Effect of Co doping on Structural, Optical and Magnetic Properties

of Fe doped ZnO Nanoparticles

Raminder Preet Pal Singh,1* I. S. Hudiara,2 Sudhakar Panday,3 Shashi Bhushan Rana4

1,3
Department of Electronics & Communication Engineering, Desh Bhagat University, Mandi
Gobindgarh, India
2
Chitkara University (Punjab Campus), Chandigarh, India
4
Department of Electronics & Communication Engineering, GNDU Regional Campus,
Gurdaspur, India
*
Corresponding author. Email: raminder_212003@rediffmail.com

Abstract

In the present work, pure ZnO, Zn 0.99Fe0.01O (ZFO) and Zn1-x-yFexCoyO (x=0.01, y=0.01, 0.03,

0.05) Fe-Co codoped ZnO dilute magnetic semiconductors were successfully synthesized by

using the wet co-precipitation method. Pure and doped samples were characterized by X-ray

diffraction, Scanning electron microscopy, X-ray energy Dispersive spectroscopy, UV-Vis

spectroscopy and vibrating sample magnetometer. The X-ray diffraction (XRD) analysis of pure

and doped samples confirms the formation of hexagonal wurtzite structure, without formation of

any other secondary and impurity phases. Surface morphology of pure and doped ZnO

nanoparticles samples was performed by scanning electron microscopy (SEM) reveals the

formation of spherical nanocrystallites with clear and well defined boundaries. X-ray energy

dispersive spectrometry (EDS) indicates the substitution of dopant Fe 2+and Co2+ successfully in

lattice site of Zn2+ and results in the formation of single-phase Zn 1-x-yFexNiyO. The UV-Visible

absorption spectra of all doped samples showed in absorption edge as compared to

undoped ZnO nanoparticles. The magnetic characterization reveals and confirms the room

temperature ferromagnetism in all doped and co-doped samples. Magnetization saturation

increases with increase in Co concentration in Fe doped sample as compare with individual Fe

doped ZnO sample which further reveal that exchange interaction between Fe and Co ions

dominates over the Fe-Fe ions interaction.

Introduction

Diluted magnetic semiconductors (DMS) have attracted much attention in recent years

because it is a type of semiconductor in which fraction of host cations can be easily replaced

by magnetic ions for its potential applications in fabricating spintronics devices such as spin-

valve transistor [1-4]. ZnO is a group II-IV compound semiconductor and has become one of

the most promising candidates for DMS materials [5]. Moreover, ZnO have potential

applications in optoelectronics due to its, wide band-gap (3.37 eV) and high exciton binding

energy (60 meV) properties. In the past few years, scientists are investigating the effect of

doping ZnO nanoparticles with transition metals such as Fe, Co, Ni and Mn. [6-18]. Lot of

theories have proposed and predicted revealed that on doping ZnO nanoparticles with these

transition elements results dramatic change in various luminescent and magnetic properties.

These transitions metals have been doped on ZnO lattice to change the different optical and

magnetic properties, which further have potential applications in spintronics devices, such as

spin field effect transistor, gas sensor and in quantum computers. In order to realize these

objectives; it is absolute necessary to create ZnO based ferromagnetic material, where their

physical and structural properties must be well understood explicitly. Experimental studies

confirmed that the ferromagnetism strongly depends on synthesis techniques and

environmental conditions used for the preparation of samples. A lot of work had been done on

single transition metal doped ZnO prepared by various techniques [19-20]. There are few

reports on co-doping of two magnetic elements simultaneously in a host material such as Fe-
Co codoped [21], Mn-Co codoped [22], Cr-Fe codoped and Co-Cu codoped [23]. Xiaojuan

Wu et al. [24] also synthesized Fe-Ni codoped ZnO (Zn 0.95Fe0.03Ni0.02O) nanorods by a

hydrothermal method and reported that room temperature ferromagnetism for codoped sample

is greater than that of single doped Fe and Ni samples. Various chemical methods have been

developed to prepare nanoparticles (NPs) of different materials of interest. Most of the ZnO

nanocrystals have been synthesized by traditional high temperature solid state reaction

method. However this method is time consuming and properties of the product can’t be

controlled. Hence, ZnO nanoparticles can be prepared on a large scale at low cost by simple

solution based methods, such as chemical co-precipitation, hydrothermal reaction, and sol-gel

synthesis.

In this work, co-precipitation method was chosen for synthesis because it requires less

temperature, cost effective and offers larger degree of solubility of dopants. The effect of Fe, Ni

and their co-doping on the structural, morphological, optical and magnetic properties on ZnO

nanoparticles were investigated by using XRD, SEM, UV-Vis and VSM respectively. It was

observed that by incorporating the Fe, Ni and their co-doping on ZnO nanoparticles not only

results in increase in ferromagnetic properties in host material but changes the optical properties

and lattice constant values in structural studies.

Organization of this research paper is summarized as follows: Section 1, illustrate the

experimental procedure followed to synthesize the doped and undoped ZnO nanoparticles,

followed by section 2, which describe the instrumentation used to characterize the structural,

morphological, optical and magnetic properties of undoped and doped ZnO sample. In Section 3,

various results have been discussed in detail related to above said properties, while the Section 4

concludes the paper.

1. Experimental Procedure
All the materials used in this work were of analytical reagent grade and we have used them

without any further purification. In order to synthesize the pure ZnO nanoparticles, Zinc Acetate

(Zn (CH3COO) 2.2H2O), was dissolved in distilled water and stirred for 1 hour. Aqueous solution

of NaOH was added drop-wise to the solution to maintain the pH ~10.The solution was then

stirred at room temperature for 4 hours followed by aging for 24 hrs at the same temperature.

After aging, precipitate that formed was filtered and washed several times and was finally

annealed at 600°C for 2 hrs. In order to synthesize the doped (ZFO and ZNO) and co-doped

sample (ZFNO) nanocrystals, same steps have been followed except adding Ferric Nitrate

(FeNO3) and Nickel Acetate (C4H6NiO4.4H2O) according to the calculated stoichiometric ratio.

2. Characterization of pure and doped samples

X-ray diffraction patterns of all the powder samples were recorded by rotating angle X-ray

diffractometer (Bruker AXS D8 Advance, Germany) equipped with graphite monochromator, a

mirror at a fixed incidence angle of 1-5° and CuKα (Wavelength= 1.540 Aº, 40 KV, 100 mA)

radiation source. The angular accuracy of the setup was 0.001º and the angular resolution was

about 0.01º. The samples were scanned in angular direction in the range from 20 to 90º (2θ) with

step size of 0.01º. Surface morphology of undoped (pure) and doped synthesized samples was

ascertained by using scanning electron microscope Carl Zeiss Supras 55 which operates at a high

accelerated voltage of 15 kV. The UV absorption spectra of the samples were recorded on the

Systronics-2205 double beam spectrophotometer having bandwidth 1nm and wavelength ranges

from 200-1100 nm. Elemental composition of various sample were ascertained by using EDS

spectroscopy at an acceleration voltage of 200 keV. Magnetic hysteresis loop at room

temperature was measured by using the Vibrating Sample Magnetometer (VSM, Microsense

EZ9) having maximum magnetic field strength of 22.5 kOe.

3. Results and discussions

3.1 XRD Analysis

Figure 1(a), (b) shows X-ray diffraction patterns of the synthesized undoped (pure ZnO) and

doped (ZFO, ZNO and ZFNO) samples. Each XRD sample exhibit the hexagonal wurtzite phase

without any impurities and secondary phase formation. It is clearly from XRD pattern that all the

characteristic diffraction peaks can be indexed to the diffractions of (100), (002), (101), (102)

and (110) planes with a hexagonal wurtzite structure. These diffraction peaks agree well within

the values of the standard value of JCPDS01-079-2205 card value. From the XRD pattern of

figure 1(a) and (b) it is clear that the doped samples show lowering of intensity and peak position

of doped samples shifts to higher angles in (101) characteristic peak as compared to undoped

(pure) ZnO. It is observed further, that the intensity of diffraction peaks decreases markedly as a

function of Fe and Ni concentration, signifying that the crystalline character of the ZnO had

reduced considerably due to Fe and Ni doping. The XRD spectra clearly show that some XRD

peaks appearing in undoped ZnO at higher angles disappear in the Fe, Ni and Fe-Ni doped ZnO

samples. This phenomenon is due to the reduction of grain size and presence of strain in the ZnO

lattice due to induction of Fe, Ni and Fe-Ni atoms. For co-doped sample, NP size reduction is

significant as compared to undoped and doped NPs as shown in Table 1.

Figure 1(b) clearly showed the shifting of peak toward higher 2θ angle value with doping of Fe,

Ni and co-doping. The change in the peak positions clearly indicates that Fe and Ni ions are

occupying the Zn position in the ZnO matrix [25].

Fig. 1: (a) XRD patterns of pure ZnO, ZFO, ZNO and ZFNO nanoparticles annealed at 600℃, (b) Shifting of (101)
peak with the doping concentration.

The average crystalline size was calculated by using Scherrer’s equation (1) and was found to be

in the range of 36 nm to 45 nm as shown in table 1.

kλ
τ= (1)
β cos θ

Where, τ is grain size, B is the full width at half maxima and λ is the wavelength of X-ray used

(1.548 Å) and θ is the diffraction angle. Lattice strain and dislocation density increases with

doping and co-doping as compared with undoped ZnO as shown in table 1. From the d values,

lattice constant ‘a’ and ‘c’ is calculated using equation (2) and values their values are given in

table 1.

( )
2 2 2
1 4 h +hk +k +l
2
= 2 2 (2)
d 3 a c

The ionic radius value for various element like Fe +3, Ni+2 and Zn+2 is 67 pm, 69 pm and 74 pm

respectively. It is clearly observed from the table 1 that value of lattice parameters and d value
goes on reducing due to the smaller ionic radius of Fe, Ni and Fe-Ni ions due the substitution of

Zn+2 by Fe+3, Ni+2 and Fe-Ni ion during the doping process.

Table 1: Micro-structural properties of Pure ZnO, ZFO, ZNO and ZFNO nanoparticles.

d101 Lattice
Particle
Sample (Å) Constant
Size
a C
Pure ZnO 45 nm 2.4768 3.233 5.280
ZFO 39 nm 2.4755 3.232 5.278
ZCO 50 nm 2.4749 3.231 5.276
ZFCO1 42 nm 2.4861 3.245 5.30
ZFCO3 44 nm 2.4847 3.243 5.297
ZFCO5 46 nm 2.4821 3.240 5.292

The XRD spectra also show that the intensity of characteristic XRD peaks decreases on changing

the doping concentration of these dopants, which further indicates the reduction in crystalline

character and decrease in crystallite size as evident from table 1.

3.2 Scanning Electron Microscope (SEM) Analysis

The morphology of pure and doped samples was studied by using the scanning electron

microscope (SEM) analysis. Figure 2(a-d) shows the SEM images of pure ZnO, ZFO, ZNO and

ZFNO nanoparticles with an average particle size of approximately 65 nm, 62 nm, 60 nm and 53

nm respectively.

The SEM image of pure ZnO shows that the particles are spherical in shape with large

agglomeration. It is clearly found from the figure 2 (b-d) that the aggregation is almost restricted

in doped ZnO (from ZFO to ZFNO) particles which appears in consistent and uniform shape

with constricted size distribution. The particle size measured from XRD is quite different from

the SEM measurement because in SEM calculation is done by taking the difference of noticeable

grain boundaries, whereas in case of XRD measurements are taken from the crystalline area that

reasonably diffracts the X-ray waves.

 Fig. 2: SEM images (a-d) of Pure ZnO, ZFO, ZNO and ZFNO nanoparticles.

From Figure 2 (b-c), it is clear that particle size goes on decreasing because dopant Fe and Ni are

diffusing homogeneously in the different sites and they are clearly visible with less porosity in

the background portion. It is clear from SEM micrograph that pure ZnO nanoparticles appears in

bigger form, while codoped ZNFO nanparticles appears in smaller size which verifies the XRD

results.

Elemental composition of the synthesized nanoparticles (doped and undoped) was determined

from the energy dispersive X-ray spectrum (EDS) as shown in figure 3. The EDS analysis

confirms the presence of Fe, Ni, O and Zn in the doped sample with no other impurity element.

Figure 3 shows the EDS spectra of ZNFO sample. The EDS spectrum indicates

that the synthesized ZNFO sample mainly contain Fe, Zn, Ni and O elements.
The EDS spectral peaks of O appeared at 0.5 keV, Zn appeared at 1, 8.6 and

9.5 keV while Fe signal appears at 0.6 keV, 6.5 keV and 7.2 keV respectively.

The EDS results further verify XRD results, which reveals that Fe and Ni

doped ZnO magnetic semiconductors were successful synthesized by the

chemical precipitation method.

Fig. 3: X-ray energy dispersive spectrometry (EDS) spectrum of ZFNO sample.

3.3 Optical Absorption Study

Pure ZnO, doped and co-doped ZnO nanoparticles were compared employing UV-Visible

absorption spectroscopy. The band gap of semiconductor nanoparticles changes

as the various dopants can cause different crystal defect on ZnO crystals.

The UV-Visible absorption study of pure ZnO, doped and codoped ZnO

nanoparticles samples has been investigated as shown in figure 4 in the

wavelength range of 300–800 nm. The value of the absorbance is purely

dependent on the various factors like size of particles, flaws or deformities in

grain structure and oxygen deficiency.

As the doping concentration is changed from ZNO, ZFO and ZNFO the

absorption edge is start to shift towards lower wavelengths (blue shift) which

mean the band gap increases which results due to defects (strain) and hence

leads to the reduction in crystallite size as discussed in XRD analysis. Figure 4,

shows the absorption spectra of the pure ZnO , ZFO, ZNO and ZFNO nanoparticles with the

absorption peak at 390 nm, 388nm, 387nm and 380 nm respectively.

Fig. 4: UV-Visible absorption spectra of Pure ZnO, ZFO, ZNO and ZFNO nanoparticles.

Table 2, summarizes the band gap energy (Eg = hc/λ) value for undoped (pure) and doped ZnO

nanoparticles. The optical band gap value calculated in our pure ZnO sample is small (3.19 eV)

as compared with standard band gap value of bulk ZnO material i.e. 3.3 eV. But, the observed

Eg value is in good agreement with the Eg value determined in literature [26-27]. From table 2, it

is concluded that band gap energy increases with Fe, Ni and Fe-Ni doping, which shows a blue

shift in wavelength.

Table 2: Band gap energy (Eg) variation of Pure ZnO, ZFO, ZNO and ZFNO nanoparticles.

Sample Absorption Band Gap

Wavelength Energy
 (λ) (Eg = hc/λ)
Pure ZnO 390 nm 3.19 eV
ZFO 388 nm 3.21 eV
ZNO 387 nm 3.22 eV
ZFNO 380 nm 3.27 eV

The increase in band gap from 3.19 eV to 3.27 eV is due to decrease or reduction in particle size

due on changing the various dopants Fe+3, Ni+2and Fe-Ni, respectively on ZnO. This

phenomenon of increase in band gap energy (Eg) and absorption at the lesser wavelength can be

explained on the basis of quantum confinement effect amongst the individual doped ZnO

nanoparticles.

3.4 Vibrating Sample Magnetometer (VSM) Analysis

Magnetization measurements of synthesized pure and doped nanoparticles were carried

out using vibrating sample magnetometer by using the magnetic hysteresis (M-H) curve. All the

measurements were made at room temperature. Pure ZnO sample shows diamagnetic behavior as

depicted from figure 5(a). Diamagnetic nature of pure ZnO has also been reported in literature

[28]. Whereas, from the magnetic hysteresis loops (M–H curve) for ZFO, ZNO and ZFNO

samples as shown in figures 5(b-d) respectively, it is clear that all samples exhibit ferromagnetic

behavior at room temperature. However, from table 3, it is clear that magnetization saturation

(Ms) and remanent (Mr) is enhanced in ZFNO sample as compare with individual magnetization

obtained in ZFO and ZNO samples. Whereas, corecivity (Hc) is reduced in ZFNO sample in

contrast to ZFO and ZNO samples. Moreover, coercivity obtained in all samples is very less

which reveals soft ferromagnetic characteristic of samples.

Table 3: Magnetic properties of ZFO, ZCO and ZFCO nanoparticles

Sample HC Mr Ms
(Oe) (emu/g) (emu/g)
 ZFO 61 0.0011 0.015
ZCO 897 0.0025 0.005
ZFCO1 298 0.0242 0.103
ZFCO3 201 0.0533 0.218
ZFCO5 550 0.0790 0.328

So far, several reasons have been discussed to explain origin of ferromagnetism and still this

subject is controversial. One of theory proposed that room temperature ferromagnetism of ZFNO

samples is exhibited due to various intrinsic and extrinsic phenomenon. Intrinsic phenomenon’s

results due exchange interaction, and extrinsic phenomenon occurs due to formation of clusters

or secondary phases of dopant semiconductor atoms [29]. The relationship between intrinsic

defects such as oxygen or Zn vacancies and magnetism is also discussed in some studies [30-31].

In our study, the XRD and EDS results showed that dopant ions are successfully incorporated in

the Zn wurtzite lattice without formation of any secondary phases and metallic clusters.

Therefore, possibility of ferromagnetism due to formation of secondary phases and metallic

clusters is completely ruled out in case of our all doped and co-doped samples.
 Fig. 5: M-H curve of (a) Pure ZnO, (b) ZFO, (c) ZCO, (d) ZFCO nanoparticles at room temperature.

Among different mechanism responsible for ferromagnetism, the oxygen mediated exchange

interaction between the dopant ions could be the possible mechanism responsible for the

observed ferromagnetic behavior in all the doped samples. In a recent paper, J. Das et al. [32],

proposed that exchange interaction mechanism mediate by oxygen vacancies is responsible for

enhancement in magnetic saturation when Ni is co-doped in Mn doped ZnO sample because co-

doping increases carrier concentration in the form of oxygen vacancies.

From XRD, EDS and VSM analysis of our samples, it is reasonable to say that observed room

temperature ferromagnetism in our samples is an intrinsic property of material and not due to

formation of any secondary phases or metallic clusters. Further, increase in magnetic saturation

of co-doped sample indicates that Ni-O-Ni and Ni-O-Fe exchange interaction in ZFNO sample

dominates the Fe-O-Fe and Ni-O-Ni exchange interaction in case of ZFO and ZNO respectively.

Therefore, we conclude that magnetic saturation increases with simultaneous doping of two

different transition metals i.e. Fe-Ni co-doping than single transition metal (Fe, Ni) doping at

room temperature. So in our discussion resulting paramagnetic is an intrinsic property of ZNFO

samples.

4. Conclusions

In our investigations, pure ZnO, Zn0.99Fe0.01O, Zn0.99Ni0.01O and Zn0.98Fe0.01Ni0.01O diluted

magnetic semiconductor nanoparticles were successfully synthesized via simple co-precipitation

method. X-Ray diffraction pattern show formation of hexagonal wurtzite structure for all

samples. UV-absorption spectrum shows blue shift in wavelength for doped and co-doped

samples as compared with undoped ZnO. Present work also confirms that the optical absorption

and band gap of ZnO nanoparticles can be controlled by Fe, Ni and Fe-Ni doping. Enhancement

in room temperature ferromagnetism has been observed in Fe-Ni co-doped ZnO sample as

compared with Fe and Ni doped ZnO samples. Few assumptions related to exhibition of room

temperature ferromagnetism have been addressed i.e. clusters, secondary phase and defect

related ferromagnetism. However, we believe that a small amount of Fe, Ni and Fe-Ni have

played the vital role in order to obtain the room temperature ferromagnetism. Oxygen mediate

exchange interaction could be the possible mechanism for observed ferromagnetism. In the co-

doped sample, Ni–O–Ni and Ni–O–Fe carrier mediated exchange interaction dominates the Fe-
O-Fe and Ni-O-Ni exchange interaction which results in increase in the value of saturation

magnetization at room temperature, is the best probable mechanism for origination of room

temperature ferromagnetism.

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