Synthesis and characterization of non-molar lithium–magnesium nanoferrite material for its applications


Non-stoichiometric ferrite magnetic nanoparticles Mg0.5+xLi1−2xFe2O4 (x = 0, 0.15, 0.35) were prepared using low-cost sol–gel method and annealed at temperature 700 °C. Thermal analysis measurement confirms that there is a decrease in weight with an increase in temperature which becomes thermally stable till 600 °C. The XRD study confirms that prepared nanoparticles are a cubic spinel structure having Fd3m space group. The crystallite size lies in the range of 26.41–31 nm. Lattice parameter was found to increase with decreasing molar ratio of Li ion. The FTIR spectroscopy confirms the spinel nature of ferrite nanomaterial having characteristics absorption peaks at 588 and 435 cm−1. HRTEM and SEM image confirms the cubic spinel structure and porosity in the material. The indirect energy band gap was evaluated for all samples using tauc plot and found to be 2.25, 1.89 and 2.03 eV respectively for x = 0, 0.15 and 0.35. The energy band gap was found function of crystallite size. Strong luminescence was observed in the visible range of 580–610 nm. The non-molar ratio of Li = 0, 0.15 and 0.35 mol leads to a systematic increase in all the magnetic parameters. The magnetization increases from 15.53 to 33.75 emu/g, retentivity from 2.66 to 7.11 emu/g and coercivity increases 116.56–161.37 Gauss, respectively. Prepared nanomaterial possesses pure phase porous crystal with luminescent property in the visible range, energy band gap in the range of 2.03–2.25 eV and uniform increase in the magnetic parameter. Hence, materials may be potential candidate for magneto-optical device, humidity sensor, hydroelectric cell applications and some other realted fields.


Ferrite magnetic materials have a wide selection of applications due to supported their structural, magnetic and optical behaviors. In recent years, soft magnetic materials became exciting for applications in microwave devices, top-quality filters, head of digital tapes, high upgrade sensors because of their magnetic behavior, nanometric size and high resistivity [1,2,3]. Substituted ferrites, which results in tuned structural, magnetic and optical properties parameters have inclined researchers to shift their research interest [4,5,6,7,8]. Llithium and substituted ferrites materials are found promising for microwave applications together with some other areas of science and technology. This may be a substitute for replacements for garnets materials, due to their low cost of production and tuned properties [9,10,11,12,13,14,15,16,17]. In this present research, we use low-cost chemical-based citrate precursor method to prepare non-molar Li substituted ferrite materials. Recent advances have also shown that it can be used in the dissociation of the water molecule and photocatalytic application. Thus, it has led to a shift and influence researcher to extract more advances in properties with substitution of alkali metal [9]. Besides, studying on pure lithium ferrite Mg, Ni, Zn, Co, Ti, Cd, Cr, Ce, etc., substituted ferrite have also been reported by other research groups [10,11,12,13,14,15,16,17,18,19,20,21,22,23,24]. In this present work, our main objective was to investigate the effect of non-stoichiometric substitution of lithium on structural, magnetic and optical properties of magnesium ferrite, which were annealed at single temperature 700 °C. Some research groups have prepared spinel based ferrite below 700 °C and found possible uses in various areas of science and technology due to its some technical parameters [11]. Since very limited scientific reports are available on the effect of non-stoichiometric in structural parameter and optical properties of Li substituted ferrite materials prepared at around 700 °C by low-cost chemical method. Different methods such as the co-precipitation technique, the sol–gel, microemulsion, the hydrothermal, the polymer pyrolysis, the citrate precursor, microwave-refluxing techniques have been used for the synthesis of spinel ferrites. [15,16,17,18,19,20,21,22,23,24]. The properties of these ferrite materials are influenced by the composition, microstructure and annealing temperature. In this present work, our main objective is to prepare Li substituted non-molar Mg0.5+xLi1−2xFe2O4 nanomaterial annealed at temperature 700 °C and measure their structural, optical and magnetic behavior as functional nanomaterials for its applications.

Materials and methods

Non-stoichiometric ferrite magnetic nanoparticles Mg0.5+xLi1−2xFe2O4 (0 ≤ x ≤ 0.35) synthesized using citrate precursor sol–gel route. Analytical pure grade LiNO3.xH2O (Alfa Aesar), Mg(NO3)2.6H2O (Merck), Fe(NO2)3.9H2O (Merck), and citric acid all chemicals have assay greater than 99% were used. The aqueous solutions of metal nitrates were used in their respective non-stoichiometric ratio. Citric acid was dissolved in deionized water as a chelating agent for obtaining a homogenous, steady and transparent solution. The dissolved solution was mixed homogenously using a magnetic stirrer. The drop-wise ammonia solution was added (35% Assay Merck) and the pH of the sample was maintained at ‘7′. After shifting the pH of the sample to 7, the synthesis temperature was maintained at 80 °C for about 4 h with continuous stirring, till a viscous gel is obtained. The gel was kept in a oven for drying. Finally, a light airy mass of brittle flakes like powder is obtained and is annealed at 700 °C for 3 h. The prepared materials were characterized using TGA-DTA (Netzsh), XRD( Bruker D8 Advance), SEM (Carl Zeiss), HRTEM, UV–Vis spectrometer (Perkin-Elmer Scan Lambda 950), photoluminescence spectrometer (Perkin-Elmer LS55), vibrating sample magnetometer (Lakeshore, 7400). The flowchart of the synthesis of materials is shown in Fig. 1.

Fig. 1

Flowchart for ferrite nanoparticles synthesis

Result and discussion

TGA–DTA measurement

TGA-DTA measurement of Mg 0.5LiFe2O4 is being shown in Fig. 2. The TG study shows that first weight loss occurs in the range of 42–127 °C (11.76%) and this weight loss might be attributed to the loss of the water molecule of the precursor. The second weight loss was observed at 160–332 °C and it is about 4% that is maybe due the presence of organic matter. Moreover, a turning point was observed which might be accredited to the phase formation as third weight loss of 28.29% in the range of 333–530 °C and this reveals that presence of impurity remaining in the components like nitrates, water vapor, etc., in the prepared ferrite nanomaterials. It has been observed that after 500 °C there is no significant weight loss till 600 °C, indicating that the nanomaterial sample is stable after 500 °C. The presence of metal impurities was also revealed by DTA measurement and a sharp exothermic peak was observed at 351 °C. Thus, based on the result obtained by TGA-DTA, we planned that 700 °C is suitable for annealing so that functional properties can be obtained for varied applications [25, 26].


TGA–DTA curve for Mg0.5LiFe2O4

XRD measurement

The X-ray diffraction pattern(XRD) for the composition of Mg0.5+xLi1−2xFe2O4 (0 ≤ x ≤ 0.35) is shown in Fig. 3. The prepared annealed powder was analyzed at an angle varying from 20 to 70 °C and found six prominent peaks with hkl (220), (311), (222), (400), (422), (511) and (440), respectively.The planes (311), (400), (511), (440) show elemental reflections having prominent intensity. The other reflection peaks (422,220) are, however, noticed to be weak in intensities compared to others. These reflection peaks confirm the cubic spinal structure having no impurity intermediate peaks. Thus, the present studies reveal that the low-cost citrate method of preparation of pure spinel phase of non-stoichiometric Li substituted ferrite materials can be important for numerous applications. The lattice constant, cell volume, X-ray density and d-spacing are also calculated for the prominent peak (311) which are shown in Table 1.

Fig. 3

XRD result for Mg0.5+xLi1−2xFe2O4 (0 ≤ x ≤ 0.35) annealed at 700 °C

Table 1 Structural parameter

The formulae for calculation of lattice constant for cubic spinal phase are as follows:

$$\frac{1}{{d^{2} }} = \frac{{h^{2} + k^{2} + l^{2} }}{{a^{2} }}$$

The interplanner d-spacing was evaluated by Bragg’s law equation,

$$\lambda \, = \,{\text{2d}}_{{{\text{hkl}}}} {\text{sin}}_{{{\text{hkl}}}} \theta$$

and the density of X-ray (dx) is evaluated using the relation.

$${\text{X - raydensity}} = \frac{8M}{{Na^{3} }}$$

X-ray density = (3)

where ‘M’ is molecular weight of the sample, ‘N’ is the Avogadro number, ‘a’ is the lattice parameter. And, the volume of unit cell is calculated using

$$v\, = \,{\text{a}}^{{3}}$$

Structural parameters are depend on the ionic radii of Li1+, which is bigger in comparison of Mg+2 ion (since the ionic radius of Li is 0.76 Å and Mg is 0.72 Å). It is clear that as the molar ratio of Li1+ ion substitution is decreased and of Mg+2 is increased resulting in systematic increment in lattice constant, cell volume and X-ray density, which are shown in Fig. 4 and Table 1. Due to the shift in the major peak position (311), angular position, which occurs due to the replacement of smaller ionic radius by larger ionic radius. This may causes stretching the bond length (Fig. 5). This also results in change in the lattice parameter, which is due to increase in unit cell volume and depicted in Fig. 4 and Table 1. Thus, with the decrement in Li content, the lattice parameter is increased. This led to increase in the X-ray density of the materials in the present research and this might be due to the increase in molar mass and volume of unit cell with the decrement in Li content. This ultimately leads to increment of Mg content in the sample and similar reports are also reported by G. Arvind et al. [27]. The shift in prominent peak Bragg’s angle (311) is shown in Fig. 5, clearly indicates that there is an increase in lattice parameter with decrease in Li+1. The more details on structural studies were also reported using Williamson hall plot for calculation of crystallite size and strain produced in the materials due non-stoichiometric substitution of Li ion and Mg2+ ion and which are shown in Fig. 6(a–c) and Table 2, respectively.


ac variation in lattice parameter, b variation in unit cell volume and c variation in X-ray density of Mg0.5+xLi1-2xFe2O4 (0 ≤ x ≤ 0.35)

Fig. 5

Shift toward lower angle in prominent peak Bragg’s angle (311)

Fig. 6

ac W–H plots of Mg0.5+xLi1−2xFe2O4 (X = 0, 0.15 and 0.35). a W–H plot of Mg0.5LiFe2O4 b W–H plot of Mg0.65Li0.3Fe2O4 c W–H plot of Mg0.85Li0.7Fe2O4

Table 2 Crystalline size and lattice strain

W–H plot analysis

W–H analysis method was developed by G.K Williamson, W.H Hall and his student, which is represented by.

$$\beta_{{{\text{hkl}}}} = \left[ {\frac{{{\mathbf{k}}\lambda }}{{\mathbf{D}}}} \right]\, + \,{4}\varepsilon {\text{sin}}\theta$$

and compared to standard equation, y = mx + c. In this equation, λ is the wavelength of the incident X-ray radiation (0.15406 nm), θ is Bragg’s angle of diffraction, D is the crystallite size, and β is (FWHM) full width at half maximum. The expression (4εSin θ)gives us the strain effect and the intercept (Kλ\D) on the axis (Βcosθ) helps us to calculate the crystallite size of the nanomaterial. The W–H plots for three samples Mg0.5LiFe2O4, Mg0.65Li0.7Fe2O4 and Mg0.85Li0.7Fe2O4 are shown in Fig. 6(a–c).The obtained plots are fitted linearly. The intercepts on y-axis help us to evaluate the crystallite size value, whereas the value of lattice strain is evaluated using the slope of the straight line. Table 2 contains the values of crystallite size and strain produces in the lattices. It is clearly observed that lattice strain increases with the increase in the Li1+ concentration. It may be due to larger atomic radii of Li1+ ions as compared to Mg2+ ions. The crystallite was found to increase with the increase in Li1+ ion as the strain value is increased. As large ionic size hinders the growth due to strain produces in the crystal. But, it is found that in Mg0.85Li0.3Fe2O4 crystallite size was found to increases and this might be because of the presence of α-Fe2O3 at angular position 32.4°, but the peak intensity is very small. Some research groups have also found similar type of finding [28].

Morphology and size investigation using SEM and HRTEM

The SEM images for Mg0.5LiFe2O4, Mg0.65Li0.7Fe2O4 and Mg0.85Li0.3Fe2O4 are shown in Fig. 7(a–c). The agglomerated micron size of nanocrystalline particles is well observed. The surface morphology can easily be seen of the sample Mg0.5LiFe2O4, which shows cubic structure and also have porous structure of different pore sizes. HRTEM measurement of the prepared nanomaterial further support the SEM measurement. The prepared materials may be a potential candidate for hydroelectric cell due to porous structure of monovalent Li ions substitution[29]. Small strain in crystal, particle–particle interaction may cause small agglomerations. It was found that almost uniform grain size and porous structure are obtained with substituted Li ion of non-stoichiometric ratio nanomaterials. The porosity is found to depend on composition of Li ion and Mg ion in the materials. Further for actual particle size determination, HRTEM image is shown in Fig. 8(a–d). The HRTEM measurement shows the cuboid structure nanomaterials, which also confirms our structural analysis shown in Fd3m cubic structure, shown in SAED (selected area electron diffraction). The crystal structure having consist of five concentric rings from which correspond the acentric hkl value in the materials, i.e., (220), (311), (400), (511) and (440). The bright spot in the SAED pattern confirms the poly nanocrystalline nature.

Fig. 7

ac Surface morphology for a Mg0.5LiFe2O4 b Mg0.65Li0.7Fe2O4 and c Mg0.85Li0.3Fe2O4. a SEM images of Mg0.5LiFe2O4 at different magnifications. b SEM images of Mg0.65Li0.7Fe2O4 at different magnification. c SEM images of Mg0.85Li0.3Fe2O4 at different magnifications

Fig. 8

a–d HRTEM image of Mg0.5LiFe2O4 ferrite magnetic

EDAX measurement

Further for elemental analysis of sample Mg0.65Li0.7Fe2O4, their EDAX measurements were reported in Fig. 9b, while EDS spectra of the same material is shown in Fig. 9a and it shows that there is no impurity peak in the prepared material having elements like Mg, Fe and O, whose concentration is shown in the EDAX measurement. Lithium is not detected by the EDS detector due to its small atomic radius and lighter element. Thus, EDS measurement reveals that the prepared compound is made of Mg, Fe and O.

Fig. 9

a EDS spectra of samples Mg0.65Li0.7Fe2O4 b elemental analysis of EDS spectra of sample Mg0.65Li0.7Fe2O4 at different sites as shown in the spectra 20

FTIR measurement

The Fourier transform infrared spectroscopy(FTIR) of non-molar lithium/magnesium ferrite is shown in Fig. 10, in the range of 800–400 cm−1.There are two characteristics of absorption bands common to all the spinel ferrites. The absorption band denoted by v1 shows high frequency in the range of (580–600 cm−1), whereas v2 denotes the low frequency range of (400–436 cm−1). This may be mostly due to the tetrahedral-octahedral site vibration common in cubic spinel ferrites nanomaterials [29, 30]. The absorption peak at 435 cm−1 generally occurred for octahedral region. It was found that its intensity increases with increment in Li1+ atom and slightly shifted as well as a result of lithium ions get distributed in octahedral sites. The remaining band lying at 580 cm−1 might be due to (Mg2+-O2) and (Fe3+-O2) interaction resulted as the presence of octahedral-tetrahedral sites in the nanomaterial, which leads to the formation of cubic spinal structure [31] (Fig. 11).


FTIR of Mg0.5+xLi1−2xFe2O4 (0 ≤ x ≤ 0.35)


UV spectra of Mg0.5+xLi1−2xFe2O4 (0 ≤ x ≤ 0.35)

Optical properties

UV–Vis measurement

The ensuing spectrums and Tauc plots obtained by UV visible spectrometer (Perkin Scan Lambda 950) are shown in Fig. 12(a–f)., while Uv-Visible spectra is shown in Fig.11. Samples were characterized in the range of 200–1000 nm at room temperature. The effect of substitution of Li atom (alkali metal) in magnesium is being studied. The spectrum shows that maximum absorption occurred in UV region of at around 235 nm. Similar finding was also reported by some research group [32]. This study shows the prepared material may be suitable for blocking UV radiation. The direct and indirect energy band gap was evaluated to analyze the effect of non-molar ratio of lithium ion and Mg ion [33, 34]. The equation used for energy band gap calculation by Tauc plot is given by [35]

$${\text{Eg}}\, = \,\frac{hc}{\lambda }$$

a–f Tauc plot of Mg0.5+xLi1−2xFe2O4( 0 ≤ x ≤ 0.35.) for direct and indirect band gap measurement

And, the symbols have usual meaning. The direct band gap and indirect band gap were calculated using equation,

$$\alpha hv = (hv - Eg)^{n}$$

where ‘h’ is Planks constant, ‘c’ is speed of light and ‘λ’ is wavelength ‘n’ = ½ and 2 for direct and indirect energy band.

The effect of non-molar Li/ Mg ferrite is being studied for optical properties of Mg0.5+xLi1−2xFe2O4 (where, 0 ≤ x ≤ 0.35). Since it is an important factor in determining electrical conductivity, as it is the energy required to jump a valence electron from valance band to conduction band and further behave as a charge carrier. It is extracted by using Tauc plot and extrapolating the linear portion. The data for optical direct and indirect energy band gap are being listed in Table 3. The band gap numerical value shows that there is a systematic decrement in direct optical energy band gap with the decrement of Li1+ ion (1.578–1.528 eV). The reduction in band gap may be due to weakening electrostatic interaction among different molar ratio of Li ion and Mg ion concentration. The indirect band gap was also evaluated and it also shows similar trend, i.e., decrease in band gap with decrement in Li mole concentration and crystallite size. It can be expressed easily by the help of Bra’s effective mass model which gives us the relation between band gap and particle size as shown in following equation [36, 37]

$$E_{g}^{*} \cong ~E_{g}^{{{\text{bulk}}}} + \frac{{h^{2} \Pi ^{2} }}{{2er^{2} }}\left( {\frac{1}{{m_{e} }} + \frac{1}{m}_{h} } \right) - \frac{{1.8e^{2} }}{{4\pi \varepsilon \varepsilon _{0} }}$$
Table 3 Direct and indirect band gap energy

Here, \({E}_{g}^{bulk}\)= bulk energy band gap, r = particle size \({m}_{e}\)= effective mass of electron, \({m}_{h}\)= holes effective mass, ε = relative permittivity ε0 = permittivityof free space, h = Planck’s constant divided by 2\(\pi\) and e = charge on an electron. Energy band gap depends on the motion of an electron in nanocrystal. At nanoscale, motion of an electron in ferrite is affected by super exchange interaction and crystalline size. In this present research, crystalline size found function of energy band gap. Generally, energy band gap in range 1.05–1.70 eV semiconductor materials is useful photovoltaic solar cell. Therefore, prepared materials may be treated as functional nanomaterials for varied applications.

Photoluminescence measurement

The Fig. 13 shows photoluminescence (PL) spectra at room temperature of non-molar Mg0.5+xLi1−2xFe2O4 (x = 0, 0.15 and 0.35), obtained in the region of (500–700) nm wavelength range, using excitation of 300 nm source of radiation. It is observed that non-molar magnesium–lithium ferrite exhibits luminous property as intense intensity peaks lie in orange range (580–610 nm). It is observed that intensity is proportional to concentration of lithium ion and it is minimum for Mg0.5LiFe2O4 and increases regularly with substitution of Li1+ ions. Oxygen deficiency might also be a reason for such luminiscence, which may also resulted due to the porosity in the material. Similar work is also onserved by some research group[38].

Fig. 13

Photoluminescence spectra of non-molar substituted Mg–Li ferrite

Magnetic measurement

Magnetic properties were calculated using Lakeshore-7400 vibrating sample magnetometer, at room temperature, varied (− 20 k Oe to + 20 k Oe) range of magnetic field and as shown in Fig. 14. It is evident that increase in applied force leads to increment in magnetization, until at magnetic field (+ 20 k), where it saturates [39]. Soft materials properties were experienced as narrow loops were found and the value of Mr/Ms which is known as squareness ratio lies in the range of 0 to 1. This shows magnetostatic interaction. Other research group works have suggested that Li1+ will occupy tetrahedral resulting into decrement in magnetic moment (MA) [40,41,42]. It further leads to affect the octahedral and tetrahedral structure in (A–B) site and saturation magnetization will proceed to increase [43]. Recent research shows that at higher concentration of Li1+ it results to accumulate at octahedral site resulting in decline of saturation magnetization, which is opposite to the stoichiometric ratio studies. Table 4 shows that the lowest magnetization value was reported for sample (Mg0.5LiFe2O4) is 15.53 emu/g having one mole lithium ion concentration, but with the decrement of Li1+ ion, the magnetization increment was found from 15.53 to 33.75 emu/g for Mg0.85Li0.3Fe2O4 having 0.3 mol lithium ion concentration [44]. Coercivity value for the materials was found to increases with decrement in Li ion concentration from 116.56 Gauss for Mg0.5LiFe2O4 to 143.25 Gauss in Mg0.65Li0.7Fe2O4 and increased further to 161.37 Gauss for Mg0.85Li0.3Fe2O4. Thus, non-molar ratio of Li = 0, 0.15 and 0.35 leads to increase all the magnetic parameters, e.g., magnetization, retentivity and coercivity with decrease in Li ion concentration. This may be the interesting observations of prepared materials having annealed at single temperature 700 °C. Such changes may be due change in supercharge interaction forces. Generally, in spinel ferrite, divalent and trivalent ion super exchange interaction plays a vital role for magnetism. But in this present study, monovalent ion Li is substitute of divalent ion. Such combination may responsible for such systematic variation in magnetic behavior. Thus, prepared monovalent substituted non-molar ration ferrite possesses porous structure of soft nature of magnetism with optical absorption in UV region, energy band gap of semiconductor nature, luminescence peaks in visible region. Hence, the prepared materials may be useful as functional materials in hydroelectric cell, optoelectronics devices, humidity sensors and some another field. Similar magnetism and optical energy band gap with different numerical values of the same materials were reported, which was annealed at temperature 550 °C [38].


Magnetization applied field plot

Table 4 Magnetic measurements

Thus, present research open a new window of non-stoichiometric substituation by monovalent Li substituted ferrite as opportunity to mass production of functional magnetic materials using low-cost chemical method for various applications. The substituted ferrite magnetic nanomaterials found as functional nanomaterials for its applications [45,46,47].


Non-stoichiometric Mg0.5+xLi1-2xFe2O4 (x = 0,0.15 and 0.35) nanoferrites having crystallite sizes, 30, 26 and 31 nm, prepared using low-cost citrate precursor method, annealed at 700 °C for 3 h. Thermal analysis confirms that annealing after 600 °C would be ideal for single phase formation as there was no significant weight loss in range of 530–600 °C. The XRD study shows that there is an increment in structural parameters like lattice constant, unit cell volume and X-ray density with the decrease in Li concentration due to its large ionic radius of Li1+ ion than Mg+2 ion. The FTIR study confirms the formation of cubic spinel structure having space group \(Fd\stackrel{-}{3}m\). A slight decrement in direct band gap was observed due to decrement in lithium ion from (1.578 eV), (1.547 eV) and (1.528 eV) and indirect band gap as well from 2.25 to 1.89 eV. The reduction in band gap is function of crystalline size. Luminescence peaks were obtained in visible range. Magnetic measurement shows increase in all magnetic parameters with increases in Li ion concentration, e.g., magnetization increases 15.53 to 33.75 emu/g, receptivity, from 2.66 to 7.11 emu/g and coercivity 116.56–161.37 Gauss respectively. Thus, prepared monovalent substituted ferrite possesses soft magnetic nature, porous like morphology with optical absorption in UV region, energy band gap of semiconductor behavior and strong luminescence in visible region. Hence, the prepared materials may be useful in hydroelectric cell, humidity sensor, magneto-optical devices with some another field. Thus, present study open a new window of non-stoichiometric compositions as opportunity to mass production of functional magnetic materials using low-cost chemical method for various industrial applications.


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Authors are thankful to TEQUIP-III of Aryabhatta Knowledge University, Patna for financial support under Collaborative Research Scheme (Ref-005/Exam/1060/AKU/2019/4455). Authors are also grateful to Department. of Education, Govt. of Bihar and Aryabhatta Knowledge University, Patna which has been very supportive in establishment and functioning of the Aryabhatta Center for Nanoscience and Nanotechnology, Aryabhatta Knowledge University, Patna, Bihar, India.

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Singh, R.K., Kumar, N. & Rangappa, D. Synthesis and characterization of non-molar lithium–magnesium nanoferrite material for its applications. Appl. Phys. A 127, 183 (2021).

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  • Ferrite
  • Nanoparticle
  • Non-molar
  • Li ion
  • Magnetism
  • Optical behavior