting Ln C0 versus irradiation time (as shown in Sup- 0
-60 -30 0 30 60 90 120 150 180
porting Information) are presented in Table 1.
Time (min)
Fig. 9 shows the effects of fuel type and content on the
photodegradation of MB dye. For the single OTAB fuel, the Fig. 9 e C/C0 vs. irradiation time curves of the as-
photodegradation efficiencies of ZnO powders are 19%, 33%, combusted ZnO powders using (a) single OTAB fuel and (b)
and 29% for the 4 values of 0.5, 0.75 and 1.5, respectively, while the mixture of OTAB and citric acid fuels.
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 1 ; 1 1 : 1 1 2 e1 2 0
120
Adsorption
100 Photodegradation
Removal efficiency (%)
80
60
40
20
0 [3] Lee KM, Lai CW, Ngai KS, Juan JC. Recent developments of
0.5 0.75
Fig. 10 e Removal efficiency of MB dye by the as-
combusted ZnO powders by using OTAB-citric acid mixed
fuels at the different f values.
surface areas, surface ligands, light absorption coefficient,
and band gap energy [44e49].Fig. 10 compares the contri-
butions of adsorption capacity and photodegradation of
MB dye by ZnO powders versus the amount of fuel. The
higher photodegradation performance by the mixed fuels
can be attributed to the higher adsorption capacity caused
by the higher specific surface areas and pore volume.
Previous studies show that the dye adsorption is a surface
process which is affected only by surface and near-surface
defects, while both surface and bulk defects controls the
photocatalytic activity in which the lower concentrations
of non-radiative defects are needed for high photocatalytic
activity [50e52]. In addition to the higher specific surface
area and pore volume for the mixed fuels, the higher
crystallinity is also benefitted to the increase of photo-
degradation rate by the ZnO catalysts synthesized by
mixed fuels.
4. Conclusion
Solution combustion synthesis method was used to synthe-
size the ZnO powders by single OTAB fuel and a mixture of
OTAB and citric acid fuels. The spongy microstructure with
high specific surface area of 416 m2/g was achieved by the
higher amounts of mixture of OTAB and citric acid fuels. The
higher photodegradation rate of the OTAB-citric acid mixed
fuels was attributed to the high specific surface areas which
increased the adsorption capacity and low recombination rate
of photogenerated electrons and holes which increased the
formation of active species.
Declaration of Competing Interest
The authors declare that they have no conflict of interest.
Appendix A. Supplementary data
Supplementary data to this article can be found online at
https://doi.org/10.1016/j.jmrt.2021.01.003.
119
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