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Synthesis Techniques and Applications of Perovskite Materials

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DOI: 10.5772/intechopen.86794

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Chapter

Synthesis Techniques and

Applications of Perovskite
Materials
Dinesh Kumar, Ram Sagar Yadav, Monika,
Akhilesh Kumar Singh and Shyam Bahadur Rai

Abstract

Perovskite material is a material with chemical formula ABX3-type, which

exhibits a similar crystal structure of CaTiO3. In this material, A and B are metal
cations with ionic valences combined to +6, e.g., Li+:Nb5+; Ba2+:Ti4+; Sr2+:Mn4+;
La3+:Fe3+, and X is an electronegative anion with ionic valence (−2), such as O2−,
S2−, etc. The properties of a perovskite material strongly depend on the synthesis
route of materials. The perovskite materials may be oxides (ABO3:CaMnO3),
halides (ABX3: X = Cl, Br, I), nitrides (ABN3:CaMoN3), sulfides (ABS3:LaYS3), etc.,
and they may exist in different forms, such as powders, thin films, etc. There are
various routes for the synthesis of several perovskites, such as solid-state synthesis,
liquid-state synthesis, gas-state synthesis, etc. In this chapter, we discuss various
techniques for the synthesis of oxide perovskites in powder form using solid-, liquid-,
and gas-state synthesis methods, and we also present an overview on the other type
of perovskite materials. The X-ray diffraction, scanning electron microscopy, and
optical techniques are used to study the purity of crystallographic phase, morphology,
and photoluminescence properties of the perovskite materials. Some applications of
different perovskite materials are also discussed.

Keywords: XRD, perovskite, Rietveld refinement, FullProf Suite, lanthanide

phosphor

1. Introduction

The general chemical formula of a perovskite material is ABX3, which contains a

crystal structure similar to CaTiO3. It was initially discovered by German geologist
Gustav Rose in 1839 in Ural Mountains, and named after Russian mineralogist Lev
Perovski [1, 2]. In ABX3 perovskite, A and B are termed as metal cations having
ionic valences combined to +6, e.g., (Li+:Nb5+; Ba2+:Ti4+; Sr2+:Mn4+; La3+:Fe3+) and
X is an electronegative anion with ionic valence −2 such as O2−, S2− etc. [3–6]. The
perovskite materials may be oxides, halides, nitrides, sulfides, etc., and they may
exist in different forms, such as powders, thin films, etc. [7–10]. The perovskite
material has attracted our attention as it can house up a variety of cations at A- and
B-sites individually and/or simultaneously along with anions at X-site [11, 12]. The
perovskite materials can be classified in ideal and distorted perovskite materials.

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Perovskite Materials, Devices and Integration

An ideal perovskite material crystallizes into a simple cubic structure with

Pm 3 m space group. In the Pm 3 m space group with perovskite structure, A atoms
occupy 1(a) site at (0, 0, 0) and B atoms occupy 1(b) site at (1/2, 1/2, 1/2) whereas
X atoms occupy 3(c) site at (1/2, 1/2, 0). However, equivalently A, B, and X atoms
can also occupy 1(a) site at (1/2, 1/2, 1/2), 1(b) site at (0, 0, 0) and 3(c) site at (0, 0,
1/2), respectively, as shown in Figure 1. In this figure, A, B, and X are presented in
terms of ionic radii [13, 14]. In the unit cell of a perovskite, the cation “B” forms
octahedral arrangement with X-anions, i.e., BX6 and the cation “A” occupies cuboc-
tahedral site with X-anions, i.e., AX12.
The family of perovskite material includes numerous types of oxide forms, such
as transition metal oxides with the general formula of ABO3. The oxide perovskite
materials are widely synthesized and are studied for wide applications in various
technological fields. In light of these properties, we describe oxide perovskites in
more detail.
Victor Moritz Goldschmidt presented an empirical relationship among the ionic
radii of A, B, and O, known as tolerance factor (t) to estimate the stability of a
perovskite structure. This relation is valid for the relevant ionic radii at room tem-
perature [15]. The numerical value of the tolerance factor can be found by Eq. (1):

rA + r0
t= (1)
2 ( rB + r0 )

where, the term rA is the ionic radius of cation A and that of rB is ionic radius of
B cation whereas rO is the ionic radius of oxygen anion (O2−). The ionic radius of
A cation is always larger than that of the B cation. The tolerance factor provides an
idea about the selection of combination of A and B cations in order to prepare an
ideal perovskite material. Eq. (1) can also be expressed in other form, which may be
valid for any temperature as given by Eq. (2):

d A-0
t= (2)
2 dB-0

where dA-O and dB-O are average bond-lengths between A-O and B-O,
respectively [16].
The distorted perovskite materials are those materials, which crystallize into
other than the cubic structures. As far as we know that the perovskite material can
accommodate different ions at the A- and B-sites. The variation in the A- and/or
B-sites cations causes a variation in the tolerance factor. The variation in tolerance
factor leads to a change in the perovskite structure from cubic to non-cubic distorted
perovskite structure. For a stable perovskite, the value of tolerance factor should lie in
the range of 0.88–1.09 [17]. An ideal perovskite crystal exhibits tolerance factor equal
to unity (i.e., t = 1). For t < 1, the perovskite materials show the rhombohedral or
monoclinic structure while in the case of t > 1; it reveals tetragonal or orthorhombic
structure [18]. Due to distortion in the perovskite system, the BO6 octahedral led
tilted from an ideal situation and causes a change/enhancement in unit cell volume.
Thus, the tolerance factor is a measure of the extent of distortion in the perovskite
structure. Figure 2 shows unit cells for some distorted perovskite structures.
There are two general requirements for the formation of a perovskite material,
which are given as:

1. Ionic radii: the average ionic radii of A- and B-sites cations should be greater
than 0.90 Å and 0.51 Å, respectively, and the value of tolerance factor should
lie in the range of 0.88–1.09 [19, 20].

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2. Electro-neutrality: the chemical formula of perovskite material should have

neutral balanced charge; consequently, the sum of total charges at A- and
B-sites cations must be equal to total charges at O-site (oxygen) of anion(s).
A suitable charge distribution is to be achieved in the forms of A3+B3+O3 or
A4+B2+O3 or A1+B5+O3 [14, 19].

Figure 1.
Molecular structures for ABX3 perovskite with Pm 3 m space group along with the positions of different atoms
in a single unit cell. The figures (a) and (b) are equivalent structures to each other. In the figure (a), A and B
take the positions at the corner and body center of the cubic cell, respectively, and X is at the center of face of
the unit cell. However, in the figure (b), A and B occupy at body center and the corner of the cubic cell,
respectively, and X lies at the center of edge of the unit cell.

Figure 2.
Different distorted perovskite unit cells; (a) tetragonal, (b) orthorhombic, (c) hexagonal, and
(d) rhombohedral. Red spheres stand for oxygen anions.

3
Perovskite Materials, Devices and Integration

The pure perovskite materials (ABO3) do not always provide the desired
properties. In order to make them useful, the doping at A- and/or B-sites is
required. Doping at A- and/or B-sites improves the properties and also generates
very interesting phenomena due to change in crystal structure, bond-lengths,
ionic states, etc. The general chemical formula of A- and B-sites after doping in
the perovskite matrix may be found in the form of A1-xA′xBO3 (0 < x < 1) and
AB1-yB′yO3 (0 < y < 1), respectively. However, the simultaneous A- and B-sites
doped oxide perovskites have general formula A1-xA′xB1-yB′yO3. Recently, there
are several reports on lanthanide-based rare-earth doped perovskites [21–24].
Initially, we discuss the synthesis process used for the preparation of rare-earth
doped perovskite materials alongwith their phase identification, structural analysis
by Rietveld refinement of X-ray diffraction (XRD) patterns, morphological and
optical properties.

2. Synthesis techniques for perovskite materials

As we know that the physical, chemical, and optical properties of the perovskite
materials are strongly synthesis route dependent. One has to choose a suitable
synthesis method to obtain the desired properties from the prepared materials.
Synthesis techniques also affect crystal structure and morphology of the samples
[25]. The synthesis techniques can be divided into three main classes as given below:

1. Solid-state synthesis

2. Liquid-state synthesis

3. Gas-state synthesis

These techniques have their own advantages. Solid-state methods are used to
synthesize bulk materials, while liquid-state techniques are used to produce nano-
materials. However, gas-state methods are mostly used to fabricate thin films. In
this, we will discuss these techniques one by one by taking some suitable examples.

2.1 Solid-state synthesis technique

Solid-state synthesis technique is used to produce polycrystalline materials. It is

also known as ceramic method because most of the ceramics are synthesized by this
method. This is most widely used technique by researchers. This method requires
raw materials in carbonates and/or oxides forms. In this method, the raw materials
do not react chemically to each-other at room temperature. When the nixture of
raw materials is heated at very high temperatures (i.e., 700–1500°C), the chemical
reaction takes place at a significant rate.

2.1.1 Mechanical ball-milling method

It is one of the solid-state synthesis methods used for the production of bulk
perovskite materials. Synthesis of perovskites using this method involves grinding,
hand mixing, ball milling, and firing of starting materials in many times. In this
case, the raw materials used in oxides and/or carbonates forms are grinded, hand
mixed, ball milled, and calcined at a high temperature.
Let us describe the whole procedure of this synthesis technique by taking an
example of Ca0.97-xTiO3:3Yb3+,xBi3+ perovskite phosphor. For the synthesis of

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DOI: http://dx.doi.org/10.5772/intechopen.86794

CaCO3, TiO2, Yb2O3, and Bi2O3 were used as the raw materials. First of all, these
materials were weighed in the stoichiometric amounts and grinded and mixed by
hand in mortor by using pestle for 1–2 h. After hand mixing and grinding of all the
starting materials, the mixture was ball milled in a planetary ball milling system to
further get homogeneous mixture in the presence of acetone/alcohol as a mixing
media for 4–12 h at a nominal rpm (round per minute) of 25–100 in clockwise
and anticlockwise directions. After the ball milling, the homogeneous mixture
was dried at ordinary temperature and divided into various parts for calcination at
different temperatures from 600 to 1500°C for 4–30 h to optimize the pure phase.
These phosphors were then structurally and optically characterized [26]. The
perovskites prepared using this method have particles size in the submicrometer
range [27]. Some other rare earths doped R0.5Ba0.5CoO3 (R = La, Pr, Nd, Sm, Eu, Gd,
Tb, Dy) perovskites were also synthesized using this method [28].

2.1.2 High energy ball-milling method

This technique is very similar to that of mechanical ball-milling technique.

Only difference is that this method used very high rpm from few hundreds to few
thousands for milling with very small sized balls. This technique uses low tem-
perature for the synthesis of the oxide materials. This method produces generally
the nanoparticles. This method only takes metal oxides because there is very high
possibility of chemical reactions during high energy ball-milling, which may yield
different toxic gases.
Now, let us describe the whole process by considering an example of 0.7BiFeO3–
0.3PbTiO3 (BF-PT) solid solution [29]. The stoichiometric amounts of Bi2O3, Fe2O3,
PbO, and TiO2 were taken as raw materials to prepare BF-PT and were mixed using
agate mortar and pestle. Then the raw materials were ball-milled for 12–30 h with
zirconia balls using alcohol as mixing media in the ratio of 1:10 with the sample and
balls at 300–1000 rpm. Here, acetone or acid is not used for the purpose of mixing
of raw materials as it may damage the milling jars and O-rings. The material dried at
90°C was annealed at various temperatures (i.e., 400–900°C) to optimize the pure
phase of the sample. The XRD pattern of the samples was recorded to check the
purity of the synthesized perovskite materials.
For additional characterizations, such as dc poling and dielectric measurements,
the annealed sample was mixed in 2% aqueous solution of PVA (polyvinyl alcohol)
as binder and a pellet was made. The pellet of the perovskites was fired at 500°C
for 10–12 h to burn out the PVA binder. Then the pellet was sintered at quite higher
temperatures than annealing temperature to obtain the highly dense perovskite
material. To further check the purity of the samples after sintering, the XRD pattern
was recorded [30]. Sometimes, this method is also used to decrease the particles size
from a micrometric scale to nanometric scale. Figure 3 represents flow chart of the
preparation procedures for the synthesis of perovskite materials using solid-state
synthesis technique.

2.2 Liquid-state synthesis technique

The liquid-state synthesis technique is a method of synthesis of nanomaterials.

It is most widely used by researchers and scientists for the production of nanopar-
ticles of the oxide materials. In this method, the raw materials may be in the form of
nitrates, acetates or oxalates, which may react to each other at an ordinary tem-
perature. Auto-combustion, sol-gel, co-precipitation, etc. are different liquid-state
synthesis techniques used for the preparation of perovskite nanomaterials, which
are to be described in more detail [19].

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Perovskite Materials, Devices and Integration

2.2.1 Auto-combustion method

The auto-combustion synthesis method is a low-cost and very facile technique

for the production of perovskite nanomaterials. In this technique, the starting
materials are used in oxalates and/or acetates and/or nitrates forms, which are easily
soluble in de-ionized water. It involves some organic fuel, such as urea, citric acid,
and glycine to assist the combustion.
Let us describe the process of synthesis of the perovskite materials using
auto-combustion method (see Figure 4(a)) with the help of an example

Figure 3.
A representative flow-chart for the synthesis of oxide materials using ball milling technique.

Figure 4.
Schematic flow charts for the synthesis of oxide nanomaterials via (a) auto-combustion and (b) sol-gel methods.

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of La0.7Sr0.3MnO3 manganite. Kumar et al. have synthesized La0.7Sr0.3MnO3

perovskite manganite using the starting materials as La2O3, SrCO3, and
Mn(CH3COO)2.4H2O and glycine was used as fuel. First of all, La2O3 and SrCO3
were dissolved in diluted nitric acid to prepare their respective nitrates and then
Mn(CH3COO)2.4H2O and glycine were dissolved into distilled water. All the
prepared precursor solutions of the materials were dissolved/prepared indepen-
dently and at the end, they were mixed simultaneously under nonstop stirring in
a large beaker and heated on a magnetic stirrer at 175–200°C [31]. After continu-
ous stirring of 6–7 h, the mixed solution became thicker and converted into gel,
with further increase in time of stirring, an auto-ignition takes place resulting in
flame that evolves huge amount of different gases. During the ignition process,
the temperature of the whole mixture may reach upto 800–1000°C for very short
time duration. The obtained blackish-brown powder was collected from the bea-
ker and divided into various parts for the calcination at different temperatures.
The La0.7Sr0.3MnO3 perovskite comes up with different particles size range. They
have also prepared bulk samples of Ba1-xSrxMnO3 perovskites using the same
method [32]. The CaTiO3:Pr3+, Al3+ phosphor was also prepared by Yin et al. using
combustion method [33].

2.2.2 Sol-gel method

The sol-gel method is used by most of the chemists for producing nanomaterials.
This technique comprises both types of processes (physical and chemical) associ-
ated with the following, such as hydrolysis, condensation, polymerization, gelation,
drying, and densification [34]. In this technique, the starting materials are used
in the form of metal alkoxides. The general chemical formula of metal alkoxides is
M(OR)x. Metal alkoxides can be assumed either a derivative of the alcohol ROH,
where R is an alkyl group or a derivative of metal hydroxide M(OH)x [35]. The
stoichiometric amounts of metal alkoxides are weighed and dissolved in alcohol
or in de-ionized water at a temperature of 60–80°C under steady stirring. It is very
important to control the pH value of the metal alkoxides solutions to avoid the for-
mation of the precipitation and to form the homogeneous gel that can be achieved
by using basic or acidic solutions. This is known as hydrolysis and condensation
leads to form the polymeric chains. The progress of the polymeric chains eventually
results to a perceptible improvement in the viscosity of the reaction mixture and
the formation of a gel. The obtained gel is to be dried in temperature range between
150 and 200°C to remove the unwanted contents from the gel [35, 36]. After the
removal of contents, the obtained gel was annealed at various temperatures in
400–800°C range to obtain the pure phased materials.
Let us discuss the practical processes involve in this technique by taking an
example of La0.6Ca0.4MnO3 perovskite. Andrade et al. have synthesized nanotubes
and nanoparticles of La0.6Ca0.4MnO3 perovskite manganite using sol-gel method
following calcination at different temperatures [37]. They have used stoichiometric
amounts of La(NO3)3.6H2O, CaCO3 and Mn(CH3COO)2.4H2O for the synthesis of
La0.6Ca0.4MnO3 perovskite. The CaCO3 was dissolved in nitric acid to convert into
calcium nitrate, while La(NO3)3.6H2O and Mn(CH3COO)2.4H2O were dissolved in
distilled water. All the solutions were mixed together in a beaker. The appropriate
amount of polyethylene glycol (PEG) was incorporated to the precursor solutions
playing the role of polymerizing agent. Then the solution was heated at 70°C for 6 h
to complete the polymerization process. At last, the whole solution was converted
in yellow viscous gel, which was calcined at different temperatures from 700 to
1000°C. Figure 4(b) displays a representative flow chart of the processes involved
in the synthesis of perovskite materials using sol-gel method.

7
Perovskite Materials, Devices and Integration

2.2.3 Co-precipitation method

The co-precipitation method is also one of the methods used of the production
of nanomaterials. This method needs raw materials of metal cations from a general
medium and precipitates in the form of oxalates, carbonates, citrates or hydroxides
[38–41]. The resultant precipitates are several times washed with distilled water
and then obtained product was calcined at various temperatures to acquire the pure
phase of the desired materials in the polycrystalline form. This method can yield
almost homogeneous polycrystalline powders. The solubility of the used compounds
should be very close to each other for a proper precipitation [42]. The precursor
solutions are mixed at atomic level resulting lower particles size and it requires very
low calcination temperature to get a pure material [43]. The controlling pH of the
precursor solution, stirring speed, concentration, and temperature of the mixture
are important parameters for the co-precipitation method [44].
The LaMn1-xFexO3 (x = 0, 0.1, 0.2) perovskite synthesized by Geetha et al. is
an example of the co-precipitation method [45]. The stoichiometric amounts of
La(NO3)3.6H2O, Fe(NO3)3.9H2O and MnCl2.4H2O were dissolved in distilled water.
These solutions were mixed at one platform and stirred continuously at 50°C for
30 min. After this, NaOH solution was added slowly until the pH of solution is
attained to 13. The mixed solution of the precursors was again stirred constantly till
the formation of black precipitate. The precipitate was collected and washed many
times to remove the excess of chlorides and kept in an oven to dry at 50°C. Thus, the
final product was calcined at 800°C for 6 h.
It was observed that liquid-state technique produces nanoparticles of perovskite
materials at very low temperature. However, the sub-micron sized perovskite materials
can be obtained by firing them at higher temperature similar to solid-state technique.

2.3 Gas-state synthesis technique

Gas-state synthesis technique is also used to prepare the nanoparticles. It

contains various procedures for the synthesis of powder oxide materials, viz.
furnaces, flames, plasmas, and lasers. The basics of thermodynamics and kinetics
of the reaction are very similar to each other; however, their reactors are different.
These methods provide narrow distribution of the nanoparticles. The dispersion
must be reduced for narrow distribution of the nanoparticles as it leads to increase
the particles size [25]. Gas-state synthesis technique is a bottom-up method for the
synthesis of multifunctional nanoparticles. Method of bottom-up nanofabrication
is based on the gathering of nanomaterials from smaller components.
A variety of electronic devices and solar cells of perovskite materials are pre-
pared in terms of thin films via these techniques and they are entirely different from
the other synthesis techniques. There are various techniques for the preparation
of thin films, such as chemical vapor deposition [46], molecular beam epitaxy
[47], laser ablation [48], DC sputtering [49], magnetron sputtering [50], thermal
evaporation [51], and electron beam evaporation [52]. The gas-state synthesis
method needs particular set up for a good quality of samples to offer the preferred
properties. The gas-state synthesis techniques are categorized into three types:

a. Fabrication at the crystallization temperature under a suitable atmosphere

condition of temperature.

b. Fabrication in an intermediate temperature range (500–800°C) followed by

post-annealing treatment at higher temperatures.

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c. Fabrication at a very low substrate temperature followed by post-annealing

treatment at very high temperature.

The perovskite materials fabricated using gas-state techniques have variety of

applications ranging from optical and anticorrosion coatings to photocatalysts and
solar cells, from semiconductor devices to capacitor dielectrics, from bio-implantable
devices to chemical reactors and catalysts. One can undoubtedly say that the
industrial interest for preparing nanomaterial-based technologies through gas-state
synthesis is going to increase in the upcoming years.

3. Structural and optical properties

3.1 Identification of phase purity: X-ray diffraction studies

It is very important to check the phase and its purity of synthesized perovskite
materials. Without knowing the phase purity, one cannot come to any conclusion
about the properties exhibited by the perovskite materials. The XRD technique
is a suitable tool to identify the phase of perovskites. From the XRD data, one
can find out relative phase fractions of different phases present in the prepared
samples. One can also find out lattice constants, unit cell volume, crystallite size,
lattice strain, and theoretical density from Rietveld refinement of the XRD pat-
tern. The XRD technique is also used to optimize the synthesis conditions for the
perovskite materials. By matching the XRD pattern of the synthesized material
with the standard XRD pattern of the cubic phase of CaTiO3 (CT) perovskite,
one can conclude about the phase purity, i.e., whether, the perovskite is pure or
has some amount of impurity phase(s) or crystallizes in the distorted perovskite.
Figure 5 shows the XRD pattern of the cubic CT perovskite with JCPDS File
No. 75-2100 using X-ray radiation of 1.5406 Å wavelength. The analysis of
XRD pattern gives unit cell lattice parameter a = 3.795 Å and unit cell volume
V = 54.656 Å3. An ideal perovskite material displays reflections from all allowed
planes of the primitive unit cell. It shows most intense XRD peak for (1 1 0) plane
in the 2θ range of 32–34° and first singlet reflection corresponding to (1 0 0) plane
between 22 and 24°.

Figure 5.
The standard XRD pattern for the cubic phase of CaTiO3 perovskite.

9
Perovskite Materials, Devices and Integration

As we know that the different materials display different XRD patterns as like
the finger print of the humans. However, a certain prototype of materials gives the
XRD pattern in a well-defined manner. In order to make sure that the synthesized
sample is perovskite or not, we have to match the XRD pattern of the synthesized
sample with the XRD pattern of CT. If it matches it forms a perovskite phase
otherwise not.
Figure 6(a) shows the room-temperature XRD pattern for BaTiO3 (BT) syn-
thesized by mechanical ball-milling method followed by calcination at 950°C for
5 h and it is compared with XRD pattern of CT. The comparison of both the XRD
patterns reveals that the XRD pattern of BT matches with that of the CT. This
further confirms that BT is a perovskite material. The Bragg’s peaks in XRD pattern
of BT perovskite is shifted towards lower angle side compared to CT. This indicates
that the lattice parameters of BT are larger than that of the CT. Furthermore, the
Bragg peak around 22° is asymmetric in lower angle side, which shows doublet
nature in the peak, i.e., the lattice plane (1 0 0) of CT split into (0 0 1) and (1 0 0)
of BT is shown as inset in Figure 6(a). Similarly, the other Bragg’s peaks also show
asymmetrical behavior. All these observations reveal that the crystal structure
of BT is distorted from an ideal perovskite structure. The Rietveld refinement
of XRD pattern of BT reveals that the BT crystallizes into tetragonally distorted
structure with P4mm space group [53]. It has been also observed that the presence
of superlattice reflection(s) in the XRD pattern indicates the formation of distorted
perovskite structure from an ideal cubic [54, 55]. The structural analysis of the
known or unknown perovskite materials can be identified by Rietveld refinement
of the powder XRD pattern with the help of some standard software [56]. Most
of researchers use FullProf Suite to identify the structure of various perovskite
materials [57]. From Rietveld refinement, one can get lattice parameters, atomic
coordinates of the constituent atoms present in the unit cell, average bond-lengths
and angles, draw molecular structure to see the surroundings of the A- and B-sites’
cations with anions, and many more [29, 33, 58]. One can also find out magnetic
structure from the Rietveld refinement of the neutron diffraction data [59].
We performed the Rietveld refinement of XRD pattern of BT using P4mm
space group of the tetragonal structure. In P4mm space group, Ti4+-ions and
Ba2+-ions occupy 1(a) site at (0, 0, 0) and 1(b) site at (0.5, 0.5, 0.5 + δz), respec-
tively, while, O2−(1) and O2−(2) anions substitute 1(a) site at (0, 0, 0.5 + δz) and
2(c) site at (0.5, 0, δz), respectively [53, 60]. The structural analysis provides

Figure 6.
(a) Room temperature XRD pattern of BaTiO3 compared with the CaTiO3. The inset in (a) shows selected
Bragg’s peak between 21.0 and 23.5°. (b) Rietveld fit of the XRD pattern of BaTiO3. The inset in (b) shows
ball and stick molecular model for the unit cell of BaTiO3 perovskite, where Ba, Ti, and O are present in their
atomic sizes.

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lattice constants a = b = 4.0005(1) Å and c = 4.0255(2) Å and unit cell volume

V = 64.423(4) Å3 with tetragonality (c/a) of 1.006 close to the earlier reported
value [60]. Figure 6(b) shows Rietveld fit of the XRD pattern for the BT
perovskite. In this figure, the scattered dots are used to present experimental XRD
pattern and continuous line over experimental pattern is to show the simulated
XRD pattern. Lower continuous curve shows difference between experimental
and simulated XRD patterns. The vertical bars represent positions of the Bragg’s
reflection. The inset of Figure 6(b) demonstrates ball and stick molecular model
for the unit cell of P4mm space group for BT in terms of atomic sizes. It is clear that
Ba atom forms octahedral with oxygen atoms (BaO6) and Ti atom forms cubocta-
hedral with oxygen atoms (TiO12).

3.2 Morphological studies

The scanning electron microscopy (SEM) and transmission electron microscopy

(TEM) can be used to study the microstructure nature of the perovskite materials.
We have recorded SEM micrographs of Nd0.4Sr0.6MnO3 manganite samples calcined
at 800°C and 1200°C synthesized by auto-combustion method using FEI, Nova
Nano SEM for the Nd0.4Sr0.6MnO3 perovskite and they are shown in Figure 7. The
average values of the particle size were analyzed by ImageJ software and they are
found to be 50 and 425 nm for the Nd0.4Sr0.6MnO3 perovskites calcined at 800°C
and 1200°C, respectively. This clearly shows that the average particle size improves
on increasing the calcination temperature. It confirms that the sample calcined at
800°C produces nanomaterial whereas that of at 1200°C gives bulk material.

3.3 Optical studies

Figure 8 shows photoluminescence (PL) excitation and PL emission spectra of

the Nd0.4Sr0.6MnO3 manganite calcined at 800°C and 1200°C. Figure 8(a) shows the
excitation spectra of the Nd0.4Sr0.6MnO3 manganite in both the cases and contains
an intense peak at 355 nm [45]. It was monitored at an emission wavelength of
646 nm. The intensity of bulk material is two times larger than the nanomaterial.
When both the materials were excited with 355 nm they give strong red color at
646 nm as shown in Figure 8(b). It also contains weak peaks at 483 and 582 nm.
The emission intensity obtained in the case of bulk material is further two times
larger than the nanomaterial. This is due to the increase in crystallinity and particles
size of the materials. Thus, the calcination affects the morphology and optical
properties of perovskites even though the perovskite material was synthesized by
auto-combustion method.

Figure 7.
SEM micrographs of Nd0.4Sr0.6MnO3 manganite calcined at (a) 800°C and (b) 1200°C temperatures.

11
Perovskite Materials, Devices and Integration

Figure 8.
(a) PL excitation and (b) PL emission spectra of the Nd0.4Sr0.6MnO3 manganite calcined at 800°C and 1200°C
temperatures.

4. Applications of perovskite materials

The perovskite materials are extensively studied by researchers due to their

attractive properties. The perovskite materials have wide applications in various
fields, which are listed below:

1. Photocatalytic activity; e.g., LaFeO3 [61].

2. Photovoltaic solar cells; e.g., LaVO3 [62].

3. Phosphor materials in photoluminescence; e.g., Ho3+/Yb3+/Mg2+ doped

CaZrO3 [63].

4. Solid oxide fuel cells; e.g., Gd0.7Ca0.3Co1 − yMnyO3 [64].

5. Sensors and actuators; e.g., PbZrxTi1-xO3 [65].

6. Magnetic memory devices; e.g., Pt/La2Co0.8Mn1.2O6/Nb:SrTiO3 [66].

7. Magnetic field sensors; e.g., La0.67Sr0.33MnO3 and La0.67Ba0.33MnO3 [67].

8. Electric field effect devices; e.g., hetrostructure of Pb(Zr0.2Ti0.8)O3/

La0.8Ca0.2MnO3 [68].

9. Ferroelectric and piezoelectric devices; e.g., BaTiO3, PbTiO3 [69].

10. Semiconducting electronic devices; e.g., La0.7Ca0.3MnO3/SrTiO3/La0.7Ce0.3M

nO3 [70].

11. High dielectric constant; e.g., Bi1-xSrxMnO3 (x = 0.4, 0.5) [71].

12. High temperature superconductor; e.g., BaPb1-xBixO3 [72].

13. Hypothermia; e.g., La0.7Sr0.3MnO3 [73].

14. Supercapacitor; e.g., KNi0.8Co0.2F3 [74].

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Synthesis Techniques and Applications of Perovskite Materials
DOI: http://dx.doi.org/10.5772/intechopen.86794

Figure 9.
Block diagram of the lanthanide based perovskite phosphor materials including their applications in various
fields [75–82].

The lanthanide based perovskite phosphors are one of them and have unique
photolumincence properties. The lanthanide ions are known for their narrow and
sharp band emissions. They give emissions in the entire range of visible spectrum
along with ultraviolet (UV) and near infrared (NIR) regions. These emissions
are observed due to presence of meta-stable energy levels in the lanthanide ions.
These levels have long lifetime and are responsible for very strong emissions. The
lanthanide ions possess upconversion, downconversion, and quantum cutting
phenomena. In upconversion, the two or more than two low energy photons are
converted into high energy photons. When a high energy photon is converted into
low energy photons it is termed as downconversion process. However, in quantun
cutting, a high energy photon is converted into two low energy NIR photons. These
processes lead numerous technological applications in different fields, such as red
phosphors, light emitting diodes (LEDs), photonics, solar cells, tunable phosphors,
temperature sensing, biological studies, drug kinetics, etc. [63, 75–82]. Figure 9
shows a block diagram for the lanthanide based perovskite phosphors, which shows
their applications in various fields.

5. Conclusions

This chapter summarizes the basics of the perovskite structure, its stability
and distortion. We have discussed the novelty of the perovskite materials, which
accommodate different cations at A- and/or B-sites individually and/or simulta-
neously. We have also discussed various routes such as solid, liquid and gas-state
synthesis for the preparation of perovskite materials mostly in the oxide powder
forms. We have also briefly described the phase identification of the perovskites
and their structural analysis using Rietveld refinement of the XRD data by tak-
ing an example of tetragonal BaTiO3 perovskite. The morphological and optical
studies were also incorporated. We have also briefly listed various applications
of perovskite materials including lanthanide based perovskite phosphors in
various fields.

Conflict of interest

The authors declare no conflict of interest in the chapter.

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Perovskite Materials, Devices and Integration

Author details

Dinesh Kumar1, Ram Sagar Yadav2*, Monika3, Akhilesh Kumar Singh1

and Shyam Bahadur Rai3

1 School of Materials Science and Technology, Indian Institute of Technology,

Banaras Hindu University, Varanasi, Uttar Pradesh, India

2 Department of Zoology, Institute of Science, Banaras Hindu University,

Varanasi, Uttar Pradesh, India

3 Department of Physics, Institute of Science, Banaras Hindu University,

Varanasi, Uttar Pradesh, India

*Address all correspondence to: [email protected]

© 2020 The Author(s). Licensee IntechOpen. This chapter is distributed under the terms
of the Creative Commons Attribution License (http://creativecommons.org/licenses/
by/3.0), which permits unrestricted use, distribution, and reproduction in any medium,
provided the original work is properly cited.

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Synthesis Techniques and Applications of Perovskite Materials
DOI: http://dx.doi.org/10.5772/intechopen.86794

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