Study of optical properties of Ce and Mn doped BiFeO3 thin films using SPR technique for magnetic field sensing

Accepted Manuscript Study of optical properties of Ce and Mn doped BiFeO3 thin films using SPR technique for magnetic field sensing Ayushi Paliwal, Monika Tomar, Vinay Gupta PII:

S0042-207X(18)31440-4

DOI:

10.1016/j.vacuum.2018.09.018

Reference:

VAC 8231

To appear in:

Vacuum

Received Date: 31 July 2018 Revised Date:

6 September 2018

Accepted Date: 11 September 2018

Please cite this article as: Paliwal A, Tomar M, Gupta V, Study of optical properties of Ce and Mn doped BiFeO3 thin films using SPR technique for magnetic field sensing, Vacuum (2018), doi: 10.1016/ j.vacuum.2018.09.018. This is a PDF file of an unedited manuscript that has been accepted for publication. As a service to our customers we are providing this early version of the manuscript. The manuscript will undergo copyediting, typesetting, and review of the resulting proof before it is published in its final form. Please note that during the production process errors may be discovered which could affect the content, and all legal disclaimers that apply to the journal pertain.

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Study of optical properties of Ce and Mn doped BiFeO3 thin films using SPR

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technique for magnetic field sensing Ayushi Paliwal1, Monika Tomar2, and Vinay Gupta1* 1

Department of Physics and Astrophysics, University of Delhi, Delhi 110007, INDIA

2

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Department of Physics, Miranda House, University of Delhi, Delhi 110007, INDIA

*

Corresponding author Email id: [email protected]; [email protected]

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Contact no: +91 9811563101

Abstract

Surface Plasmon Resonance (SPR) technique has been used in the present work, to study the

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optical properties of pulsed laser deposited single phase BiFeO3, Mn doped BiFeO3 (BFMO) and Ce doped BiFeO3 (BCFO) thin films. Refractive index dispersion studies with varying incident wavelengths has also been studied. Magnetic field dependence on the optical properties of

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BFMO thin films have also been determined using SPR. A very sensitivity of 147 °/Tesla was

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found for the prism/Au/BFMO structure exhibiting maximum change in optical properties with magnetic field indicating the potential use of BFMO thin films for the realization of efficient optical sensor.

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Introduction

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Magnetic field sensor is a physical sensor which find enormous applications in the multidisciplinary fields such as magnetic storage, automotive sensors, navigation systems, nondestructive material testing, security systems, structural stability, military instruments etc. [1].

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Various magnetic field sensors depending on different principle of operation are available including SQUID [2], Hall effect [3], magnetoelectric effect [4] etc. SQUID based magnetic field

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sensors are used extensively and are highly sensitive, but they have several drawbacks like bulky instrument, costly, consume high power, low operating temperature, and electromagnetic interferences [5]. However, magneto-electric (ME) sensors are advantageous but require good quality and single phase multiferroics as sensitive materials. The growth of multiferroic materials

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with good crystallinity is a challenge and demand high processing temperatures besides epitaxially matched single crystal substrates. Hence, to conclude majority of the available magnetic field sensors suffer from certain drawbacks and require an alternate sensor in order to overcome these

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issues.

Research efforts are continuing towards the development of magnetic field sensors based on other

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optical techniques including interferometer, MOKE, refractive index of microfluid, fiber bragg grating etc [6]. Most of the research on magnetic field sensors exploited bulk magnetostrictive materials and magneto-optical crystals. Dai et al. used magnetic fluid based fiber bragg grating (FBG) as magnetically sensitive probe and measured the change in refractive index of fluid with magnetic field [6]. However, FBG is sensitive to the ambient temperature and suitable compensation circuits are essentially required. Angular magnetic field sensor for automotive

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applications is reported using magnetic tunnel junctions (MJT), but the requirement of complex electronic circuitry which should not be subjected to high temperatures was the problem [7]. Surface Plasmon Resonance (SPR) is an established and highly sensitive technique for the

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development of an optical sensor [8, 9, 10, 11]. Hence, SPR phenomena can be exploited for development of efficient magnetic field sensors and is a powerful technique that can overcome most of the problems encountered with above mentioned magnetic field sensors John Kerr in 1877

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discovered the Magneto-optic Kerr effect (MOKE) while he was examining the polarization of light reflected from a polished electromagnet pole [12]. The combination of these effects (MO)

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with SPR phenomena can result in the realization of efficient magnetic field sensors with high sensitivity. These novel optical sensors do not need any complicated electronic processing circuitry and have low power consumption.

In the field of photonic devices, magneto-optic materials have gained importance owing to their

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unique applications such as fiber-optic current sensing [13], polarization control [14], magnetic field measurements [15], optical modulation [16] and MO recording [17]. MOKE is a preferred technique for studying the MO properties of magnetic thin films for developing a magnetic field-

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based sensor. At room temperature both ferroelectric (FE) and ferromagnetic (FM) orders exists in multiferroic thin film proving it as promising candidates for various device applications like

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electrochemical sensors, photovoltaic devices, magnetic storage memories, high frequency magnetic devices, micro actuators, etc. [18, 19, 20, 21]. Perovskite-type oxide materials such as BiFeO3, BiMnO3, TbMnO3 etc. exhibit multiferroic properties and magnetization/dielectric polarization is expected to be modulated by the electric field/ magnetic field. Bismuth ferrite (BFO) possess simultaneous ferroelectric and antiferromagnetic orders (G-type) above the room temperature (Curie temperature,

>800 °C, Neel temperature

= 370 °C) and a weak

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ferromagnetism at room temperature [19]. These unique properties make BFO appropriate for various novel applications in the field of spintronics, many state memory devices, transducers (magnetically modulated), sensors based on magnetic field and ultrafast optoelectronic devices

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[19, 22, 23]. Furthermore, it is reported that the properties of BFO can be improved by A-site or B-site doping. Amongst all the rare earth elements in Lanthanides series, Cerium (Ce) has been identified as most suitable A-site dopant because of the similar value of the ionic radii of Ce3+ as

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that of Bi3+ [24]. Also, stabilization of BiO6 octahedron in BFO thin film can be achieved by Ce doping further decreasing the Bi volatilization [25]. In addition, the most suited element for B-

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site doping is Manganese (Mn) which can substitute the Fe site in BFO lattice with ease, due to comparable ionic size [26]. Hence, Ce and Mn have been identified as one of the most suitable dopant to enhance the ferromagnetic properties of BFO thin films [27]. Hence, in the present work efforts are done to study the optical properties of pure BFO, Mn doped BFO (BFMO) thin

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and Ce doped BFO (BCFO) thin films using SPR technique. The optimized configuration (prism/Au/BFMO) have been further exploited towards the development of magnetic field sensor in MOKE configuration using SPR.

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Experimental Details

Quartz prisms have been used in the present work for preparation of prism/Au/BFO/air system,

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since the growth of BFO thin film (single phase) require a high substrate temperature of about 600°C deposition. BFO thin films (100 nm thickness) were deposited on Au coated quartz prisms by PLD technique at the optimized deposition parameters as discussed in our previous reports [28]. Thin film of 10% Mn doped BFO (BiFe0.90Mn0.10O3) has been prepared by PLD using ceramic target (1-inch diameter) of respective composition. Ceramic target of composition BiFe0.90Mn0.10O3 with 20% Bi excess was synthesized by the conventional co-precipitation method using stock

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precursor solutions of required composition. Similarly, thin film of 12% Ce doped BFO (Bi0.88Ce0.12FeO3) has been prepared by PLD using ceramic target (1-inch diameter) of respective composition (BiCe0.20Fe0.80O3). These targets with 20% excess bismuth are prepared using the

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conventional co-precipitation method by preparing required composition of stock precursor solutions by dissolving Bi(NO3)3.5H2O}, Fe (III), {Fe(NO3)3.9H2O}, C4H6MnO4.4H2O} and Ce(NO3)3.6H2O into CH3OCH2CH2OH as solvent with suitable additives like formadide. This is

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followed by mixing the mixture vigorously using magnetic stirrer for 2 hours at room temperature in order to obtain the dark wine red color sol. After this, alkali ammonia solution is

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added drop wise to the final obtained solution and finally the voluminous organic based fluffy brown mass is left. The synthesized BFMO and BCFO powders of particular doping concentration are mixed with 5 wt% poly-vinyl alcohol as binder in order to get the 1-inch diameter pellets. The final for deposition is prepared by sintering of these pellets is done at 800 o

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C for 1 hour in temperature-controlled muffle furnace (Nabertherm programmable furnace).

Thin films of Mn doped BFO (BFMO) and Ce doped BFO (BCFO) thin films of 100 nm have been deposited on Au coated quartz prisms using PLD technique. Detailed optimized parameters

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for the deposition of BFO, BCFO and BFMO thin films are tabulated in table 1. Table 1: Deposition parameters for preparation of BFO, BCFO and BFMO thin films. For BFO thin film

For BCFO thin film

For BFMO thin film

Targets

BFO

BCFO

BFMO

Pressure

0.133 mbar

0.133 mbar

0.133 mbar

Laser energy

1.5 J/cm2

1.5 J/cm2

1.5 J/cm2

Gas composition

100% O2

100% O2

100% O2

Target to substrate distance

4.5 cm

4.5 cm

4.5 cm

Thickness

100 nm

100 nm

100 nm

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Deposition Parameters

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600 oC

Substrate temperature

600 oC

600 oC

The SPR responses for all the prepared thin films i.e. BFO, BFMO and BCFO thin films were recorded using the prism/Au/BFO, prism/Au/BFMO and prism/Au/BCFO systems respectively

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using angular interrogation method. Fresnel’s equations were used to fit the obtained SPR reflectance data to estimate the values of refractive index and dielectric constant for BiFeO3 thin films at a wavelength, λ= 633 nm. For the development of SPR based magnetic field sensor under

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transverse MOKE (TMOKE) configuration, the optimized multiferroic BFMO thin film deposited on prism/Au substrate is used as a sensitive layer in the present study. An external magnetic field

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was applied parallel to the BFMO thin film surface and in a perpendicular direction to the plane of incidence to make a TMOKE configuration (figure 1). The magnitude of applied magnetic field was varied from 0 to 0.1 T by taking the two magnets distant from each other. The value of the applied magnetic field was measured using a gauss meter. A change in intensity of reflected light

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occurs which is related to the component of magnetization vector which is in perpendicular direction to the plane of incidence [29]. Thus, TMOKE using SPR technique can be used to study

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the change in the intensity of SPR reflected light with respect to the applied magnetic field.

Figure 1: (a) Description of transverse MOKE (TMOKE) configuration, and (b) Schematic of the experimental setup. Results and discussion

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SPR reflectance study Figure 2 depicts the SPR reflectance data observed for the present prism/Au/BFO/air, prism/Au/BFMO/air and prism/Au/BCFO/air systems. The SPR dip angle was found to shift to

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lower values i.e. from 46.7o to 40.7o by changing the dielectric layer from BFO to BFMO thin films and from 40.7o to 39.1o with BFMO to BCFO thin films. The shift in SPR curves is due to change in the dielectric properties of the deposited thin films on Au coated prisms. Furthermore,

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the BFMO based SPR structure (prism/Au/BFMO/air) has the lowest FWHM (or sharpest SPR reflectance curve) as compared to SPR reflectance curves obtained for other structures. FWHM of

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SPR curve is directly related to the absorption losses in the dielectric (BFMO) thin film, which got drastically reduced for the BFMO film deposited at a pressure of 0.1 mbar. Hence, BFMO thin film has been efficiently exploited for further sensing applications based on magnetic field.

0.90 0.85

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Reflectance

0.95

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1.00

0.80

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0.75 0.70

0.65 25

Figure 2:

Theoretical prism/Au/BFO/air prism/Au/BFMO/air prism/Au/BCFO/air

30

35

40 Angle(°)

45

50

55

Experimental SPR reflectance curves observed for the prepared prism/Au/BFO/air, prism/Au/BFMO/air and prism/Au/BCFO/air systems along with theoretical fitting

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Theoretical fitting of experimental SPR reflectance curves using Fresnel’s equations resulted in evaluating the values of complex dielectric constant (εi) and refractive index (ni). The detailed Fresnel’s equations have been explained in our previous work [30]. The values of reflectance

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versus incident angle were obtained by using well known Fresnel’s equation by fixing the thicknesses of Au and BFO thin films at 40 nm and 100 nm respectively. Another parameter used to simulate the SPR reflectance curves is complex dielectric constant of Au thin film which is

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obtained by fitting the experimental SPR curve for prism/Au/air system with Fresnel’s equations [30]. The values of dielectric constants and refractive index obtained for BFO thin film are 5.27+

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i0.09 and 2.29 + 0.019i respectively. Similarly, the values of dielectric constants and refractive index evaluate for BFMO thin film are 5.66+ i0.178 and 2.28 + 0.038i respectively. The values of dielectric constants and refractive index obtained for BCFO thin film are 5.09+ i0.017 and 2.25 + 0.039i respectively. The estimated values of dielectric constants and refractive index were found to

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in agreement to the corresponding values reported in literature [18, 31]. Prism/Au/BFMO/air based SPR magnetic field sensor Since, BFMO thin film grown at 0.1mbar shows the sharpest SPR reflectance curve (figure 2), the

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same film is used for realization of SPR based magnetic field sensor. The effect of external applied

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magnetic field on the prism/Au/BFMO/air SPR reflectance data are shown in figure 3 (a).

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50

1.00

0.79

0.80

10 15 20 25 30 35 40 45 50 55 60 65 Angle(°)

0.76

35

0.75 0.74

30

0.73

25

0.00

0.02

0.04

0.06

0.08

0.10

0.72

Magnetic field (T)

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0.75

0.77 40

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Reflectance

Theoretical 0T 0.02 T 0.04 T 0.06 T 0.1 T

0.85

45

Minimum Reflectance

0.90

SPR dip angle (θ SPR) (° )

0.78

0.95

(a)

(b)

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Figure 3: (a) Reflectance curves observed for Prism/Au/BFMO/air SPR sensor with magnetic field (0 to 0.1T) and (b) Plots of θSPR and minimum reflectance with magnetic field (0 to 0.1 T) As indicated by the SPR spectra a continuous shift was observed due to the applied magnetic field towards the decreasing value along with the consequent increase in FWHM (figure 3 (a)). The variation in θSPR and corresponding minimum reflectance for BFMO thin film as a function of

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varying magnetic field strength is plotted in figure 3 (b). The value of θSPR for BFMO thin film was found to decrease linearly from 40.8° to 26.6° with magnetic field (figure 3 (b)). This variation with magnetic field is related to the magneto-optic coupling between the ferromagnetic domains of

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the MO-layer and surface plasmon wave vector (SPW). This further leads to change in the SPW

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propagation constant causing a shift in resonance position. The value of sensitivity obtained from the caliberation curve i.e. linear variation of θSPR with magnetic field (figure 3 (b)) is about 147 °/ Tesla. The obtained value of sensitivity for BFMO based sensor is very high in comparison to the sensitivity obtained for undoped BFO thin film-based sensor (46.4 o/Tesla) as discussed in our previous report [28]. There is a linear dependence of θSPR on magnetic field with a sensitivity of about 147 °/ Tesla (∼0.0147 °/Gauss) which is reproducible, clearly demonstrates that the

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prism/Au/BFMO/air system finds its potential application for highly sensitive magnetic field sensor. The SPR curves were fitted using modified fresnel’s equations shown by solid lines in figure 3 (b), +

′) and magneto-optic constant Q (Q′+ iQ″)

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while considering complex dielectric constant (

of BFMO film as fitting parameters are also shown in figure 4 (a) [32]. The significance of the high Q value indicates the efficient magneto-optic coupling i.e. appreciable variation in optical

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properties of FM (BFMO) thin film with small change in the magnitude of magnetic field. The value of real part of magneto-optic constant Q (Q′) of BFMO thin film was found to vary from

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0.008 to 0.076 with increase in magnetic field from 0.02 to 0.1 T as obtained from perfect fitting of data. However, the value of the imaginary part of Q (Q″) is very small and was found to vary from 0.5 x 10-3 to 1 x 10-3 with magnetic field varying from 0.02 to 0.1 T. The fitted values of real and imaginary part of dielectric constant and the corresponding values of n and k for BFMO thin films

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are plotted in figure 3.19 (a) and (b) respectively versus applied magnetic field. The values of and n show a linear decrease from 5.66 to 5.11 (figure 4 (a)) and 2.38 to 2.26 (figure 4 (b)) respectively as the magnitude of applied magnetic field varies from 0 to 0.1 T. However, the

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dielectric loss (ε″) and extinction coefficient ( ) shows a very small change (ε″= 0.178 to 0.183 in

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figure 4 (a)) and (k=0.038 to 0.0394 in figure 4 (b)) with magnetic field from 0 to 0.1 T. The observed results suggest that the developed SPR optical sensor (prism/Au/BFMO/air) is highly sensitive to magnetic field. A small variation in external magnetic field is clearly reflected as the corresponding change in the value of refractive index of BFMO thin film (figure 4 (b)), along with change in θSPR (figure 3 (b)). The sensitivity calculated from the calibration curve for refractive index versus applied magnetic field (figure 4 (b)) is about 1.15 RIU/Tesla.

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0.0420

0.190 5.6

2.37

0.0410

2.31

5.4 0.186

0.0400

2.25

0.0395

2.22 0.182

4.8 0.180

4.6

2.19

0.0390

2.16

0.0385

2.13 0.178 0.02 0.04 0.06 0.08 Magnetic field (T)

0.10

0.00

0.02

0.04

0.06

0.08

0.10

Magnetic field (T)

(a)

(b)

Variation in (a) ε and ε , and (b) n and k for BFMO thin film obtained at a

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Figure 4:

0.0380

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0.00

2.10

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5.0

n

ε′

0.184

0.0405

2.28

k

ε″

5.2

4.4

0.0415

2.34

0.188

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wavelength λ = 633 nm with varying applied magnetic field.

Conclusion

In the present work, SPR optical sensor for detection of magnetic field has been developed using

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magneto-optic Kerr effect (MOKE) in multiferroic films. Pulsed Laser Deposited (PLD) technique has been used to deposit BFO, Mn-doped BFO and Ce- doped BFO thin film. The optical

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properties of the prepared films were observed using SPR technique. 10% Mn is doped in BFO (BFMO) thin film to enhance the sensitivity of SPR sensor towards magnetic field giving sharp SPR curve with minimum loss. The developed prism/Au/BFMO/air sensor exhibits more shift in θSPR (sensitivity ≈ 147°/Tesla) in comparison to that of BFO (sensitivity ≈ 46.4°/Tesla), indicating its potential as an efficient magnetic field sensor. Acknowledgements

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Authors are thankful to Department of Science and technology (DST), Govt. of India and University of Delhi for financial support.

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Highlights Observed the optical properties of pulsed laser deposited single phase BiFeO3, Mn doped BiFeO3 (BFMO) and Ce doped BiFeO3 (BCFO) thin films •

Magnetic field dependence on the optical properties of BFMO thin films have also been determined using SPR.

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A very sensitivity of 147 °/Tesla was found for the prism/Au/BFMO structure exhibiting

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maximum change in optical properties with magnetic field.

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•

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•