4.1 A simple and effective method of the synthesis of nanosized …shodhganga.inflibnet.ac.in/bitstream/10603/19192/9/09_chapter4.pdf · materials and their magnetic properties have

CHAPTER4 SYNTHESIS AND CHARACTERISATION OF NANOSIZED FERRITES (RESULTS AND DISCUSSION)

162

4.1 A simple and effective method of the synthesis of nanosized ZnFe2O4 particles

Spinel ferrites are magnetic materials and have wide applications in magnetic devices and

switching devices [1-3]. Zinc ferrite (ZnFe2O4) is of interest as it has wide applications in not

only to basic research in magnetism, but also has great potential in technological application,

such as magnetic materials [4–10], gas sensors [11], catalysts [12], photocatalysts [13], and

absorbent materials [14–18]. Different methods have been reported for the synthesis of

ZnFe2O4. The zinc-doped maghemite nanoparticles were prepared using ultrasonic radiation

[19]. Zn/Fe oxide composite nanoparticles were synthesized by basic hydrolysis of Fe2+ and

Zn2+ ions in aqueous continuous phase containing gelatin. The obtained composite

nanoparticles were composed of iron oxide, zinc oxide and zinc ferrite phases [20]. The

antibacterial activity of these nanoparticles was tested against Staphylococcus aureus and

Escherichia coli. Ordered ZnFe2O4 nanotube arrays with the average outer diameter of 100

nm were prepared in porous anodic aluminum oxide template using an improved sol-gel

approach [21]. Crystallographically oriented magnetic ZnFe2O4 nanoparticles have been

synthesized by Fe implantation into ZnO and their super paramagnetic behavior has been

studied [22]. Mixed oxide ZnO-Fe2O3 has been synthesized by improved sol gel synthesis

and their photocatalytic behavior has been studied by photocatalytic degradation of potassium

cyanide in aqueous dissolution. Ferromagnetic zinc ferrite nanocrystals at ambient

temperature were synthesized via the thermal decomposition of metal-surfactant complexes

[23]. Nanometer-sized zinc ferrite particles capped with a layer of surfactant has been

synthesized [24]. The effect of the surfactant capping on the grain growth of the zinc ferrite

nanoparticles was investigated. The surfactant capping effectively inhibited grain growth, and

it was observed that the zinc ferrite nanoparticles with a capping layer could readily be

dispersed in some organic media due to their surface modification. Nanostructured

semiconductor thin films of Zn-Fe2O3 modified with underlying layer of Fe-TiO2 have been

synthesized and studied as photoelectrode in photoelectrochemical (PEC) cell for generation

of hydrogen through water splitting [25]. Zinc ferrite (ZnFe2O4) photocatalysts with different

crystallite sizes have been prepared using the colloid mill and hydrothermal technique and

have been applied to photodecompose acid orange II azodye molecule under UV irradiation

[26]. Co(1−x)ZnxFe2O4 and Mn(1−x)ZnxFe2O4 (x=0.1–0.5) nanoparticles are prepared by

chemical co-precipitation method and their applications for the synthesis of ferrofluids have

been discussed [27]. Nanostructured zinc ferrite has been prepared by mechanical milling and

change in magnetic behavior with change in size has been discussed [28]. In the present

work, synthesis of ZnFe2O4 nanoparticles has been reported by simple aqueous precipitation


163

method by taking ammonia as precipitating agent. This method involves a simple, cheap and

one step process for synthesis of ZnFe2O4 nanaoparticles as compared to other methods of

synthesis like ultrasonic radiation, sol-gel approach, thermal decomposition of metal-

surfactant complexes, colloid mill, mechanical milling etc. The obtained particles of ZnFe2O4

have size from 10-30 nm. The synthesized nanoparticles were characterized by

XRD,TGA/DTA, Magnetic susceptibility, SEM and TEM.

4.1.1. Results and discussions:

X-ray studies:

X-ray diffraction of synthesized ZnFe2O4 is shown in Figure (4.1). X-ray diffraction pattern

of ZnFe2O4 pure indicated that zinc ferrite is in the form of ZnFe2O4. In X-ray diffraction,

some prominent peaks were considered and corresponding d-values were compared with the

standard i.e. JCPDS file No. 82-1049 (Table-4.1). X-ray diffraction shows that metal oxide is

pure ZnFe2O4 having spinel structure. Thickness of the crystals has been calculated using

Scherrer’s formula and it also support the TEM observations.

Magnetic measurements:

The magnetic measurement of ZnFe2O4 was carried out at room temperature and it has been

observed that ZnFe2O4 shows super paramagnetic behavior at room temperature (300 K) with

saturation magnetization (Ms) value 50 (Fig.4.2). Previously reported values of Ms for zinc

ferrite nanoparticles prepared by various methods has been reported in Table 4.2. The value

of Ms ranging from 12-88 emug-1 shows that Ms strongly depends on the synthesis method

used. This Ms value at room temperature is good and comparable with methods of synthesis

as thermal decomposition method (Ms value 42 at 300K and Ms value 65.4 emug-1 at 10K),

ball milling (Ms value 20.7 in at 4.2K) and other co-precipitation routes which shows a

maximum Ms 46.9 at 4.2 K [Table 4.2].

TGA/DTA

Thermal analysis involves thermogravity (TG), differential thermal analysis (DTA) and

derivative Thermogravimetry (DTG). Thermal gravimetric studies of the calcined oxides

prepared were done between a temperature range of 10-10000C under N2 atmosphere. The

TGA/DTA curves of the zinc ferrite are shown in Fig. (4.3). The maximum total weight loss

observed for zinc ferrite and their corresponding temperature is summarized in Table (4.3).

Results showed that in the synthesized oxides shows some weight loss and oxide undergoing

decomposition, dehydration or any physical change. In DTA curve also, there is exothermic

and endothermic peak which shows phase transition, solid state reach on any chemical

reaction occurred during heating treatment.


164

SEM/ TEM studies

Morphology of the sample was investigated by using SEM and TEM. Morphology of the

sample is shown by the SEM micrographs (Figure-4.4).TEM studies were carried to find out

exact particle size of synthesized ZnFe2O4. Figure 4.5 shows the TEM image of the

synthesized ZnFe2O4 nanoparticles. It shows that the size of the obtained nanaoparticles is in

the range of 10-30 nm. Most of the particles are in the range of 20-30 nm. TEM images

indicate that ZnFe2O4 samples were all spherical particles with uniform grain size distribution.

4.1.2 Abstract:

ZnFe2O4 nanoparticles with spinel structure are synthesized successfully by aqueous

precipitation method. From TEM study it is found that particles are having average size of

10-30 nm. Magnetic measurements show that ZnFe2O4 is super paramagnetic in nature

having saturation magnetization (Ms) value 50 emu/g. This method is advantageous over

existing methods of synthesis of nanoparticles because other methods require specialized

instrumentation, highly skilled labour, expensive materials and methods. Therefore, the

proposed precipitation method is very promising, easy and cheap and may have extensive

applications.


165

4.2 A simple and effective method of the synthesis of single phase nanosized NiFe2O4

particles

Spinel ferrites are magnetic materials and have wide applications in magnetic devices and

switching devices [29-31]. Nickel ferrite (NiFe2O4) is of interest as it has wide applications in

RF/ microwave because of its high Neel temperature, low microwave loss, low magnetic

anisotropy [32-36]. Nanosized nickel ferrite possesses attractive properties for the application

as soft magnets, core materials in power transformers and low loss materials at high

frequencies [37]. Nickel ferrites are technologically important material. Nickel ferrite has

inverse spinel structure. The crystal structure is face centered cubic with the unit cell

containing 32 O2–, 8 Ni2+ and 16 Fe3+ ions. The oxygen ions form 64 tetrahedral and 32

octahedral sites, where 24 cations are distributed. The eight Ni2+ and eight Fe3+ cations

occupy half of the octahedral sites and the other eight Fe3+ ions occupy eight tetrahedral sites

[38-39]. Ferrimagnetic property of the material arises from magnetic moments of anti-parallel

spins between Fe3+ ions at tetrahedral sites and Ni2+ and Fe3+ ions at octahedral sites [40].

The properties of ferrite nanoparticles are influenced by the composition and microstructure

which are sensitive to the preparation methodology used. Ni ferrites as well as Ni-based

mixed ferrites are extensively investigated by various researchers [41-44]. Different methods

have been reported for the synthesis of NiFe2O4. Nickel ferrite particles have been prepared

by using hydrothermal method [45]. Samples were prepared in presence of glycerol and

sodium dodecyl sulfate and inhibition effect of surfactant on NiFe2O4 particles growth has

been studied. Nickel ferrite NiFe2O4 particles of high crystallinity have been synthesized by

forced hydrolysis of ionic iron (III) and nickel (II) solutions in 2-hydroxyethyl ether [46].

NiFe2O4 nanoparticles have been prepared by the sol-gel method using polyacrylic acid

(PAA) as a chelating agent [47]. Nickel ferrite nanoparicles with various grain sizes are

synthesized using annealing treatment followed by ball milling of its bulk component

materials and their magnetic properties have been studied [48]. NiFe2O4 particle/organic

hybrid were synthesized in situ from iron-organic and nickel organic compounds below 100

°C and the remanent magnetization and coercive field of the hybrid were evaluated as 7.4

emu/g and 460 Oe, respectively, at 5 K [49]. Solvothermal synthesis of size controlled nickel

ferrite particles has been carried out and their magnetic properties have been studied [50].

NiFe2O4 have been synthesized by citrate precursor gel formation of average size 55.4 nm

and their magnetic behavior has been studied [51]. Synthesis of chromium-substituted nickel

ferrites has been carried out by aerosol route and cation distribution along with magnetic

properties has been studied [52]. Oxidative stress mediated apoptosis induced by nickel


166

ferrite nanoparticles in cultured A549 cells has been studied and it has been observed that

nickel ferrite nanoparticles induced dose-dependent cytotoxicity in A549 cells demonstrated

by MTT, NRU and LDH assays [53]. In the present manuscript, synthesis of NiFe2O4

nanoparticles has been reported by simple aqueous precipitation method using aqueous

ammonia as precipitating agent.No stabilizing agent has been used in the synthesis. This

method involves a simple, cheap and one step process for synthesis of very fine NiFe2O4

nanaoparticles as compared to other methods of synthesis like ultrasonic radiation, sol-gel

approach, Fe implantation thermal decomposition of metal-surfactant complexes, colloid

mill, mechanical milling etc. The obtained particles of NiFe2O4 have size from 10-28 nm.

The synthesized nanoparticles were characterized by XRD, TEM and VSM studies.

4.2.1 Results and discussions:

X-ray studies:

X-ray diffraction of synthesized NiFe2O4 is shown in Figure (4.6). X-ray diffraction pattern

of NiFe2O4 pure indicated that Nickel ferrite is in the form of NiFe2O4. In X-ray diffraction,

some prominent peaks were considered and corresponding d-values were compared with the

standard i.e. JCPDS file No. 74-2081 (Table-4.5). X-ray diffraction shows that metal oxide is

pure NiFe2O4 having cubic spinel structure. The peaks indexed to (220), (311), (400), (422),

(511) and (440) planes of a cubic unit cell, corresponds to single phase spinal crystal

structure. Sharpness of the peaks shows good crystal growth of the ferrite particles. Average

particle size (t) of the particles have been calculated from high intensity peak (311) using the

Debye-Scherrer equation

t = Kλ/ B cos θ

Where t is the average crystallite size of the phase under investigation, K is the Scherrer

constant (0.89), λ is the wave length of X – ray beam used, B is the full-with half

maximum(FWHM) of diffraction (in radians) and θ is the Bragg’s angle. The average

crystallite size calculated is 23nm which is in close agreement with the TEM results. Lattice

constant of ferrite nanocrystals are computed using the d value (interplaner spacing) and their

respective lattice (h k l) parameters. Lattice constant for ferrite nanocrystals has been found

to be 8.31915A0. The actual (X-ray) density of NiFe2O4 nanoparticles is calculated using the

formula Ρx = 8M/Na3 and is given in Table 4.6. Where M is the molecular weight (kg) of the

sample, N the Avogadro’s number (per mol) and a the lattice constant (Å). Value of Px was

calculated as 5.40707 (g/cc).


167


Magnetic measurements were carried out to find out the magnetic behavior of synthesized

nickel ferrite. The magnetic measurement of NiFe2O4 was carried out at room temperature

and it has been observed that NiFe2O4 shows ferromagnetic behavior in nanocrystaline form

as there is no hysteresis observed. It showed very small Ms value (15 emu/g) obtained

[Fig.4.7]. Previously reported values of Ms for nickel ferrite nanoparticles prepared by

various methods have been reported in Table 4.7. The value of Ms ranging from 30-55.56

emug-1 shows that Ms strongly depends on the synthesis method used . This Ms Value of 15

emu/g at room temperature is comparable with earlier synthesized nanoparticles.

TGA/DTA


derivative Thermogravimetry (DTG). Thermal Gravimetric studies of the calcined oxides


TGA/DTA curves of the Nicklel ferrite are shown in Fig. (4.8). The maximum total weight

loss observed for Nickel ferrite and their corresponding temperature is summarized in Table

(4.8). Results showed that in the synthesized oxides shows some weight loss and oxide

undergoing decomposition, dehydration or any physical change. In DTA curve also, there is

exothermic and endothermic peak which shows phase transition, solid state reach on any

chemical reaction occurred during heating treatment.

SEM/ TEM studies

Morphology of the sample was investigated by using SEM and TEM. Morphology of the

sample is shown by the SEM micrograph (Figure-4.9 a, b, c, d). TEM studies were carried to

find out exact particle size of synthesized NiFe2O4. Figure 4.10 shows the TEM image of the

synthesized NiFe2O4 nanoparticles. The single crystal nature of the NiFe2O4 is revealed by

TEM analysis. A very fine spherical NiFe2O4 nanoparticle in the range of 10-28 nm with

average size of ~20nm is obtained. The size distribution histograms for nanoparticles provided

their respective sizes as 23.4 ± 5.2 nm [Fig. 4.10 a], 22 ± 5.6 nm [Fig. 4.10 b], 20.5 ± 5.7 nm

[Fig. 4.10 c], 19.6 ± 4.6 nm [Fig. 4.10 d], 17.9 ± 5.8 nm [Fig. 4.10 e], 22.7 ± 3.4 nm [Fig.

4.10f], respectively. The average crystallite size DXRD, DTEM, and the lattice constant (a) of the

sample obtained are summarized in Table 4.6.


168

4.2.2 Abstract:

NiFe2O4 nanoparticles with cubic structure are synthesized successfully by aqueous

precipitation method. TEM study show very fine nanoparticles of diameter 10-28 nm with

average size of 20nm. VSM studies show ferromagnetic behavior of synthesized

nanoparticles. This method is advantageous over the existing methods of synthesis of

nanoparticles because other methods require specialized instrumentation, highly skilled

labour, expensive materials and methods. Therefore, the proposed precipitation method is

very promising and may have extensive applications.


169

4.3 A simple and effective method of the synthesis of nanosized CuFe2O4 particles

copper ferrite (CuFe2O4) is one of the important spinel as copper ferrite (CuFe2O4 ) have

paramount advantages over other type of magnetic materials due to its unmatched flexibility

in magnetic and mechanical parameters , high stability , high quality, low cost and low eddy

current losses over a wide range of frequency from 10 KHz to 50 KHz [54-55]. Copper ferrite

(CuFe2O4) is an important material to be used in different applications such as catalyst [56-

58], synthesis of temperature sensitive magnetic fluid [59-60], new pigments [61],

sensors[62], Li-ion batteries [63], magnetic refrigeration [64] and electrochemical cells [65].

Unlike ferromagnetic metals ferrites are also good electrical insulators. Microstructure and

magnetic performance of ferrites considerably depends upon chemical composition of sample

[66]. Copper ferrite (CuFe2O4) occurs mainly in two different crystal structures in cubic and

tetragonal. The tetragonal structure is stable at room temperature and changes into cubic

phase at 623K temperature due to Johan-Teller distortion [67]. Due to the potential

applications of ferrites they are synthesized from industrial wastes by using ball milling

technique [68], wet method [69] using Box- Behnken design model [70] and by using silica

nanosphere [71]. Published papers in the literature have been done to apply Box-Behnken

design model for food control [72], Pharmaceutics [73] and Integrated membrane system

(1ms) [74]. Yang et al [75] synthesized copper ferrite (CuFe2O4 ) by using different

techniques like solid state reaction and sol-gel method. Hankare and co-workers [75] used

oxalate precipitatation method. Ahmed et al [76] synthesized crystalline copper ferrite with

higher bulk density (3.93g/cm3). Synthesis of nanosized copper ferrite (CuFe2O4) is also

explained by various methods [77-78] like mechanochemical [79], combustion synthesis [80-

89], polyol route [90-95] and microemulsion hydrothermal rote [96-102]. The current method

is most convenient to synthesize nanosized copper ferrite (CuFe2O4 ) because of its simplicity

and low coast.

4.3.1 Results and discussions:

X-ray studies:

XRD studies were carried out to the above nano ferrite and XRD spectrum is presented in

Fig. 4.11. X-ray diffraction pattern of CuFe2O4 pure indicated that copper ferrite is in the

form of CuFe2O4 (Figure 4.11). In X-ray diffraction, some prominent peaks were considered

and corresponding d-values were compared with the standard i.e. JCPDS file No.34-0425

(Table-4.10). X-ray diffraction shows that metal oxide is pure CuFe2O4 having spinel

structure. This shows that the synthesized powder has nano size crystalline. X-ray diffraction


170

pattern confirms that formation of single – phase cubic structure. It has been observed that the

material prepared is having lattice constant of 8.398 A0. Thickness of the crystals has been

calculated using Scherrer’s formula and it also support the TEM observations.


The magnetic measurement of CuFe2O4 was carried out at room temperature and it has been

observed that CuFe2O4 shows super paramagnetic behavior at room temperature (300 K) with

saturation magnetization (Ms) value 50 (Fig.4.12). Previously reported values of Ms for

copper ferrite nanoparticles prepared by various methods has been reported in (Fig.4.12). The

value of Ms ranging from 12-88 emug-1 shows that Ms strongly depends on the synthesis

method used . This Ms value at room temperature is good and comparable with methods of

synthesis as thermal decomposition method (Ms value 42 at 300K and Ms value 65 emug-1 at

10K), ball milling (Ms value 20.7 in at 4 K) and other co-precipitation routes which shows a

maximum Ms 46 at 4 K .

Thermal Analysis:


derivative Thermogravimetry (DTG). Thermal Gravimetric studies of the calcined ferrites.


TGA/DTA curves of the copper ferrite are shown in Fig. (4.13). The maximum total weight

loss observed for copper ferrite and their corresponding temperature is summarized in Table

(4.11). Results showed that in the synthesized oxides shows some weight loss and oxide

undergoing decomposition, dehydration or any physical change. In DTA curve also, there is

exothermic and endothermic peak which shows phase transition, solid state reach on any

chemical reaction occurred during heating treatment.

SEM / TEM Studies:

Morphology of the sample was investigated by using SEM and TEM. It is evident by the

SEM micrograph (Fig. -4.14) that the CuFe2O4 have almost uniform spherical structure. It is

observed less number of pores with smaller lump size, resulting fine grained microstructure

with respect to ferrites.

TEM studies were carried to find out exact particle size of synthesized CuFe2O4 (Fig.4.1 4a,b)

shows the TEM images of synthesized CuFe2O4 nano particles. It shows that the size of the

obtained nano particles is in the range of the size of the nano particles calculated using TEM

images were found to be in the range of 20-40 nm (Table4.12)which is in good agreement

with the particle size calculated using XRD data. TEM images indicate that CuFe2O4 samples


171

were all spherical particles with uniform grain size distribution. CuFe2O4 nanoparticles were

prepared by economical and simple precipitation method.

4.3.2 Abstract:

XRD pattern of the sample prepared by precipitation method shows nano crystalline nature

of the sample. It has been observed that the material prepared is having lattice constant of

8.398A0. The average particle size resulting synthesized were observed to the 30nm which is

well supported by SEM/TEM micrographs (ranging from 20-40nm). Magnetic measurements

show that CuFe2O4 is super paramagnetic in nature having saturation magnetization (Ms)

value 50 emu/g. The notable advantages are high yield of product less expensive, shorter

reaction times, mild reaction, conditions and easy workup. This method is advantageous over

existing methods of synthesis of nanoparticles because other methods require specialized

instrumentation, highly skilled labour, expensive materials and methods. Therefore, the

proposed precipitation method is very promising, easy and cheap and may have extensive

applications.


172

Table-4.1 X-RAY diffraction data for ZnFe2O4

S. No. d=λ / 2sinθ

(Observed)

d=λ / 2sinθ

(Reported)

I/I 0X100%

(Observed)

I/I 0X100%

(Reported)

1. 2.98857 2.98800 40 35

2. 2.54627 2.54611 100 100

3. 2.43412 2.43857 16 5

4. 2.10861 2.11170 18 16

5. 1.72381 1.72342 14 7

6. 1.62691 1.62478 30 30

7. 1.48866 1.49278 46 30

8. 1.35144 1.33522 8 2


173

Table-4.2 Reported value of saturation magnetization in literature

Ms(emu/g) temp size Synthesis method

50 300 10-30 precipitation

38 60 4 hydrothermal method

25 5 12 Ultrasound-assisted emulsion

53.9 5 14.8 Polyol method

70 3 3.7 Oil-in-water micelles

61.87 80 300 hydrothermal in ammonia solution

11.9 2 32 self-propagating combustion

37 4.2 47 ball milling

22 5 8.1 supercritical sol-gel + drying at 513 K

38 4.2 5-20 hydrothermal in supercritical methanol

20.7 4.2 36 ball milling

40.3 4.2 50 ball milling + calcinations at 773 K

10 300 11 ball milling

58 5 9 ball milling

46.9 4.2 55 co-precipitation at 373 K

26.4 5 29 co-precipitation at 373 K + calcination

65.4 10 9.8 thermal decomposition

56.6 300 thin film pulsed lased deposition


174

TABLE: 4.3: Observations of weight loss for zinc ferrite at corresponding temperature

range

TABLE-4.4:- Partical size of synthesized zinc ferrite at different scales

S.N. Scale (20nm) Scale (100nm)

1 28 25

2 10 20

3 30 31

4 20 30

5 31 30

6 31 29

7 28 12

8 31 20

9 28 10

10 31 16

Range 10nm to 30nm 10nm to 30nm

S.N Maximum % loss in weight Temperature range

1 4.223% 714.22-908.2


175


(Observed)

d=λ / 2sinθ

(Reported)

I/I 0X100%

(Observed)

I/I 0X100%

(Reported)

1. 2.50832 2.5139 100 100

2. 2.95501 2.9478 41 30

3. 2.40448 2.4069 21 7

4. 2.09075 2.0844 35 20

5. 1.70883 1.7019 16 08

6. 1.60606 1.6046 38 26

7. 4.82418 4.8138 19 11

8. 1.47254 1.4739 60 33

Table-4.5 X-RAY diffraction data for NiFe2O4


176

Table 4.6

Different parameters for synthesized NiFe2O4

Table 4.7

Size and Magnetic parameters for as synthesized Nickel Ferrite

Particle size

DTEM(nm)

Particle size

DXRD(nm)

Lattice

constant[A0]

X- ray

density(Ρx)

Magnetization

M(emu/g)

20nm 23nm 8.31915 5.40707 15

Nickel ferrite Ms

(emu/g)

Temp Size Synthesis method

NiFe2O4 15 600 10-30 Precipitation

NiFe2O4 38 478K 4.4 Forced hydrolysis

NiFe2O4 55.56 - 20-30 Thermal Plasma

NiFe2O4 31.62 600 16.7 Sol gel

NiFe2O4 30.8990 600 15.009 Precipitation


177

TABLE: 4.8

Observations of weight loss for nickel ferrite at corresponding temperature range

Sr.No. Maximum % loss in weight Temperature range

1 4.223% 714.22-908.2

TABLE-4.9

Partical size of synthesized nickel ferrite at different scales

S.N. Scale (20nm) Scale (100nm)

1 28 25

2 10 20

3 20 10

4 20 20

5 20 28

6 20 20

7 28 22

8 25 20

9 28 22

10 10 20



178

Table-4.10 X-RAY diffraction data for CuFe2O4


(Observed)

d=λ / 2sinθ

(Reported)

I/I0X100%

(Observed)

I/I0X100%

(Reported)

1. 4.8390 4.8390 17 17

2. 2.9851 2.9850 32 32

3. 2.9230 2.9232 13 12

4. 2.5817 2.5816 53 54

5. 2.5020 2.5020 100 100

6. 2.4199 2.4199 14 12

7. 2.1580 2.1582 11 10

8. 2.066 2.061 22 22

9. 1.9345 1.9340 1 1

10. 1.7360 1.7363 5 4

11. 1.6989 1.6987 10 11

12. 1.6550 1.6553 12 11

13. 1.6134 1.6130 11 10

14. 1.5931 1.5931 24 24

15. 1.4921 1.4920 40 40

16. 1.4611 1.4610 16 17

17. 1.4119 1.4117 1 2

18. 1.3582 1.3581 2 1

19. 1.3117 1.3116 2 2

20. 1.3067 1.3065 2 3

21. 1.2922 1.2921 5 5

22. 1.2899 1.2897 4 4

23. 1.2713 1.2710 9 7

24. 1.2506 1.2504 4 4

25. 1.2098 1.2098 5 5


179


180

Table-4.11 Reported value of saturation magnetization in literature

Ms(emu/g) temp size Synthesis method

50 300 10-30 precipitation

38 60 4 hydrothermal method

25 5 12 Ultrasound-assisted emulsion

53 5 14.8 Polyol method

70 3 3.7 Oil-in-water micelles

61 80 300 hydrothermal in ammonia solution

11 2 32 self-propagating combustion

37 4.2 47 ball milling

22 5 8.1 supercritical sol-gel + drying at 513 K

38 4 5-20 hydrothermal in supercritical methanol


40 4 50 ball milling + calcinations at 773 K


58 5 9 ball milling

46.9 4 55 co-precipitation at 373 K

26.4 5 29 co-precipitation at 373 K + calcination

65.4 10 9.8 thermal decomposition

56. 300 thin film pulsed lased deposition


181

TABLE: 4.12: Observations of weight loss for copper ferrite at corresponding

temperature range

S.N. Maximum % loss in weight Temperature range

1 4.223% 714.22-908.2

TABLE-4.13:- Partical size of synthesized copper ferrite at different scales

S.N.. Scale (20nm) Scale (100nm)

1 28 25

2 31 20

3 40 31

4 20 32

5 31 33

6 31 31

7 28 22

8 31 20

9 28 40

10 31 36



182

Figure 4.1 XRD spectra of Zinc Ferrite


183

-60

-40

-20

0

20

40

60

-4000 -3000 -2000 -1000 0 1000 2000 3000 4000

Oe

M(

emu

/g)

Figure 4.2: Magnetic measurement of synthesized Zinc ferrite particles


184

Fig.4.3 TGA-DTA of zinc ferrite particles


185

Fig.4.4 SEM images of zinc ferrite


186

Figure 4.5 TEM images of zinc ferrite nanoparticles


187

-20

-15

-10

-5

0

5

10

15

20

-3000 -2000 -1000 0 1000 2000 3000

Figure 4.6 XRD spectra of nickel ferrite

220

311

400

422

511

440

Oe

M (emu/g)

222

Figure 4.7 Magnetic measurements of nickel ferrite nanoparticles


188

Fig.4.8 TGA-DTA of nickel ferrite particles


189

Fig.4.9 SEM images of nickel ferrite


190

Figure 4.10 TEM images of Nickel Ferrite nanoparticles

0

10

20

30

40

50

60

10 20 30 40

Average = 23.4 ± 5.2nm

Fre

quen

cy (

%)

Diameter (nm)0

10

20

30

40

50

60

10 20 30 40

Average = 22 ± 5.6nm

Fre

quen

cy (

%)

Diameter (nm)

a b


191

Figure 4.10TEM images of nickel ferrite nanoparticles

0

10

20

30

40

50

60

10 20 30 40


Fre

quen

cy /

nm

Diameter (nm)

0

10

20

30

40

50

60

70

80

10 20 30 40


Fre

quen

cy (

%)

Diameter (nm)

c d


192

0

10

20

30

40

50

60

10 20 30 40


Fre

quen

cy (

%)

Diameter (nm)

0

10

20

30

40

50

60

70

10 20 30 40


Fre

quen

cy (

%)

Diameter (nm)

e f

Figure 4.10TEM images of nickel ferrite nanoparticles


193

Figure 4.11 XRD spectra of copper ferrite

CHAPTER4 SYNTHESIS AND CHARACTERISATION

Figure 4. 12: Magnetic measurement of

Fig.4.13

SIS AND CHARACTERISATION OF NANOSIZED FERRITES (RESULTS AND DISCUSSION)

194

Figure 4. 12: Magnetic measurement of synthesized copper ferrite particles

Fig.4.13 TGA-DTA of copper ferrite particles

FERRITES (RESULTS AND DISCUSSION)

ferrite particles


195

Figure 4.14: SEM images of copper ferrite particles


196

Figure 4.15: TEM images of copper ferrite particles


197

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