Comparative trial of saccharin-added electrolyte for improving the structure of an electrodeposited magnetic FeCoNi thin film

doi:10.1016/j.tsf.2017.09.017

Thin Solid Films

Volume 642, 30 November 2017, Pages 51-57

https://doi.org/10.1016/j.tsf.2017.09.017 Get rights and content

Highlights

•
Thin film of FeCoNi alloy was successfully deposited on a flexible substrate.
•
The alloy was pure-phase of ternary solid solution of nanocrystalline FeCoNi.
•
Saccharin reduced crystallite size and modified the FeCoNi composition.
•
A very low coercivity film was obtained from electrolyte containing saccharin.

Abstract

Magnetic thin films composed of FeCoNi alloy nanocrystals were electrodeposited on an indium tin oxide-coated polyethylene terephthalate sheet from sulfate electrolyte in the presence of saccharin. The resultant films were characterized by several analytical techniques, including X-ray diffraction, transmission electron microscopy (TEM), scanning TEM, X-ray photoelectron spectroscopy, and superconducting quantum interference device magnetometer. Microstructural analyses confirmed the formation of pure-phase ternary solid solutions of face-centered cubic FeCoNi. Saccharin was found to play an important role in controlling the crystallite size, composition, and morphology of the FeCoNi film that influenced the magnetic properties of the film. The FeCoNi film exhibited excellent soft magnetic behavior at room temperature with a relatively high saturation magnetization.

Introduction

FeCoNi alloy exhibits excellent soft magnetic properties, namely, low coercivity, high saturation magnetization, and high permeability [1], [2], [3]. It also shows good microwave absorption properties [4], [5], high corrosion resistance [3], and thermal stability [6]. Therefore, FeCoNi films can potentially be employed for high frequency inductors [7], transformers [8], micromagnetic sensors [3], and absorber or electromagnetic interference shielding [1], [2]. Many attempts on the synthesis of FeCoNi films using different techniques, such as chemical vapor deposition [9], sputtering [10], electrospinning [11], electroless deposition [5], and electrodeposition [12], [13], have been reported because of their potential applications. Among them, electrodeposition has become a promising technique to synthesize FeCoNi as nanostructured thin films exhibiting many advantages in productivity as well as in practical and low-cost processes. Electrodeposition is also recognized as a versatile approach that enables the fabrication of metal-based films with desired properties by modifying deposit growth orientation through the adjustment of electrodeposition conditions.

In the last two decades, electrodeposition of FeCoNi ternary alloy films has been conducted on various substrates, such as sputtered Cu/Ti/Si [14], Ta/Fe/Co-coated glass or SiO₂ wafer [1], titanium [12], CuBe wire [15], and Cu-coated Si wafer [13]. However, the current development in electronic devices demands very thin magnetic films that are mechanically flexible, durable, lightweight [16], [17], and applicable to uneven surface. This development refers to the so-called flexible electronics, which is a technology used for the fabrication of electronic circuits or devices on bendable substrates [18]. Therefore, the fabrication technique for a metal magnetic thin film on a flexible substrate has become one of the keys for the realization of the many functionalities of flexible devices [19]. However, reports on the preparation of magnetic FeCoNi thin films on flexible substrates have been very limited.

In this study, the FeCoNi thin film was directly electrodeposited onto a flexible substrate, i.e., a polyethylene terephthalate (PET) sheet coated with a conductive layer of indium tin oxide (ITO). The FeCoNi film was grown on the ITO-coated PET substrate at room temperature by controlling the co-deposition potential using a one-step potentiostatic deposition approach. The magnetic properties of the films were investigated, and the effects of the change in the composition and microstructure of the alloy were reported. Saccharin was added to the electrolyte as a structure-controlling agent. The use of saccharin has been known to be effective in enhancing the microstructure and smoothing the surface of the deposited material [20]. As previously investigated, the presence of saccharin can increase the cathodic overpotential in the electrochemical system that increases the nucleation rate during the deposition process, thus resulting in grain refinement and reduced internal and residual stress in some metal and alloy deposits such as Zn [21], ZnNi [22], and CoNi [23].

Section snippets

Experimental

FeCoNi thin films were electrodeposited on ITO-coated PET substrates with a thickness of 125 nm and sheet resistance of 10 Ω/sq supplied by Kintec Company (Hong Kong). Before each electrodeposition, the substrates were rinsed with ethanol and double-distilled water and then dried with high-purity nitrogen (N₂) gas. As the source of metal ions, sulfate electrolytes were freshly prepared using analytical grade chemicals purchased from Merck: FeSO₄·7H₂O, CoSO₄·7H₂O, NiSO₄·6H₂O, and H₃BO₃. The

Results and discussion

XRD patterns of the FeCoNi thin films electrodeposited from both electrolytes (el1 and el2) are shown in Fig. 1. The XRD patterns show that both films are composed of the face-centered-cubic (fcc) phase of the FeCoNi alloy. This phase is indicated by the observed peaks at 2θ = 44.34°, 51.81°, 76.24°, 92.86°, and 98.02°, which represent the Bragg reflections of the (111), (200), (220), (311), and (222) planes of the fcc FeCoNi phase, respectively. These XRD patterns agree well with the fcc CoNi

Conclusion

Thin films of nanocrystalline FeCoNi alloy were synthesized on flexible PET-coated ITO layer substrates using the electrodeposition technique. Phase and structure analyses of XRD and SAED patterns showed that a polycrystalline FeCoNi with an fcc structure and a fine crystallite size was successfully grown on the substrate. Elemental mapping at high magnification conducted using STEM-EDS revealed a homogenous distribution of the Fe, Co, and Ni over the analysis area, thus supporting the XRD

Acknowledgment

This work was financially supported by Universitas Negeri Jakarta and Directorate General of Higher Education Republic of Indonesia through the PPT research grant number 11/SP2H/DRPM/LPPM-UNJ/IV/2017 and sandwich-like scholarship, respectively. The authors are grateful to the Japan Advanced Institute for Science and Technology, especially to the Maenosono Laboratory, for providing us with access to the characterization equipment facilities during the sandwich-like program.

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Comparative trial of saccharin-added electrolyte for improving the structure of an electrodeposited magnetic FeCoNi thin film

Highlights

Abstract

Introduction

Section snippets

Experimental

Results and discussion

Conclusion

Acknowledgment

J. Alloys Compd.

Inorg. Chem. Commun.

J. Alloys Compd.

J. Magn. Magn. Mater.

Electrochem. Commun.

J. Magn. Magn. Mater.

J. Magn. Magn. Mater.

Appl. Surf. Sci.

Colloids Surf. A Physicochem. Eng. Asp.

Mater. Chem. Phys.

Appl. Surf. Sci.

Prog. Mater. Sci.

J. Magn. Magn. Mater.

Electrodeposition of granular FeCoNi films with large permeability for microwave applications

J. Mater. Chem.

Evolution study of microstructure and electromagnetic behaviors of Fe-Co-Ni alloy with mechanical alloying

Mater. Sci. Eng., B

A soft magnetic CoNiFe film with high saturation magnetic flux density and low coercivity

Nature

Characterization and microwave resonance in nanocrystalline FeCoNi flake composite

J. Appl. Phys.