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Nanomedicine & Nanotechnology Open Access Research Article 9 min read

Tailored Synergy: Synthesis and In-Depth Structural Analysis of x[Ni0.2Cu0.3Co0.5Fe2O4] + (1-x)[Ba0.7Sr0.3TiO3] Composites

Mathad SN*
* Corresponding author
ISSN: 2574-187X  10.23880/nnoa-16000293  Received: February 05, 2024  Published: February 23, 2024
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 28 references
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Keywords
Ferrites Ferroelectrics Porosity Micrographs Grain Diameter
Abstract

M E Composites with composition x[Ni0.2 Cu0.3 CO0.5 Fe2O4] + (1-x)[Ba0.7Sr0.3TiO3], Where x varying from 0.1 to 0.4 in molar ratio, were prepared by standard double sintering ceramic technique. The presence of ferrites phase, namely [Ni0.2 Cu0.3 CO0.5 Fe2O4] and ferroelectric phase, namely [Ba0.7Sr0.3TiO3], were confirmed by X-Ray Diffraction analysis, whereas SEM micrographs were obtained to study the morphology of samples. The x ray diffraction patterns exhibit a set of well-defined ferrites and ferroelectric peaks. The tetragonality ratio c/a, of the ferroelectric phase remains the same in all the samples, the porosity varies from 20% to30% while the average grain diameter lies in the range of 0.5μm to 2 μm.

Introduction

Ferroelectrics and ferrites play crucial roles in various electronic applications, from nonvolatile materials to data storage. In the pursuit of advancing materials science, the exploration of multifunctional composites has gained significant attention. These composites, which combine different phases, offer a wide range of applications, from electronic devices to energy storage systems [1, 2, 3, 4]. One promising avenue is the synthesis and characterization of ferrite-ferroelectric composites, leveraging the unique properties of both materials. Ferrite-ferroelectric composites combine magnetic ferrites, typically composed of iron oxide compounds, with ferroelectrics, which exhibit spontaneous electric polarization. This combination results in materials with enhanced electromagnetic and ferroelectric properties [5, 6, 7, 8, 9]. Key aspects of these composites include synthesis, electromagnetic and ferroelectric properties, magnetoelectric coupling, tunable microwave devices, energy harvesting, and lead-free ferroelectrics [10, 11, 12, 13, 14, 15, 16, 17].

There are two types of multiferroics: single-phase, where one material possesses both ferroelectric and magnetic ordering, and composites, consisting of different phases with ferroelectric and magnetic properties [18, 19, 20, 21]. Examples include BiFeO3 and BiMnO3 for single-phase, and (Ni,Zn)Fe2O4−BaTiO3, BaSrTiO3−(Ni,Zn)Fe2O4, Ni(Co,Mn) Fe2O4−BaTiO3, and CoFe2O4−BaTiO3 for composites [22, 23, 24, 25].

In this research, the focus is on integrating Ni-Cu-Co Ferrite with BST, aiming to exploit synergies from their complementary properties. Various compositions are explored to find the optimal blend with superior attributes for specific applications. The study involves synthesizing the x[Ni0.2Cu0.3CO0.5Fe2O4] + (1-x) [Ba0.7Sr0.3TiO3] composites through the solid-state method, followed by in-depth characterization of their structural properties. Ultimately, the goal is to contribute valuable insights for the development of advanced materials with tailored functionalities and improved performance.

Experiment

Both ferrite and ferroelectric phases were prepared through a standard solid state reaction method, using AR grade NiO, CuO, CoO and Fe2O3 powders in molar ratio as starting materials (Ferrite). Whereas ferroelectric phases was prepared by same method, using AR grade BaCO3, 3SrCO3, and TiO2 as starting materials. The mixture was pre- sintered at 800ºC for 10 hours in each case. ME Composites were synthesized by mixing 10 to 40 molar percentage of ferrite phase with 90 to 60 mole percentage of ferroelectric phase respectively. And presintered at 1000℃ for 12 hours. These composites were pressed in to pellets about 1 gram, 2mm in thickness and 1cm in diameter and subjected to final sintering at 1200 ºC for about 15 hours in muffle furnace and then furnace cooled. A detailed Schematic synthesis method for ferrite and ferroelectric phase is shown in Figures 1 & 2.

Figure 1: Schematic Synthesis of Ferrite Phase of sample.
Click to enlarge
Figure 1: Schematic Synthesis of Ferrite Phase of sample.
Figure 2: Schematic Synthesis of Ferroelectric Phase of sample.
Click to enlarge
Figure 2: Schematic Synthesis of Ferroelectric Phase of sample.

Characterization

The presence of crystalline phases and crystal structure of the composites and constituents phases were determined by powder X-Ray Diffraction, using Cu-Kα monochromatic radiation of wavelength 1.5148Å, in a wide range of glancing angle 2θ from 10º to 90º the micrographs of the samples were obtained to study the surface morphology, grain size and microstructure through SEM.

Results and Discussion

X-Ray diffraction patterns of the Ni0.2Cu0.3CO0.5Fe2O4 represented from the Figure 3. X ray diffraction patterns indexing by JCPD data ferrite and ferroelectric exhibits face centered cubic structure and tetragonal structure. The absence of extra line confirms the formation of single phase ferrites the calculated values of interplanar distances and lattice constant are in good agreement with those expected for spinel ferrites. The cyclic sum of miller indices is even number which confirms FCC Structure (Table 1). The same behaviour is observed in the present case. X ray diffraction pattern of Ba0.7Sr0.3TiO3 ferroelectric phase (Figure 4) are indexed with the help of JCPD data. The observed doublet (002) (200); (103) (301); and (113) (311) without additional peaks confirms the formation of tetragonal perovskite structure of ferroelectric phase (Table 2).

Figure 3: X ray diffraction patterns indexing by JCPD data ferrite and ferroelectric exhibits face centered cubic structure and tetragonal structure. The absence of extra line confirms the formation of single phase ferrites the calculated values of interplanar distances and lattice constant are in good agreement with those expected for spinel ferrites. The cyclic sum of miller indices is even number which confirms FCC Structure (Table 1). The same behaviour is observed in the present case. X ray diffraction pattern of Ba0.7Sr0.3TiO3 ferroelectric phase (Figure 4) are indexed with the help of JCPD data. The observed doublet (002) (200); (103) (301); and (113) (311) without additional peaks confirms the formation of tetragonal perovskite structure of ferroelectric phase (Table 2).
Click to enlarge
Figure 3: X ray diffraction patterns indexing by JCPD data ferrite and ferroelectric exhibits face centered cubic structure and tetragonal structure. The absence of extra line confirms the formation of single phase ferrites the calculated values of interplanar distances and lattice constant are in good agreement with those expected for spinel ferrites. The cyclic sum of miller indices is even number which confirms FCC Structure (Table 1). The same behaviour is observed in the present case. X ray diffraction pattern of Ba0.7Sr0.3TiO3 ferroelectric phase (Figure 4) are indexed with the help of JCPD data. The observed doublet (002) (200); (103) (301); and (113) (311) without additional peaks confirms the formation of tetragonal perovskite structure of ferroelectric phase (Table 2).
2ΘΘsin Θhkld (Å)
obs		D (Å)
cal		Lattice Constant
18.44549.22270.16021114.81014.8146a=8.3389Å
30.30815.1540.26142202.94912.9482
35.713817.85690.30663112.51412.5142
37.149718.57480.3 1852222.42022.4072
43.31152,16,5570.3694002.0892.0847
53.905426.95270.45324221.70081.7021
5,74,29928.71490.48045111.60461.6048
74.59837.2990.60596221.27221.2571

Table 1: Lattice constant of Ferrite sample.

Figure 4: XRD pattern of Ba0.7Sr0.3TiO3 ferroelectric phase.
Click to enlarge
Figure 4: XRD pattern of Ba0.7Sr0.3TiO3 ferroelectric phase.
2ΘΘSinΘhkld (Å)
cal		d (Å)
obs		Lattice Parameter
22.2431 1 .12130.192913.996639,968a=3.99463Å c=3.9986Å
(Tetragonality) c/a=1.001
31.67815.83890.27291102.82442.8246
39.03519.51770.33411112.30742.3075
45.48722.74360.38662001.9941.9941
51.18425.59210.4322101.78461.784
57.57428.78720.481521116,0081.6009
66.18733.09350.5462101.41 1 81 .4119
70.70735.35350.57861031 .33231 .3323
75.33937.66940.61113011.02611.2615
79.62339.81160.64022221.2041.204
83.83441.91680.6683201.15391.153

Table 2: Lattice constant of Ferroelectric sample.

The absence of intermediate peaks apart from x[Ni0.2 Cu0.3 CO0.5 Fe2O4] + (1-x) [Ba0.7Sr0.3TiO3] ferrites and ferroelectric phases Figure 5 is attributed to the fact that no chemical reaction have been taken between the constituent phases during final sintering. The peaks exhibit both perovskite (110) and cubic (311) peaks which are the characteristics of ferroelectric and ferrites phase respectively. The lattice parameters in case of composites (Tables 3-6) are almost equal to those of constituents phases. This indicates the absence of structural changes with varyingmolar portions [26, 27]. However the intensity of peaks is found decrease with components. This is due to the capacity of ferrites phase to dissolve in to the spinel lattice [26, 27].The data on patterns is given in tables from 1 to 6. Figures 1&2 exhibit a set of well defined ferric and ferroelectric peaks [26, 27]. The variation of X ray Density , actual density and porosity with doping is shown in Figure 6.

Figure 5: XRD patterns of x[Ni0.2 Cu0.3 CO0.5 Fe2O4] + (1-x)[Ba0.7Sr0.3TiO3] ( x=0.1,0.2,0.3 and 0.4).
Click to enlarge
Figure 5: XRD patterns of x[Ni0.2 Cu0.3 CO0.5 Fe2O4] + (1-x)[Ba0.7Sr0.3TiO3] ( x=0.1,0.2,0.3 and 0.4).
2ΘΘSinΘhkld
cal		Lattice Parameter
22.15611.0780.1922*( 100)4.0111Ferrite phase a=8.3758Å
30.14615.0730.262202.965
31.57415.7870.2721*(101)2.8331Ferroelectric phase
a=8.3758Å c=4.0096Å
35.53517.76750.30523112.5259
38.90119.45050.3329*(111)2.3157(tetragonality) c/a=1.0009
42.62421.3120.36344002.1214
45.24222.6210.3846*(002)2.004
50.97125.48550.43028* (210)1.7916
53.57226.7860.45074221.7105
56.24128.12050.4713*(211)1 .6357
62.73531.36750.52054401.4811
65.96532.98250.5444*(220)1.4161
70.58935.29450.5778* (221)1.3342
75.07737.53850.6093*( 301)1.2652
79.39539.69750.6387*(311)1.2069
83.71341.85650.6673*(222)1.1553
92.36646.1830.72167311.0683
22.32611.1630.194* (100)3.982Ferrite phase
a=8.3638Å
30.23 115.1160.261*(220)2.956
45.61622.8080.388* ( 002)1.989Ferroelectric phase
a=8.39796Å c=3.9809Å
51.36225.6810.433* (210)1.779
56.71728.3590.475* (211)1.623
62.88831.4440.5224401.478
66.0533.0250.545* (220)1.415(tetragonality)
c/a=1.0003
71.09935.550.581* (221)1.326
75.63837.8190.613* (301)1.257
79.41239.7060.639* (311)1.207
84.37642.1880.672* (222)1.148
93.06346.5320.726*(731)1.062

Table 3: Lattice parameter of 0.1[Ni0.2 Cu0.3 CO0.5 Fe2O4] + 0.9 [Ba0.7Sr0.3TiO3].

2ΘΘSinΘhkld
cal		Lattice Parameter
22.1411.070.192* (100)4.0172Ferrite phase
a=8.3747Å
30.1815.090.26* (220)2.9616
31.5415.770.272*(106 )2.8363Ferroelectric phase
a=4.0103Å c=4.0128Å
35.5517.7760,3053* (311)2.5251
38.919.4510.333*(111)2.3157
43.2221.610.368* (400)2.0931
45.3122.6650.385* (002)2.0013(tetragonality)
c/a=1.0006
50.9425.4690.43*(210)1.7928
53.6426.820.451*(422)1.7086
56.2228.1 120.471*(211)1.636
62.831.4020.521*(440)1.4797
66.0233.0080.545*(220)1 .4150
70.535.2520.577*(221)1.3356
75.337.6490.611*(301)1.2621
79.5739.7830.64*(31 1)1.2047
83.741.8480.667*(222)1.1557
92.246.0980.721*(731)1.0699
2ΘΘSinΘhkld
cal		Lattice parameter
22.1911.0950.192*(100)4.007Ferrite phase
a=8.3775Å
30.1615.0820.26*(200)2.963
31.5715.7870.272* (111)2.833Ferroelectric phase
a=4.007Å c=4.009Å
35.5417.7680.305*(311)2.526
38.9419.4680.333*(111)2.313
43.221.6010.368*(400)2.094(tetragonality)
c/a=1.0005
45.2622.6290.385* (002)2.003
51.0125.5030.431* (210)1.79
53.6226.8120.451*(422)1.709
56.2628.1290.472*(211)1.635
62.8231.410.521*(440)1.479
65.932.9490.544*(220)1.417
75.2637.6320.611* (301)1.263
79.2439.6210.638* (311)1.209
92.446.20.722*(731)1.068

Table 4: Lattice parameter of 0.3[Ni0.2 Cu0.3 CO0.5 Fe2O4] + 0.7 [Ba0.7Sr0.3TiO3].

Figure 6: X-ray Density and Porosity of x[Ni0.2Cu0.3Co0.5Fe2O4] + (1-x)[Ba0.7Sr0.3TiO3] Composites.
Click to enlarge
Figure 6: X-ray Density and Porosity of x[Ni0.2Cu0.3Co0.5Fe2O4] + (1-x)[Ba0.7Sr0.3TiO3] Composites.

SEM analysis

Scanning Electron Microscopy (SEM) is a powerful imaging technique that provides high-resolution, three- dimensional images of the surface morphology of ferrites & ferroelectric samples. The average grain size was estimated by Cotrell’s method [28], which lies in between 0.8 µm to 2.0 µm and decrease with increase in mole percentage of ferrites phase (Figure 7) and cause for the decrease of mean free path of electrons. The porosity is an inherent phase associated with the samples prepared by ceramic method. Porosity is a crucial aspect of materials prepared by ceramic methods, and it plays a significant role in influencing the properties and applications of these materials In the present case porosity in composites varies from 20 to 30 percent (Figure 6). The grain growth in the ME composite is assigned to the presence of inclusions and pores in the solid solution which migrate to the grain boundary. The grain growth in the ME Composite depends on the particle size of individual phases and their distribution , homogeneity of chemical composition and sintering conditions [26, 27, 28]. Increase in ferrite phase decrease the porosity and hence decrease the grain size. This leads to decrease in magnetization of the ME composites.

Because, of large grain and less effective in inducing ferrite and ferroelectric coefficients rather than smaller ones [26, 27, 28].

Figure 7
Click to enlarge
Figure 7

Conclusions

A simple and cost-effective solid-state technique was employed to synthesize both ferrite & ferroelectric samples. Phase of Ferrite sample cubic, Ferroelectric as tetragonal and further composites were analyzed through XRD analysis. The study focused on investigating variation of structural properties of x[Ni0.2Cu0.3Co0.5Fe2O4] + (1-x)[Ba0.7Sr0.3TiO3] Composites. The presence of cubic phase of [Ni0.2Cu0.3CO0.5 Fe2O4], ferroelectric phase (tetragonal) [Ba0.7Sr0.3TiO3], were confirmed by X-Ray Diffraction analysis and SEMaverage grain diameter lies in the range of 0.5µm to 2 µm.

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@article{mathad2024,
  title   = {Tailored Synergy: Synthesis and In-Depth Structural Analysis of
x[Ni0.2Cu0.3Co0.5Fe2O4] + (1-x)[Ba0.7Sr0.3TiO3] Composites},
  author  = {Mathad SN},
  journal = {Nanomedicine & Nanotechnology Open Access},
  year    = {2024},
  volume  = {9},
  number  = {1},
  doi     = {10.23880/nnoa-16000293}
}
Mathad SN (2024). Tailored Synergy: Synthesis and In-Depth Structural Analysis of
x[Ni0.2Cu0.3Co0.5Fe2O4] + (1-x)[Ba0.7Sr0.3TiO3] Composites. Nanomedicine & Nanotechnology Open Access, 9(1). https://doi.org/10.23880/nnoa-16000293
TY  - JOUR
TI  - Tailored Synergy: Synthesis and In-Depth Structural Analysis of
x[Ni0.2Cu0.3Co0.5Fe2O4] + (1-x)[Ba0.7Sr0.3TiO3] Composites
AU  - Mathad SN
JO  - Nanomedicine & Nanotechnology Open Access
PY  - 2024
VL  - 9
IS  - 1
DO  - 10.23880/nnoa-16000293
ER  -