The amorphous phase of Co₆₇Si₂₃B₁₀ alloy produced by mechanical alloying

ABSTRACT

In this work, the evolution and formation of the amorphous phase during the preparation of amorphous Co₆₇Si₂₃B₁₀ (at.%) powder by mechanical alloying (MA) under an argon atmosphere were studied. The grinding time of 15 h had a profound effect on the phase transformation, microstructure, morphology development, and thermal and magnetic behavior of the powders. These effects were studied by X-ray diffraction (XRD), EDX scanning electron microscopy (SEM), thermal analysis (TGA/DTA), N₂ texture analysis (BET/BJH) and, magnetic measurements (VSM). The results show that the evolution of the amorphous phase in the early stage of milling consists of nanocrystalline α-Co₂B and β-Co₂Si phases, which are diluted and coexist with the amorphous phase. After 15 hours of ball milling, the amorphous phase became the main phase with a proportion of 98.1%, which is relatively high compared to the 1.9% of the nanocrystalline phases α-Co₂B and β-Co₂Si. The results obtained indicate that amorphization develops with higher thermal stability than a small fraction of the nanocrystalline phase diluted in the amorphous phase. This behavior suggests the presence of the amorphous phase coexisting with the nanocrystalline phase in a small fraction with overlapping crystallization and recrystallization at a temperature of around 924.42°C.

Keywords:
amorphous phase; Co₆₇Si₂₃B₁₀ powder; mechanical alloying (MA)

1. INTRODUCTION

Amorphous alloys are a unique class of materials characterized by a lack of long-range structural order ordering while retaining short-range chemical ordering, and they giving them a series of superior physical properties compared to their polycrystalline counterparts [¹, ²] . Amorphous alloys also have practical applications due to their unique magnetic properties [³], good mechanical behavior [⁴], and high corrosion resistance [⁵], making them suitable for a variety of industrial applications in fields such as energy [⁶], aeronautics, chemistry [⁷], and orthopedic biomaterials [⁸].

The Co-based amorphous alloys exhibit near-zero magnetostriction and magnetocrystalline anisotropy [⁹], giving them outstanding soft magnetic properties such as low coercivity [¹⁰], high permeability [¹¹], low hysteresis losses [¹²], lower saturation induction and high mechanical strength compared to their crystalline counterparts [¹³]. This is due to the relatively large amount of metalloid atoms present in their composition. Metalloid elements (B, Si, P, C, and Ge) in order to understand their effects on the atomic structure, glass formation ability (GFA), thermal stability, and magnetic properties of Co-based amorphous alloys [¹⁴, ¹⁵]. Over the years, several synthesis routes have been used to produce amorphous soft magnetic materials, including melt spinning [¹⁶], gas atomization [¹⁷], mechanical alloying [¹⁸], copper mould casting [¹⁹], vapour deposition [²⁰], and plasma processing [²¹].

Mechanical alloying (MA) is an alternative process for producing amorphous alloys from either a mixture of pure elemental powders [²²]. MA offers several advantages over traditional casting or rapid solidification methods. Mechanically alloyed amorphous powders can be easily solidified into high-density amorphous bulk samples of any shape and size in a supercooled liquid region without the need for any post-processing processes such as mechanical processing [²³, ²⁴]. Furthermore, MA is versatile enough to allow amorphization over a composition range that is wider than that corresponding to rapid solidification and is close to the eutectic composition [²⁵, ²⁶].

A major advantage of the mechanical alloying route is that this technique can successfully produce amorphous materials in systems where conventional routes, such as melt spinning, fail or are difficult to achieve metallic alloy amorphization evolution [²⁷]. Different authors have demonstrated the effectiveness of mechanical alloying in promoting the amorphization of various Co-based alloys, such as Co–B [²⁸], Co–Si [²⁹], Co-Fe-Si-B-Nb [³⁰], Co-Fe-B-Si-Nb [³¹], Co–Ta–B [³²], and Co–Cr–Mo–Nb–B [³³]. On the other hand, the main disadvantage of the MA process is that the balls or milling media introduce impurities and grinding residues into the powder, which may affect the thermal stability and some physical properties of the amorphous powder [³⁴].

The amorphous phase formed by MA depends on the energy provided by the grinding media, the atomic size of the components, and the thermodynamic properties of the alloy system [³⁵]. Currently, two criteria are required for the formation of amorphous phases during MA processes in binary and ternary systems: (i) large negative mixing heats between the basic components and (ii) large asymmetries in elemental diffusion coefficients [³⁶]. The amorphous phase is kinetically formed when the amorphization reaction occurs much faster than the formation of the nanocrystalline and crystalline phases [³⁷]. It has also been shown that the introduction of crystal defects into the lattice during the MA process increases the internal energy [³⁸]. When the free energy of the crystal exceeds the free energy of the amorphous phase, the crystal structure becomes thermodynamically unstable and can transform into the amorphous phase [³⁹].

In this paper, we report on the preparation of Co₆₇Si₂₃B₁₀ (at. %) amorphous powder via a wet mechanical alloying (MA) route. The milling time of 15 h was required for alloy amorphization. The evolution of the morphological and microstructural characteristics of the powder, magnetic properties, and thermal stability of the powders are presented and discussed.

2. MATERIALS AND METHODS

Elemental metallic powders (99.9% purity, from Êxodo Científica − LTDA/Brasil) of Co, Si, and B with a nominal composition of Co₆₇Si₂₃B₁₀ (at. %) were mechanically alloyed using a planetary ball mill (Type Fritsch Pulverisette 5) under an Ar atmosphere (99.9% purity). To produce this alloy, 20 g of each batch metal powder was stoichiometrically weighed and placed in a grinding bowl made of hardened stainless-steel balls and vials, with seven balls (12 mm diameter), and subjected to a total milling time of 15 h. The mill speed was set at 350 rpm, and the ball-to-powder ratio (BPR) was kept at 20:1. Ethyl alcohol (C₂H₆O) from Sigma-Aldrich Brasil Ltda was used as a process control agent (PCA) to regulate the morphology of the homogenized powder. The microstructural evaluation of the samples obtained from the mechanical alloying was carried out by X-ray diffraction (XRD; BRUKER diffractometer, model D2 Phaser) using CuK_α (λ = 1.54056 Å) radiation produced at 45 kV and 40 mA. The diffraction angle (2θ) was ranging between 10° and 80° with a step size of 0.013°, and a time of 5 s.

Microstructural morphology and chemical composition of the powders milled was evaluated by scanning electron microscope (SEM; TESCAN VEGA3) equipped with the energy dispersive X-ray (EDX), operating at 30 kV with a magnification of 100 kx. In the EDX diagram, the Au element was detected, which was caused by the gold spraying treatment to the sample before the test. Thermal studies of the milled amorphous powder Co₆₇Si₂₃B₁₀ were collected after milling using differential thermal analysis (DTA) and thermogravimetric analysis (TGA) equipment from the brand SHIMADZU DTG-60H. All thermal studies were conducted under argon atmosphere with a heating rate of 10°C/min. Textural analysis was conducted using a Quantachrome NOVA 2200E BET surface area and pore size analyzer, model Autosorb IQ, to obtain adsorption/desorption isotherms of the amorphous alloy Co₆₇Si₂₃B₁₀. The uniaxial compressive mechanical tests were conducted on a WDW-100 testing machine at a strain rate of 4 10^–4 s^–1 at room temperature. The size of the Co₆₇Si₂₃B₁₀ powder pressed into a cylindrical disc shape is 2 mm in diameter and 4mm in height. The compression tests were performed at least in triplicate for the Co₆₇Si₂₃B₁₀ powder. Magnetic properties were studied by a vibrating sample magnetometer (VSM) at 25°C within a ± 40 kOe magnetic field range.

3. RESULTS AND DISCUSSION

Figure 1 displays the X-ray pattern of Co₆₇Si₂₃B₁₀ powder during milling time of 15 h. The diffraction pattern contains of a diffuse halo that includes the amorphous phase and small two diffraction reflections corresponding to the nanocrystalline phases of the α-Co₂B and β-Co₂Si type [⁴⁰] in Figure 1.

Figure 1
XRD pattern of Co₆₇Si₂₃B₁₀ powder.

A broad diffusion peak near 2θ = 45º suggests the presence of an amorphous structure in the prepared Co₆₇Si₂₃B₁₀ powder, as illustrated in Figure 1 obtained by MA. The nanocrystalline α-Co₂B and β-Co₂Si phases showed a weak reflection that corresponds to 1.9%. It indicates that they are embedded in the amorphous matrix with a larger fraction of 98.1% in this phase. Thus, nanocrystals were formed under strain with an average size of 30 nm during the MA process of powder milling [⁴¹].

Figure 2 shows the SEM/EDS micrograph of the amorphous powder Co₆₇Si₂₃B₁₀. A particle morphology is observed with shapes of irregular aggregates of snowflakes and small flat spheres with a typical size of 50 μm [⁴²].

Figure 2
SEM/EDS micrographs of the Co₆₇Si₂₃B₁₀ powder.

In the upper right corner of Figure 2, a small spherical particle flattened at the poles with a typical size of 20 μm is visible, indicating strong plastic deformation effects during the 15 h milling process, leading to the evolution of the amorphous phase in the structural composition. By milling for 15 h as illustrated in Figure 2, we observe that, the powders are strain-hardened by heavy plastic deformation during milling and become brittle in nature [⁴³]. In this case, no agglomeration and cold welding occur due to fracturing mechanisms. As a result, the particle size is reduced, producing a mixture of semi-spherical and flattened particles, as can be seen at the top of the SEM micrograph in Figure 2. A narrow size distribution of 20 μm is developed.

Figure 2 displays the EDS analysis and mapping of the powder that was obtained after 15 h of milling. Co, Si, and B were present in the initial mixture, according to the EDS analysis. However, the EDS mapping reveals that the powders became inhomogeneous, and distinct clusters of Co, Si and B indicate the development of small fractions of nanocrystalline phases α-Co₂B and β-Co₂Si diluted and coexisting with the amorphous phase towards the end result of the amorphous powder Co₆₇Si₂₃B₁₀ mixture during milling [⁴⁴].

Figure 3 shows the TGA-DTG curves of Co₆₇Si₂₃B₁₀ powder obtained by heating until 1000ºC under an Ar atmosphere.

Figure 3
Overlapping TGA/DTA curves of the Co₆₇Si₂₃B₁₀ powder.

According to Figure 3, it can be said that the amorphous Co₆₇Si₂₃B₁₀ powder remains an amorphous metallic alloy up to a temperature of approximately 449.44°C, where a mass loss of only 1.03% occurs, which can be attributed to the loss of adhered moisture in conjunction with the presence of some reducible oxides, burnt carbon, etc.

Subsequently, in the temperature range of 449.44°C–672.56°C, a small mass gain of 5.676% is observed, showing the beginning of the crystallization and phase transformation of the amorphous Co₆₇Si₂₃B₁₀ powder. It also indicated that the crystallization was followed by the high temperature oxidation with some mass gains. The onset temperatures of the first and second exothermic peaks (T_x1 and T_x2) obtained from Figure 3.

For each curve, two separate exothermic peaks can be recognized, indicating a two-stage crystallization behavior. To clarify the precipitation phases, the structures of the alloys milled for 15 h under the effect of grinding in a wet environment were examined by XRD. Two of these peaks are the primary and secondary crystallization temperatures, where the formation of crystals from the amorphous phase is observed during the oxidation process.

The other two peaks show the oxidation transformation in the ribbons, and one of them shows a phase transformation. In region I, the exothermic peak in the DTA curve occurs around 675.87°C. After 15 h of milling time, a phase transition occurs. Heating the Co₆₇Si₂₃B₁₀ powder to higher temperatures leads to the formation of stable α-Co₂B and β-Co₂Si from the residual disordered phase [⁴⁵, ⁴⁶]. The phase of the (Co, Si)₃B type is retained in this case. The glass transition temperature (T_g1) is about 637.59°C and the first crystallization temperature (T_x1) is around is around 675.87°C for the amorphous Co₆₇Si₂₃B₁₀ powder, which corresponds to the supercooled liquid region associated to the endothermic peak, being considered higher value of ΔT causes a growth delay in the grain, i.e. ΔT₁=T_x1 −T_g1 =38.28°C with bulk metal glasses (BMG) of the cycle I region dotted in red. In the last stage of region II, we observed an exothermic peak in the DTA at ∼924.42°C, α-Co₂B and β-Co₂Si can be fixed in the phase composition of the alloy to a stable crystalline state through the mechanism of crystal nucleation and growth [⁴⁷, ⁴⁸]. Thus, the comparative study of the peculiarities of the crystallization and thermal stability of amorphous phases produced by MA. In circle II, the glass transition temperature (T_g2) is about 836.89°C, and the first crystallization temperature (T_2x) is around 924.42°C for the amorphous Co₆₇Si₂₃B₁₀ powder [⁴⁹]. The supercooled liquid region of circle II is associated with the endothermic peak by a temperature higher value of ΔT₂ causes a growth delay in the grain, i.e., ΔT₂=T_x2 − T_g2 = 87.53°C with bulk metal glasses (BMG) [⁵⁰, ⁵¹].

The transition to a stable crystalline state upon heating occurs through the mechanism of crystal nucleation and growth [⁵², ⁵³]. Under the effect of a thermodynamic driving force, such a process can be realized, depending on the kinetic features, either through the formation of stable crystals directly from the amorphous phase or, if this way is kinetically hindered, through the formation of a number of metastable crystal structures [⁵⁴, ⁵⁵]. It is known that plastic deformation of an amorphous phase increases the fraction of excess free volume in it, which facilitates the diffusion of atoms [⁵⁶]. Consequently, in the MA amorphous alloys, we can expect, because of an increased excess free volume, the acceleration of diffusion, the elimination of kinetic restrictions, a decrease in thermal stability, and a simpler mechanism of crystallization (amorphous phase→stable crystalline phase) compared to the amorphous ribbons of the same chemical composition of the amorphous alloy [⁵⁷, ⁵⁸].

Figure 4 shows the Co₆₇Si₂₃B₁₀ powder with isothermal type IV adsorption lines and H3-type hysteresis loops. The hysteresis loops of the black and red lines represent the adsorption (ADS) and desorption (DES) curves.

Figure 4
Adsorption/desorption isotherms of N₂ for Co₆₂Nb₃₂B₆ alloy.

Furthermore, they presented type IV isotherm profiles as shown in Figure 4, indicating mesoporous properties due to their high mesopore density according to the IUPAC classification [⁵⁹]. The pore structure is provided by the aggregates of small powders in flake-like shapes and small spherical particles flattened with a maximum specific surface area of 3.195 m²/g and an average pore size of the adsorbent reached 1.0505 nm, respectively.

Figure 5 shows the hysteresis loops M-H for the powder Co₆₇Si₂₃B₁₀ at temperatures of 300 K, respectively, with a magnetic field range of –15 kOe to 15 kOe.

Figure 5
Hysteresis loop M-H for the powder Co₆₇Si₂₃B₁₀.

The hysteresis loop M-H of the powder Co₆₇Si₂₃B₁₀ shows an estimated saturation magnetization M_s= 114.31 emu/g, remanent magnetization M_r= 7.27 emu/g, and a coercive field H_c= 0.04869 kOe. In the upper part of Fig. 5, it exhibits strong typical soft magnetic alloy characteristics after milling the powder for 15 h. It is observed that the saturation remanence ratio (M_r/M_s) of powder Co₆₇Si₂₃B₁₀ is 0.05144, i.e., multidomains (M_r/M_s << 0.1) during 15 h of milling. The milled powders display the same ferromagnetic behavior with sigmoidal hysteresis curves as those typically seen in nanostructured materials with small magnetic multidomains. Despite the independence of the Co-based solid solution concentrations as identified by XRD investigation, the magnetic characteristics remain only partially stable. This suggests that due to the evolution of the amorphous phase with a small fraction of nanocrystalline phases α-Co₂B and β-Co₂Si as a solid solution, there is a single Bloch wall in magnetic domains [⁶⁰].

4. CONCLUSIONS

The α-Co₂B and β-Co₂Si nanocrystalline phases (around 1.9%) dispersed within an amorphous matrix (around 98.1%) are achieved after milling Co, Si, and B powder mixtures. This was confirmed by XRD patterns (showed the formation of a diffuse halo around 2θ = 45°, exhibiting the shape of an amorphous structure) as a function of milling time up to 15 h by MA.

The micrograph of amorphous Co₆₇Si₂₃B₁₀ powder showed aggregates of small powders in flake-like shapes and small spherical particles flattened with a size of 50μm, along with the-EDS analysis and mapping of the powder obtained from 15 h of milling. Co, Si, and B were present in the initial mixture, as indicated by the EDS analysis. However, the EDS mapping reveals that the powders became inhomogeneous, with distinct clusters of Co and Si indicating the development of the nanocrystalline phases α-Co₂B and β-Co₂Si coexisting with the amorphous phase towards the end result of the powder mixture’s milling. The Co₆₇Si₂₃B₁₀ powder exhibited typical soft magnetic properties. Conversely, the Co₆₇Si₂₃B₁₀ powder showed two crystallization exothermic peaks at primary and secondary temperatures.

The formation of nanocrystalline phases α-Co₂B and β-Co₂Si from the amorphous phase is observed during the oxidation process at high temperatures, resulting in some mass gains. The N₂ adsorption-desorption isotherm of Co₆₇Si₂₃B₁₀ powder alloy represents a type IV isotherm with a hysteresis loop profile characteristic of H3 type mesoporous materials. The saturation magnetization was M_s = 114.31 emu/g, remanent magnetization was M_r = 7.27 emu/g, a coercive field H_c= 0.04869 kOe, and it showed a saturation remanence ratio in the order of M_r/M_s = 0.051447, revealing multidomains (M_r/M_s << 0.1) during 15 h of milling.

5. ACKNOWLEDGEMENTS

The authors wish to thank CAPES for the financial support of this researcher.

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Publication Dates

• Publication in this collection
  24 June 2024
• Date of issue
  2024

History

• Received
  06 May 2024
• Accepted
  13 May 2024