Effect of Saccharin and Sodium Dodecyl Sulfate Additives on the Structural and Morphological Properties of Ni-Fe Coatings

Abstract

This study systematically investigates the synergistic effects of saccharin and sodium dodecyl sulfate (SDS) additives on the structural and morphological properties of electrodeposited Ni-Fe coatings. Copper substrates were electroplated in a sulfate-chloride electrolyte under controlled conditions (pH 5.5, 1 A/dm², 10 min), with saccharin (0–0.5 g/L) and SDS (0–0.9 g/L) concentrations varied to optimize coating performance. Comprehensive characterization via SEM, XRD, and crystallite size analysis revealed that saccharin significantly refines grain structure, achieving minimal crystallite size (25 nm) and optimal surface homogeneity at 0.33 g/L. Conversely, SDS (0.4–0.6 g/L) reduced grain size to 18 nm but induced porosity and roughness at higher concentrations (0.9 g/L) due to hydrogen evolution. XRD analysis further demonstrated that SDS modulates phase homogeneity, suppressing secondary Ni-Fe alloy formation at elevated concentrations. The combined additives promoted (111)-oriented face-centered cubic (FCC) growth, enhancing microstructural integrity. Optimal parameters 0.33 g/L saccharin and 0.4–0.6 g/L SDS yielded coatings with refined grains, reduced internal stresses, and improved corrosion resistance. These results provide critical insights for tailoring high-performance Ni-Fe coatings in magnetic and anti-corrosion applications.

Keywords:
Electrodeposition; Ni-Fe coatings; Saccharin; Sodium Dodecyl Sulfate (SDS); Morphology; Grain refinement; Phase orientation

1. Introduction

Ni-Fe alloys are increasingly utilized in applications demanding high magnetic performance and corrosion resistance, such as data storage, electronic components, and memory systems. The efficiency and durability of these coatings are influenced by key factors, including surface morphology, crystallographic structure, and internal stresses, all of which are governed by electrodeposition parameters and additive selection. Additives like saccharin and Sodium Dodecyl Sulfate (SDS) have proven beneficial in enhancing these properties.

Saccharin is recognized for its grain refinement capabilities, which reduce internal stresses and lead to a finer grain structure, ultimately improving surface quality and coating durability. In parallel, SDS acts as a surfactant that stabilizes particles, modifies surface morphology, and enhances corrosion resistance by promoting a uniform distribution of particles across the coating. Together, these additives play a vital role in improving the structural and functional characteristics of Ni-Fe coatings.

Previous research has demonstrated that incorporating saccharin and SDS into Ni-based alloy electrodeposition significantly improves microstructure, hardness, corrosion resistance, and tribological properties. Saccharin, often employed to relieve stress and enhance morphology, has been shown to reduce crack formation and refine grain size in Ni-based alloys. Adjustments in saccharin concentration, especially between 2 and 4 g/L in Ni-WP alloys, optimize wear and corrosion resistance under high rotational conditions¹. Similar benefits in hardness and grain size reduction have been achieved in Ni-Fe alloys with saccharin levels up to 8 g/L, yielding finer, more robust microstructures².

Additionally, the tensile and fracture resistance of nanocrystalline Ni-Fe alloys benefit from saccharin, which enhances plasticity and strengthens grain boundaries to prevent intergranular crack propagation³. Saccharin also influences growth mechanisms in Ni - Fe alloy films, creating smoother surfaces under direct and pulse currents, although pulse-reverse currents result in rougher textures due to inhibited vertical grain growth⁴.

SDS serves as an essential surfactant in nickel-based composites by promoting uniform particle distribution and reducing friction, which improves coating consistency and tribological properties. In SDS-enhanced CNT/Ni composite layers, optimized concentrations refine grain structure, alter crystal orientation, and lower friction coefficients, making these coatings smoother and more durable⁵,⁶. Saccharin has also shown success in Ni-Zn alloys, where it boosts corrosion resistance and reduces friction, further contributing to coating longevity⁷.

In magnetic applications, coatings like Ni-Co-Fe benefit from saccharin’s grain refinement, which enhances magnetic properties such as reduced coercivity (Hc) and increased saturation magnetization (Ms)⁸,⁹. Saccharin not only boosts mechanical properties but also optimizes film texture and crystallographic orientation, which is crucial for electronic applications¹⁰. In particular, the role of saccharin in NiFeCu alloy coatings yields FCC structures with preferred orientations, aligning with superior magnetic properties¹¹.

Further studies reveal that incorporating elements like Cu and ZrO₂ into Ni-based alloys improves structural integrity and corrosion resistance, where both saccharin and SDS contribute to these enhancements. For instance, Li et al.¹² demonstrated that including Cu and ZrO₂ in Ni matrix coatings produced finer textures and higher hardness, attributed to the effect of SDS on the deposition process¹³-¹⁵. Additionally, saccharin has shown to improve crystallite size and morphology in FeCoNi thin films, enhancing their magnetic performance by reducing magnetic anisotropy and improving soft magnetic properties¹²,¹⁶.

Recent studies have demonstrated significant advancements in the development of corrosion-resistant alloy coatings through electrodeposition techniques. Bhat et al.¹⁷ developed Zn–Ni monolayer and compositionally modulated multilayer alloy coatings on mild steel using acidic sulphate baths, optimizing current density and layer count to achieve coatings with up to 65 times greater corrosion resistance than single-layer counterparts, as confirmed by potentio dynamic polarization and electrochemical impedance spectroscopy. Similarly, Bhat et al.¹⁸ explored Zn-Fe alloy coatings, finding that multilayer coatings with 300 layers deposited at 2.0/3.0 A dm⁻² exhibited up to five times higher corrosion resistance than single-layer coatings, with microhardness increasing with applied current densities, making them particularly valuable for automotive applications. In another study, Bhat et al.¹⁹ investigated Zn-Ni alloy coatings using a sulphate bath, demonstrating superior corrosion resistance (0.213 mm y⁻¹) at an optimal current density of 3 A dm⁻², with surface roughness and topography analyzed via atomic force microscopy (AFM) and scanning electron microscopy (SEM). Additionally, Bhat et al.²⁰ optimized a sulfate bath for Zn-Ni electroplating on mild steel, achieving a corrosion resistance of 8.62 μA cm⁻² at 4 A dm⁻², with nickel content verified through colorimetric and energy-dispersive X-ray (EDX) analyses. Furthermore, Bhat (2021) fabricated Zn-Fe multilayer coatings using square current pulses, achieving a 43-fold improvement in corrosion resistance for 300-layer deposits compared to monolayers, attributed to phase structure variations and validated through SEM and AFM analyses, highlighting their industrial applicability in defense, machinery, and automotive sectors²¹. These studies collectively underscore the importance of optimizing electrodeposition parameters and multilayer designs to enhance the corrosion resistance and mechanical properties of alloy coatings for industrial applications.

This study uniquely investigates the combined influence of saccharin and SDS on the structural, morphological, and magnetic properties of Ni-Fe coatings, which has not been extensively explored in prior research. While previous studies have examined the effects of these additives individually, this work provides a comprehensive analysis of their synergistic effects, particularly in optimizing grain refinement, surface morphology, and corrosion resistance. Additionally, we identify optimal concentration ranges for both additives (0.33 g/L for saccharin and 0.4–0.6 g/L for SDS), offering practical insights for industrial applications.

2. Methodology

2.1. Preparation of Ni-Fe coating on copper substrates

Copper substrates measuring 10x20 mm² were prepared through a meticulous multi-step process to achieve an optimal surface for coating. Initially, the substrates were polished mechanically with silicon carbide (SiC) abrasive papers of varying grits (from 120 up to 4000), providing a uniformly smooth base. After polishing, each substrate was rinsed with distilled water and degreased in an alkaline solution containing 50 g/L of Na₂CO₃ and 15 g/L of NaOH. Following this degreasing step, a 10% HCl treatment was applied to remove any remaining oxides, and a final rinse in distilled water was performed to ensure the removal of all surface impurities before proceeding to electrodeposition.

For the electrochemical deposition of the Ni-Fe coating, a dual-anode configuration was employed. As illustrated in Figure 1, each copper substrate was positioned between two nickel anodes, both kept parallel to the substrate and at a consistent distance of 1 cm. This arrangement promoted uniform, double-sided plating, allowing for even deposition on both sides of the copper substrate.

Figure 1
Schematic Representation of the Ni-Fe Electrodeposition Setup.

The electrolyte solution was carefully prepared with the following specifications:

9.46 g/L of nickel sulfate hexahydrate (NiSO₄·6H₂O), 25.09 g/L of ammonium iron(II) sulfate hexahydrate ((NH₄)₂Fe(SO₄)₂·6H₂O), 5 g/L of sodium chloride (NaCl), and 6 g/L of boric acid (H₃BO₃).

To examine the effects of specific additives on coating quality, saccharin and SDS were introduced at various concentrations. Saccharin was tested at 0, 0.06, 0.33, and 0.5 g/L, while SDS concentrations were adjusted to 0, 0.4, 0.6, and 0.9 g/L.

• Electrolyte temperature: Room temperature.

• Stirring rate: 200 rpm.

• pH: 5.5 ± 0.1.

• Deposition time: 10 minutes.

• Current density: 1A/dm².

• Estimated layer thickness: 10 ± 2 nm.

2.2. Characterization techniques

• SEM Analysis: Surface morphology was characterized using environmental scanning electron microscopy (SEM) (FEI QUANTA 200). Analysis focused on assessing surface smoothness, grain distribution, and the impact of various additive concentrations.

• XRD Analysis: X-ray diffraction (XRD) was performed using a Mini Flex 600, with a 2θ scan range from 30° to 90° at 0.040° increments. Crystallite size calculations were based on the Debye-Scherrer Equation 1:

  $D=\frac{k\lambda }{\beta cos\theta }$(1)

Where k is the Scherrer constant, λ is the wavelength of X-ray (CuKα radiation, λ = 1.54059 Å), β is the full width at half maximum (FWHM), and θ is the Bragg angle.

2.3. Adhesion and surface morphology tests

To evaluate adhesion quality, samples were subjected to a heating process at 250 °C for 30 minutes, followed by immersion in water. SEM coupled with energy-dispersive X-ray (EDX) analysis was conducted to examine variations in crystalline phases and preferred growth orientations.

3. Results and Discussion

3.1. Influence of SDS on Ni-Fe coating morphology

Figure 2 presents the X-ray diffraction (XRD) patterns of Ni-Fe coatings electrodeposited at SDS concentrations of 0, 0.4, 0.6, and 0.9 g/L. The X-ray diffraction (XRD) patterns revealed that the electrodeposited coatings are complex composites whose microstructure is significantly influenced by the dodecyl additive concentration. All samples exhibited a multi-phase structure. The primary metallic component consists of two distinct face-centered cubic (FCC) phases: a Nickel-rich phase, identified by the intense (111) peak at 2θ ≈ 44.6°, and a secondary Ni-Fe alloy phase, with its (111) peak shifted to a lower angle of 2θ ≈ 43.7°. This phase separation suggests a non-homogeneous incorporation of iron into the nickel lattice. Furthermore, a non-metallic secondary phase, identified as beta-nickel hydroxide (β-Ni(OH)₂), was consistently detected via its (101) peak at 2θ ≈ 38.4°, arising from the localized pH increase at the cathode.

Figure 2
XRD diffractograms of Ni-Fe coatings with varying SDS concentrations (a) 0 g/L, (b) 0.4 g/L, (c) 0,6 g/L. (d) 0.9 g/L.

The dodecyl additive was found to critically modulate this complex microstructure in two ways. Firstly, it controlled the phase homogeneity of the metallic deposit. At high concentrations (1.35 g/L), the formation of the secondary Ni-Fe alloy phase was almost completely suppressed, leading to a more homogeneous Ni-rich coating

Figure 3 quantifies the relationship between SDS concentration and crystallite size, derived from XRD data using the Debye-Scherrer equation. Crystallite size decreases sharply from 32 nm (0 g/L SDS) to 18 nm at 0.6 g/L SDS, followed by a slight increase to 22 nm at 0.9 g/L SDS. The initial reduction (0–0.6 g/L) is due to SDS adsorption, which suppresses grain coalescence by limiting ion mobility. At 0.9 g/L, excessive SDS induces hydrogen evolution, destabilizing the deposition process and causing irregular grain growth. This non-monotonic trend highlights the dual role of SDS: a grain refiner at moderate concentrations (0.4–0.6 g/L) and a disruptor at higher levels. The optimal SDS range (0.4–0.6 g/L) corresponds to the smoothest morphology in Figure 4, where smaller grains enhance corrosion resistance via dense grain boundaries and passive oxide layer formation.

Figure 3
Crystallite size variation in relation to SDS concentration.

Figure 4
SEM images of Ni-Fe coatings at different SDS concentrations (0, 0.4, 0.6, and 0.9 g/L).

3.2. Grain Size and morphological adaptations with SDS concentration

SEM imaging (Figure 4) demonstrates the correlation between SDS concentration and surface morphology. At lower SDS levels (0–0.4 g/L), the coating surface appears smooth with minimal porosity. However, as SDS concentration rises to 0.6 g/L and beyond, increased surface roughness and porosity become evident. This roughening is linked to hydrogen evolution, which disrupts coating uniformity at higher SDS levels. At higher SDS concentrations (0.6–0.9 g/L), increased porosity enhances corrosion resistance by promoting the formation of a passive oxide layer, which acts as a barrier to further corrosion.

An optimal SDS concentration range of 0.4–0.6 g/L was identified, where the coating achieves a balanced structure with minimal porosity and smooth morphology. Excessive SDS concentrations, as observed at 0.9 g/L, lead to increased surface roughness and a porous, less dense structure.

3.3. Influence of saccharin on Ni-Fe coating properties

SEM analysis (Figure 5) of coatings with saccharin reveals a progressive improvement in surface smoothness and grain refinement with increasing saccharin concentrations. At 0.33 g/L saccharin, optimal coating quality is achieved, with a homogenous, smooth surface and minimal internal stress. Higher concentrations (0.5 g/L) result in slight roughness, with localized "islands" due to over-refinement, potentially impacting structural uniformity.

Figure 5
SEM images of Ni-Fe coatings with varying saccharin concentrations (0, 0.06, 0.33, and 0.5 g/L).

3.4. Crystallographic analysis with varying saccharin concentrations

Figure 6 shows the XRD spectra of coatings electrodeposited with saccharin concentrations of 0, 0.06, 0.33, and 0.5 g/L. The effect of saccharin concentration on the crystal orientation of Ni–Fe coatings was systematically investigated using X-ray diffraction (XRD). As saccharin concentration decreased from 0.1 g to 0.03 g, a notable improvement in peak symmetry and distribution was observed. The sample with 0.03 g saccharin exhibited a balanced crystallographic texture with intense reflections from the (111), (200), and (630) planes, suggesting a refined grain structure and homogenous growth. In contrast, the 0.075 g sample showed dominant growth along the (200) plane, indicating strong preferred orientation but reduced overall crystallinity. The appearance of pure Ni phases in all compositions, especially at 0.1 g, points to selective deposition behavior influenced by saccharin as a leveling agent. Therefore, the 0.03 g concentration provides an optimal balance between crystallinity and surface uniformity, rendering it the most favorable condition for engineering high-performance Ni–Fe electrochemical coatings.

Figure 6
XRD spectra of Ni-Fe coatings at different saccharin concentrations, (a) 0 g/L, (b) 0.06 g/L, (c) 0.33 g/L (d) 0.5 g/L.

3.5. Crystallite size analysis with saccharin concentrations

Figure 7 plots crystallite size as a function of saccharin concentration, revealing a steep decline from 36 nm (0 g/L) to 25 nm (0.33 g/L), followed by a minor increase to 28 nm (0.5 g/L). This trend reflects saccharin’s saturation effect: at 0.33 g/L, molecules adsorb uniformly, enabling homogeneous nucleation and ultra-fine grains. Beyond this threshold, molecular aggregation disrupts adsorption, reducing refinement efficacy. The minimal crystallite size at 0.33 g/L correlates with the optimal smoothness in Figure 5, where coatings exhibit a defect-free, homogenous morphology. These ultra-fine grains enhance mechanical properties (e.g., hardness and wear resistance) but may compromise ductility due to increased grain boundary density. The results underscore saccharin’s superiority in achieving nanocrystallinity but emphasize the necessity of strict concentration limits for industrial applications.

Figure 7
Crystallite size vs. Saccharin concentration.

4. Conclusion

This study demonstrates the critical role of saccharin and SDS in tailoring the structural and morphological characteristics of Ni-Fe coatings. Saccharin, at an optimal concentration of 0.33 g/L, effectively promotes grain refinement and reduces internal stresses, achieving a smooth and uniform surface with minimal imperfections. SDS, at concentrations between 0.6 g/L, modifying surface morphology, though excessive concentrations lead to increased porosity and roughness, compromising coating integrity. The findings highlight an optimal concentration range for both additives: saccharin at 0.33 g/L and SDS between 0.4–0.6 g/L. These conditions promote refined grain structures, stable phase orientations, and improved mechanical integrity, making them suitable for industrial applications that demand robust coatings with fine-tuned morphological properties. By precisely adjusting saccharin and SDS concentrations, manufacturers can achieve specific performance requirements for Ni-Fe coatings in advanced electronic, magnetic, and anti-corrosive applications. Furthermore, the study validates the importance of additive optimization in electrodeposition processes, providing a framework for future research on the synergistic effects of additives in alloy coatings. These insights offer valuable guidance for industries aiming to enhance the durability.

• DATA AVAILABILITY
  The full dataset supporting the findings of this study is available upon request to the corresponding author, Farid Lekmine, at [e-mail].

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Edited by

• Associate Editor:
  Ana Sofia de Oliveira.

• Editor-in-Chief:
  Luiz Antonio Pessan.

Data availability

The full dataset supporting the findings of this study is available upon request to the corresponding author, Farid Lekmine, at [e-mail].

Publication Dates

• Publication in this collection
  03 Nov 2025
• Date of issue
  2025

History

• Received
  19 Feb 2025
• Reviewed
  28 July 2025
• Accepted
  21 Sept 2025