Ceramics International 48 (2022) 35100–35107

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Ceramics International
journal homepage: www.elsevier.com/locate/ceramint

Evaluation of La0.8 Sr0⋅2MnO3 perovskite prepared by fast

solution combustion
Ramón Cobo Rendón a, *, R. Udayabhaskar b, Christopher Salvo c, Erwin Sepúlveda a,
José Jiménez Rodríguez d, Carlos P. Camurri a, Mangalaraja Ramalinga Viswanathan a, e, **
a
Advanced Ceramics and Nanotechnology Laboratory, Department of Materials Engineering. Faculty of Engineering, University of Concepcion, Concepcion, Chile
b
Instituto de Investigaciones Científicas y Tecnológicas (IDICTEC), Universidad de Atacama, Copayapu 485, Copiapó, Chile
c
Departamento de Ingeniería Mecánica, Facultad de Ingeniería, Universidad Del Bío-Bío, Concepción, 4030000, Chile
d
National Center for Metallurgical Research, Superior Council of Scientific Investigations (CENIM-CSIC), X-ray Laboratory, Madrid, Spain
e
Faculty of Engineering and Sciences, Universidad Adolfo Ibáñez, Diagonal Las Torres 2640, Peñalolén, Santiago, Chile

A R T I C L E I N F O A B S T R A C T

Keywords: La0⋅8Sr0⋅2MnO3 (LSM) perovskite as oxygen electrode material for the reversible solid oxide fuel cells (ReSOFC)
LSM was synthesized by the fast solution combustion method and assessed for subsequent calcination influence. The
Fast solution combustion synthesis microstructural, morphological, compositional and optical properties of the obtained material were analyzed
Microstructure
with X-ray diffraction (XRD), high-resolution transmission electron microscopy (HR-TEM), scanning electron
ReSOFC
microscopy (SEM) coupled with an energy-dispersive X-ray spectroscopy detector (EDS) and UV–visible spec­
troscopy techniques. The XRD results showed the coexistence of rhombohedral R-3c and Pm-3m polymorphs for
the perovskite phase, with a decreased fraction of the cubic phase as the temperature and/or time used for the
calcination were increased. The HR-TEM images confirmed the existence of the R-3c and Pm-3m polymorphs for
the sample subjected to calcination at 1300 ◦ C, showing that the rapid combustion method did not allow the pure
formation of the La0⋅8Sr0⋅2MnO3 phase for the calcination temperatures below 1400 ◦ C, due to the swiftness of
the combustion synthesis 500 ◦ C for 5 min. The average grain size was found to be increased with the calcination
time. The EDS analysis depicted a better agreement in stoichiometry with the theoretical composition. The
apparent porosity was decreased with the increase in the temperature and calcination time due to the coales­
cence of the sintering pores. The sample obtained after the calcination at 1400 ◦ C for 8 h exhibited 1.6% of
porosity. The hardness was improved with the higher calcination time and temperature and reached a maximum
value of 5.7 GPa that merely matched the bulk density. A similar trend was observed in the temperature
dependence resistivity studies and all the samples presented a low resistivity of ~1.2 Ω cm in the temperature
range of 600–700 ◦ C. The optical characterization exhibited a broad absorption in 560–660 nm.

1. Introduction their high thermo-chemical compatibility. The remarkable electronic

Strontium-doped lanthanum manganite La1-xSrxMnO3 (LSM) is a
widely used material for magnetic sensors, gas monitoring, information
storage, carbon monoxide (CO) pollutant removal and fuel cell tech­
nology. Especially as cathode material in the reversible solid oxide fuel
cells (ReSOFC) due to its high chemical and thermal stability and elec­
trocatalytic activity for oxygen (O2) reduction [1–4]. LSM is used
together with yttrium-stabilized zirconia (YSZ) electrolytes by virtue of
conductivity and thermal expansion coefficient of La0⋅8Sr0⋅2MnO3, pave
its way as a suitable commercial component for the ReSOFC applica­
tions. As a result, significant efforts have been devoted to the processing
and characterization of this material. Various methods such as
solid-state reaction, polymer precursor method [5,6], hydrothermal [7,
8], spray pyrolysis [9,10], sol-gel [11–14], co-precipitation [15–18],
and combustion process [19–25], have been explored to fine tune the
size (dispersion) of particles, conductivity (electronic and

* Corresponding author..
** Corresponding author. Advanced Ceramics and Nanotechnology Laboratory, Department of Materials Engineering. Faculty of Engineering, University of Con­
cepcion, Concepcion, Chile.
E-mail addresses: rcobo@udec.cl (R. Cobo Rendón), mangal@uai.cl (M.R. Viswanathan).

https://doi.org/10.1016/j.ceramint.2022.08.105
Received 18 June 2022; Received in revised form 1 August 2022; Accepted 9 August 2022
Available online 13 August 2022
0272-8842/© 2022 Published by Elsevier Ltd.
R. Cobo Rendón et al. Ceramics International 48 (2022) 35100–35107

electrocatalytic), chemical and thermal stability. Table 2

The development of new synthesis approaches for the commercial La0⋅8Sr0⋅2MnO3 preparation parameters.
scale, fast and cost-effective, to produce the powders with desired Temperature, ◦ C
characteristics, and the use of tools to evaluate the efficiency of the
500 C
◦
processing steps are of vital interest to improve the electrode perfor­ 1300 ◦ C
mance. In this concern, the solution combustion synthesis, which has 1300 ◦ C
been used to prepare a variety of compounds for technological appli­ 1400 ◦ C
cations and especially for the development of ReSOFC components with 1400 ◦ C
Time, hrs Code name
5min LSM500
4 LSM1300-4h
8 LSM1300-8h
4 LSM1400-4h
8 LSM1400-8h

the desired composition and structure, is a good option due to its

simplicity, cost-effectiveness, and quality of the product obtained
[26–29]. Thus, in this work, the La0⋅8Sr0⋅2MnO3 materials were syn­ Table 3
thesized by the fast solution synthesis method [29], which is a modified Positional parameters for perovskite phases in the Rietveld refinements [30].
version of the combustion solution method to make it faster. The Atoms Sites Site Occupancy Atomic coordinates
morphology, structure, composition, and optical properties of the pre­ La0⋅8Sr0⋅2MnO3 Space group R-3c (167)
pared LSM were systematically investigated. La,Sr 6a 0.8La+0.2Sr 0, 0, 1/4
Mn 6b 1 0, 0, 0
2. Materials and methods O 18e 1 x, 0, 1/4
Space group Pm-3m (221)
La,Sr 1b 0.8La+0.2Sr 1/2, 1/2, 1/2
2.1. Processing and characterization of powders Mn 1a 1 0, 0, 0
O 3d 1 1/2, 0, 0
For the synthesis of La0⋅8Sr0⋅2MnO3: La(NO3)3⋅6H2O (99.9%), Sr LaSrMnO4
(NO3)2 (99.8%), Mn(NO3)2.4H2O (97%) were used as precursors for La, Space group I4/mmm (139)
La,Sr 4e 0.5La+0.5Sr 0, 0, 0.356
Sr, and Mn metals, respectively. As a fuel, citric acid (C6H8O7, 99.99%) Mn 2a 1 0, 0, 0
in the stoichiometric ratio (Table 1) was dissolved with the metal pre­ O1 4c 1 0, 1/2, 0
cursors in 50 mL of double distilled water by magnetic stirring (500 rpm) O2 4e 1 0, 0, 0.153
at room temperature for 1 h.
The resultant homogeneous solution was transferred to an alumina
contribution to peak broadening. Uncertainties in all fitted parameters
crucible and placed in a preheated furnace (Nabertherm, LT 40/12,
were determined from the standard deviations obtained from the Riet­
Lilienthal, DE) at 500 ◦ C for 5 min to engage the fast solution combus­
veld refinements. However, it should be noted that the domain size and
tion process. After the combustion process, a foam-like spongy material
deformation parameters have reliability ranging between 10 and 20%,
was obtained, gently crushed, and grounded in a mortar to get the
associated with limitations in the description of the profiles of the
corresponding powder. The powder was then calcined at 1300 and
diffraction lines that could lead to large standard deviations. The
1400 ◦ C for two different time durations (4 and 8 h) by using a tem­
agreement between the observed and calculated intensities in the re­
perature rate of 10 ◦ C/min to remove any residues from the combustion
finements was evaluated quantitatively by the figure of merit (FoM) or
process and to consolidate the crystalline phase.
R-factor [32]. The most often used agreement factors are the statistically
Also, the combusted LSM powder (0.5 g) was compacted (10000 Lb
expected least-squares factor of the count statistic (Rexp), the weighted
for 1 min) to form pellets of 11.2 mm in diameter and 1.1 mm in
summation of residual of the least-squares fit (Rwp), and the goodness of
thickness. Each pellet was then sintered at the same temperatures of
fit (GoF or chi-square), which can be determined from the other two
1300 and 1400 ◦ C for 4 and 8 h to obtain the crystal structure of the
R-factors as GoF= (Rwp/Rexp)2. Small values of Rwp and Rexp are the
cathode. The code numbers of the samples are given in Table 2.
indicators of successful minimization and good data quality, respec­
The crystallographic information of the calcined powders was ob­
tively. When the data collected to a very high precision, the Rwp and Rexp
tained using the XRD patterns recorded at room temperature with a
values should be similar for a good refinement, and then a GoF close to 1
Bruker AXS D4 Endeavor diffractometer using Cu-Kα radiation (λ =
means that the model is correct.
1.5418 Å). The XRD spectra were collected in Bragg-Brentano geometry
The morphology and composition of the material were studied by a
ranging from 20 to 70◦ with a step width of 0.02◦ and a counting time of
scanning electron microscope (SEM) (Tescan, Vega 3 Easyprobe SBU,
1s per step. The obtained patterns were refined using version 4.2 of the
Czech Republic) equipped with an energy-dispersive X-ray detector
Rietveld analysis program TOPAS (Bruker AXS) and the crystallographic
(EDS). Also, high-resolution transmission electron microscopy (HRTEM,
information of the rhombohedral R-3c and cubic Pm-3m polymorphs for
Boston, MA, USA) was adopted to obtain the high-resolution images to
La0⋅8Sr0⋅2MnO3 perovskite and the SrLaMnO4 phase obtained from the
verify the existence of phases in the material using the Gatan Microscopy
Pearson’s crystal structure databases and are provided in Table 3 [30].
Suite software. A UV–vis spectrophotometer (Shimadzu UV-2600,
The refinement protocol included the unit-cell parameters, the oxygen
Japan) was utilized for optical absorption studies. For the temperature
fractional coordinates x for the rhombohedral phase, background, and
dependence resistivity studies (50–700 ◦ C), the LSM samples were
two-theta offset. Finally, the microstructural parameters like crystallite
examined using the conventional four collinear probe method with
size and microstrain were simultaneously determined from line broad­
Keithley 4200-SCS. The mechanical microhardness at room temperature
ening of the diffraction patterns by the double Voigt approach [31]. For
of the consolidated material was evaluated using an 8187.5 ZHU Zwick/
this analysis, a corundum reference sample provided by Bruker was
Roell microhardness tester. The bulk microhardness of each sample was
measured under the same conditions to eliminate the instrumental
characterized by an average value taken from ten indentations carried
out by applying a load of 10 N on a polished surface for 10 s at different
Table 1 locations.
La0⋅8Sr0⋅2MnO3 preparation parameters.
Precursors Quantity (g)
3. Results and discussion

La(NO3)3⋅6H2O 2.992
The XRD patterns of the La0⋅8Sr0⋅2MnO3 samples synthesized by the
Sr(NO3)2 0.366
Mn(NO3)2⋅4H2O 2.168 rapid solution combustion method are shown in Fig. 1. It shows the XRD
C6H8O7 2.212 of the combusted sample (LSM500), and the samples calcined at 1300

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phase in the Rietveld refinement led to a significant improvement of the

Fig. 1. XRD patterns of the La0⋅8Sr0⋅2MnO3 combusted and calcined at 1300
and 1400 ◦ C for different time duration (4 and 8 h).
and 1400 ◦ C for two different time durations (4 and 8 h). It is clearly
observed an increment in the intensity of the diffraction peaks, which is
associated with a higher crystallinity and the increase of the particle size
produced by the calcination process and is increased with the sintering
temperature [33,34]. The primary phase observed in these diffracto­
grams corresponds to the rhombohedral R-3c polymorphs of the
La0⋅8Sr0⋅2MnO3 perovskite (JCPDS card 98-009-7866) as the superlattice
peaks due to MO6 octahedral tilting can be observed. It is evident that all
samples are formed by a single phase, but the sample without heat
treatment (LSM500) includes the presence of some impurities. On the
other hand, it has been reported that very different physical properties
can be obtained in perovskites with this composition by the various
synthesis methods and heat treatments, which have been related to the
variation of the composition, stoichiometry and defect structures in the
material [1,18,35]. Thus, it is not wrong to expect the presence of other
polymorphs with nominally identical compositions or some impure
phases, which may play an essential role in the properties. However,
matching the XRD pattern with the JCPDS database did not allow un­
ambiguous identification of other polymorphs of this phase in these
samples due to the overlapping of the diffraction peaks. This problem
can be surpassed by using the Rietveld analysis, which provides a viable
decomposition of the experimental XRD pattern calculated from the
crystal structures of the reported polymorphs of the La0⋅8Sr0⋅2MnO3
perovskite.
The Rietveld analysis was performed carefully to ascertain the exact
crystallographic nature of the samples. Although the XRD data have
been successfully modeled with space-group symmetry R-3c as the
major perovskite phase, the inclusion of Pm-3m polymorphs as a second
fit (GoF) for the sample calcined at 1300 ◦ C for 4 h. The Rietveld
refinement of XRD patterns of LSM1300-4h is shown in Fig. S1. The
difference between the experimental data and the fitted simulated
pattern is provided as a continuous. A closer inspection of the difference
curve (grey line) depicted the better fit in Fig. S1 (a), suggesting the
coexistence of two distinct La0⋅8Sr0⋅2MnO3 perovskite polymorphs in the
samples, which include a higher fraction of a less distorted version of the
stable La0⋅8Sr0⋅2MnO3 polymorph at room temperature when the tem­
perature and/or the calcination time decreased. Assuming that the sum
of those crystalline phases was 100%, the concentration distribution (in
wt.%) among the different phases determined from the Rietveld
refinement is listed in Table 4. Also, it can be seen in this table the
presence of less than 1% of the LaSrMnO4 phase. A small amount of this
phase in the material is under study, which has also been reported in
previous works [36–38]. The presence of this phase degrades the per­
formance of LSM in SOFC since the electrical conductivity of the
LaSrMnO4 phase is much lower than the LSM perovskite [39].
LaMnO3 perovskites adopt a highly symmetric Pm-3m cubic struc­
ture at elevated temperatures. As temperature decreases, the corner-
sharing MO6 octahedral in this parent structure may tilt that concerns
one another, giving rise to the polymorphic transition to lower sym­
metry. Therefore, the two most common space groups at room tem­
perature for this compound are R-3c and Pnma. In LaMnO3 perovskite,
when La2+ is substituted by Sr3+, the calcination process leads to an off-
stoichiometric product with the composition (LaMn)1-δO3, thereby the
Mn3+ must partially oxidize to Mn4+ to keep the charge neutrality. The
increase in the total fraction of Mn4+ cations also reduces the Jahn-
Teller static distortion, leading to a “more cubic” structure [40]. Thus,
some investigations reported that the structure of La1-xSrxMnO3 perov­
skites materials calcined in air and slowly cooled to room temperature
are rhombohedral for 0 ≤ x ≤ 0.5 [1,18,36,41] and cubic after annealing
in oxygen for 0.7≤ x ≤ 1 [18,42–44].
The temperature and calcination time are the key factors that in­
fluence phase segregation. This is also associated with the heteroge­
neous distribution of Sr and La in the as-prepared powder samples
obtained from the fast solution combustion method. At a low tempera­
ture and/or calcination time, a higher concentration of Sr in some re­
gions of the as-prepared powders and a high cation vacancy
concentration at the ultrafine-grain boundaries will convert Mn3+ into
Mn4+. Thus the crystal structure of the perovskite material can change
locally to cubic. When the calcination temperature and annealing time
were increased to 1400 ◦ C and 8 h, it promoted a homogenous solid
solution formation with a single uniform R-3c phase. Thus, the cubic
phase is not present in the sample calcined at 1400 ◦ C for 8 h.
The morphology and microstructure of the calcined powders were
examined by scanning electron microscopy (SEM) and high-resolution
transmission electron microscopy (HRTEM). To corroborate the exis­
tence of the polymorphs described in the Rietveld analysis, the samples
LSM1300-4h and LSM1400-8h are analyzed as they exhibited the
highest and lowest quantities of different LSM polymorphs. Figs. 2 and 3

Table 4
Quantitative phase analysis and microstructural parameters obtained after Rietveld refinement of the LSM samples.
Sample Phases wt. % Lattice parameters (Ǻ) O (18e)-Position (x) Crystallite size (nm) R-factors

LSM1300-4h La0⋅8Sr0⋅2MnO3 S.G: R-3c 88.6% a = b = 5.519 (2) c = 13.350 (3) 0.448 (1) >150 Rexp = 3.13
S.G: Pm-3m 10.9% a = 3.873 (1) >150 Rwp = 5.10
LaSrMnO4 S.G:I4/mmm 0.5% a = b = 3.837 (2) c = 12.55 (2) GoF = 1.63
LSM1300-8h La0⋅8Sr0⋅2MnO3 S.G: R-3c 94.3% a = b = 5.519 (2) c = 13.350 (3) 0.449 (1) >150 Rexp = 2.93
S.G: Pm-3m 5.2% a = 3.861 (2) >150 Rwp = 6.18
LaSrMnO4 S.G:I4/mmm 0.5% a = b = 3.837 (2)c = 12.55 (2) GoF = 2.11
LSM1400-4h La0⋅8Sr0⋅2MnO3 S.G: R-3c 97.3% a = b = 5.521 (2) 0.450 (1) >150 Rexp = 3.13
c = 13.354 (3)
S.G: Pm-3m 2.1% a = 3.863 (2) >150 Rwp = 5.57
LaSrMnO4 S.G:I4/mmm 0.5% a = b = 3.837 (2) c = 12.55 (2) GoF = 1.78
LSM1400-8h La0⋅8Sr0⋅2MnO3 S.G: R-3c 99.5% a = b = 5.522 (2) c = 13.357 (3) 0.452 (1) >150 Rexp = 3.35. Rwp = 5.62. GoF = 1.68
LaSrMnO4 S.G:I4/mmm 0.5% a = b = 3.841 (2) c = 12.50 (2)

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Fig. 2. HRTEM images for LSM1300-4h powder sample.

Fig. 3. HRTEM images for LSM1400-8h powder sample.

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R. Cobo Rendón et al.
show the images examined by HRTEM for the samples LSM1300-4h and
LSM1400-8h. Both the images show well-defined lattice fringes,
corroborating the findings of the Rietveld analysis of the XRD patterns.
From Fig. 2, the LSM1300-4h sample exhibited the coexistence of the
three phases that correspond to different interplanar distances: (i) 0.224
nm related to the lattice plane (006) of the R-3c rhombohedral phase of
La0⋅8Sr0⋅2MnO3; (ii) 0.1192 nm coinciding with the (130) plane of the
LaSrMnO4 phase and (iii) 0.2231 nm associated to the (111) plane of the
Pm-3m cubic polymorph of the perovskite La0⋅8Sr0⋅2MnO3.
In the case of sample LSM1400-8h (Fig. 3), an extensive search for
the presence of the phases detailed by Rietveld analysis was carried out.
Two zones of the same image were analyzed to determine the presence
of these phases. In zone 1, only the presence of the La0⋅8Sr0⋅2MnO3 in the
rhombohedral R-3c phase was exhibited that confirmed by the identi­
fication of (104) and (012) planes that coincide with the interplanar
distance of 0.221 and 0.395 nm, respectively. By performing the analysis
of zone 2, it was possible to associate the presence of the interplanar
distance of 0.2655 nm coinciding with the (110) plane of the minority
LaSrMnO4 phase. The results are in line with the refined XRD data.
Similar results were reported by the research of several authors [36–39],
where they noticed the presence of the LaSrMnO4 phase for
800–1200 ◦ C, using the glycine/nitrate process (GNP). The existence of
this phase is a result of the A/B cation ratio, Sr content and sintering
temperature. According to several authors, this phase is present when
A/B > 1. It is also mentioned that doping with Sr in 0.2 mol content
facilitates the formation of this phase. The Rietveld analysis and the
images obtained by HR-TEM confirmed the existence of a minority
LaSrMnO4 phase in our samples that calcined at 1300 and 1400 ◦ C.
Thus, the fast combustion method does not allow the pure formation of
the La0⋅8Sr0⋅2MnO3 phase at calcination temperatures below 1400 ◦ C,
due to the rapidity of the synthesis process at low formation
temperatures.
The morphology of the synthesized powders, as shown in Fig. 4,
represented irregular grain distribution with less than 1.5 μm for all
samples. The sample only combusted (LSM500) does not exhibit clear
grain boundaries. With heat treatment application, grain boundaries
become evident, grain size and number of grain boundaries increase and
decreased intragranular porosity. The formation of agglomerates with a
size of less than 1.8 μm was evident for the temperature change from
1300 to 1400 ◦ C. La0.8Sr0.2MnO3 particles from LSM1400-8h showed the
most prominent grain sizes.
The average grain size of the samples is shown in Table 5. The higher
sintering/calcination temperature provides better diffusion of the crys­
tallites or grains, which leads to an increase in the grain size or
agglomerate formation [45], as observed in the measured grain sizes.
These sizes agree with several investigations of other synthesis methods
[1,46,47].
Furthermore, the samples exhibited a porous structure. The bulk
density and apparent porosity were measured using the Archimedes
method, and the values are presented in Table 5. As expected, the
porosity is reduced by increasing the sintering/calcination temperature
and time due to the coalescence of the pores. On the other hand, the
hardness is increased at a higher calcination temperature and time,
which is closely related to the higher bulk density, reaching a maximum
value of 5.7 GPa for the samples calcined at 1400 ◦ C for 8 h (LSM1400-
8h).
The compositional analysis and stoichiometric percentages by
weight of La, Sr and Mn of the calcined powder samples were obtained
by energy dispersive X-ray spectroscopy (EDS) and are shown in Table 6.
These results are in close agreement with the intended stoichiometry
and support the results obtained by the Rietveld analysis of XRD.
From the EDS analysis, an intimate relationship between the applied
heat treatment and the optimization of the desired stoichiometry is
observed. It can be verified that the increase in temperature and time of
calcination favors the narrowing of the differences between the theo­
retical and experimental values of stoichiometry. This narrowing may be
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Ceramics International 48 (2022) 35100–35107
due to the loss of elements with increasing temperature and exposure
times. The nature of the values obtained in the EDS analysis confirms the
stoichiometric control during the synthesis and avoids any wrong in­
terpretations about the composition of the material. The relevant over-
stoichiometry of the oxygen is due to the oxygen’s minor weight na­
ture for the scattering of X-ray radiation [48–50].
The LSM samples are ceramic, but several investigations show min­
imal resistance, so it was decided to measure by the four collinear probes
technique to eliminate the contact resistance between the sample and
the electrical contacts. The measurement was carried out by passing a
constant DC voltage in the range of − 3 to 3 mV with a 2 × 10− 6 step,
through a pair of electrical wires at the ends of the sample, and through
another pair of wires the current due to the sample resistance was
measured.
The variation of resistivity with temperature is shown in Fig. 5 for the
LSM samples. All the samples exhibited a decrease in resistivity with an
increase in temperature, which is typical for the LSM samples [45,51].
The decline in resistivity with increasing temperature is associated with
the increased charge carrier mobility. The increase in the conductivity of
LSM is attributed to the electron hopping from Mn3+ to Mn2+.
The electrical transport properties depend not only on the grain size
of the samples but also on the porosity of the sample. LSM1400-8 h
sample presented a lower resistivity and lower resistive change con­
cerning the temperature. This is an excellent factor since it also
exhibited a larger grain size, as observed from the morphological
characterization and lower porosity that triggers an appreciable
decrease in resistivity. Earlier investigations reported higher resistivities
at lower characterization temperatures, thus supporting the low re­
sistivity behavior of the developed samples [52–54]. Varshney and
Dodiya [52] noted a minimum resistivity of 3.5 Ω cm at low
temperatures.
For intermediate temperatures, Wu, Qiu [53] and Zhu and Liu [54]
reported resistivities of 21 and 40 Ω cm, respectively. It is important to
note that the previously described findings are developed at low and
intermediate temperatures, while our study has been developed at
operational temperatures using LSM as the oxygen electrodes in SOFC,
SOEC, and ReSOFC modes. Despite this, our results showed resistivity
values lower than previously mentioned, approaching 1.2 Ω cm in the
temperature range of 600–700 ◦ C.
The optical absorption properties of the La0⋅8Sr0⋅2MnO3 are shown in
Fig. 6. A strong, broad absorption band of 300–800 nm was observed.
The broad absorption band extended towards 680 nm and then
decreased. However, a second relevant absorbance can be seen at 370
nm for the samples calcined at 1300 ◦ C (irrespective of calcination time)
and for the sample LSM1400-8h, which presented the highest purity
phase. The absence of this absorption peak in LSM1400-4h may be due
to the crystal defects formed during the growth of the LSM nano­
powders. The observed trend is attributed to the increase in grain size
identified by the SEM analysis [18,55,56].
4. Conclusions
La0⋅8Sr0⋅2MnO3 was successfully obtained by the fast solution com­
bustion synthesis followed by the heat treatment at 1300 and 1400 ◦ C
for 4 and 8 h. The results obtained by the XRD indicated that the samples
had perovskite structure, and the highest purity phase was presented in
the samples calcined at 1400 ◦ C for 8 h (LSM1400-8h) with rhombo­
hedral structure (R-3c) and the crystallite size of >150 nm. The Rietveld
analysis of the XRD data indicated the coexistence of R-3c and Pm-3m
polymorphs of La0⋅8Sr0⋅2MnO3 samples obtained from calcination tem­
peratures below 1400 ◦ C. The images obtained by HR-TEM and analyzed
by Fast Fourier Transform (FFT) showed the coexistence of the poly­
morphs R-3c and Pm-3m for the sample LSM1300-4h and the existence
of the pure phase of La0⋅8Sr0⋅2MnO3 in the sample LSM-1400-8h. The
images extracted by SEM showed the influence of calcination parame­
ters on the grain size and the formation of agglomerates up to 3 μm. The
R. Cobo Rendón et al. Ceramics International 48 (2022) 35100–35107

Fig. 4. SEM images and grain size distribution of the combusted and calcined LSM powders.

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Table 5
Mechanical and physical properties of the La0⋅8Sr0⋅2MnO3 samples obtained at
different calcination temperatures and times.
Sample LSM1300- LSM1300- LSM1400- LSM1400-
4h 8h 4h 8h

Hardness (GPa) 0.8 ± 0.1 3.5 ± 2.1 2.3 ± 1.3 5.7 ± 1.3
Bulk density (g/ 5.2 5.3 5.5 5.7
cm3)
Apparent porosity 13.5 9.7 5.1 1.6
(%)
Average grain size 580 620 580 670
(nm)

Table 6
Stoichiometric weight percentage of the La0⋅8Sr0⋅2MnO3 powder samples
calcined at different temperatures and times.
Sample Atom La Sr Mn O Total

Stoichiometric 0.8 0.2 1 3

LSM1300-4h Weight % (Expe.) 46.54 6.43 23.1 23.93 100

Weight % (Theo.) 47.98 7.57 23.72 20.73 100 Fig. 6. Absorbance spectra of the La0⋅8Sr0⋅2MnO3 samples.
Difference (%) 3.00 15.06 2.61 15.44
LSM1300-8h Weight % (Expe.) 46.19 6.99 21.83 24.99 100 sample LSM1400-8h exhibited low resistivity of approximately 1.2 Ω cm
Weight % (Theo.) 47.98 7.57 23.72 20.73 100
over a SOFC, SOEC, and ReSOFC operational temperature range
Difference (%) 3.73 7.66 7.97 20.55
LSM1400-4h Weight % (Expe.) 45.71 6.91 21.55 25.83 100 (600–700 ◦ C). The optical property for the developed samples showed a
Weight % (Theo.) 47.98 7.57 23.72 20.73 100 broad absorption maximum of 300–800 nm and sharp secondary ab­
Difference (%) 4.73 8.72 9.15 24.60 sorption at 370 nm. Based on these results, the La0⋅8Sr0⋅2MnO3 perov­
LSM1400-8h Weight % (Expe.) 46.68 7.3 22.01 24.01 100 skite cathode material obtained by the fast solution combustion
Weight % (Theo.) 47.98 7.57 23.72 20.73 100
Difference (%) 2.71 3.57 7.21 15.82
synthesis method exhibited the development of a material with critical
physicochemical properties in a fast and controlled way that can have an
application as the oxygen electrode in the ReSOFC and related fields of
advanced ceramics.

Declaration of competing interest

The authors declare that they have no known competing financial

interests or personal relationships that could have appeared to influence
the work reported in this paper.

Acknowledgments

The authors acknowledge the FONDECYT-ANID (Project No.

1181703) for the financial support. Ramón Cobo-Rendón thanks to
ANID-Chile Grant No.: 21210463.

Appendix A. Supplementary data

Supplementary data to this article can be found online at https://doi.

org/10.1016/j.ceramint.2022.08.105.

Fig. 5. Variation of resistivity with the temperature of calcined

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stoichiometry. The dependence of resistivity with temperature for the
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