Graphical abstract

The long-term dispersion stability of exfoliated MoS2 nanoflakes was evaluated using Turbiscan analysis. Long-chain alcohols and mixed IPA–THF solvents showed significantly lower TSI values, highlighting the role of molecular chain length and solvent blending in suppressing sedimentation through optimized interfacial compatibility.

1. Introduction

With the growing global emphasis on achieving carbon neutrality and securing sustainable energy solutions, hydrogen has emerged as a promising next-generation energy vector [1]. In particular, electrochemical water splitting has gained significant attention as an environmentally benign method for hydrogen production, owing to its absence of carbon dioxide emissions and potential for long-term viability [2, 3]. Consequently, the development of efficient electrocatalysts for the hydrogen evolution reaction (HER) has become a central focus of contemporary energy research, prompting extensive efforts to identify cost-effective alternatives to noble-metal catalysts [3].

Platinum (Pt)-based catalysts have exhibited the highest catalytic performance toward HER. However, their high cost and limited natural abundance restrict large-scale applications, thereby necessitating the search for alternative materials with comparable catalytic activity but lower economic and resource constraints [3]. Among these, molybdenum disulfide (MoS₂), a representative transition-metal dichalcogenide (TMD), has attracted significant interest due to its chemical stability, earth abundance, and unique two-dimensional layered structure [2, 4]. The catalytically active edge sites of MoS₂ provide abundant reaction centers owing to their unsaturated coordination, while the basal planes remain largely inert [3]. Nevertheless, strong van der Waals interactions between the layers in bulk MoS₂ limit ion accessibility and hinder charge transport, resulting in suboptimal electrochemical performance [4].

To overcome these limitations, various structural engineering strategies have been proposed to reduce the layer thickness and expand the interlayer spacing through exfoliation [2]. In particular, the intercalation of small cations such as lithium (Li^⁺) or sodium (Na^⁺) has been reported to effectively widen the interlayer gaps and enhance the electronic properties and catalytic efficiency of MoS₂ [4-6]. However, the success of such intercalation-based modifications strongly depends on the dispersion state of exfoliated Modis powders [3]. Inadequate dispersion often leads to flake agglomeration or sedimentation, thereby reducing ion accessibility and impairing electrochemical performance. Thus, achieving long-term colloidal stability in suitable solvents is essential to enable uniform ion intercalation and ensure reproducible material modifications [7, 8].

The dispersion behavior of two-dimensional materials such as MoS₂ is governed by solvent physicochemical properties, including polarity, viscosity, surface tension, and density [4]. Of particular importance is the interfacial compatibility between the solvent medium and the MoS₂ surface, which determines not only exfoliation efficiency but also long-term colloidal stability. Alcohol-based solvents, whose polarity and hydrophobicity can be systematically tuned by varying alkyl chain length, are well suited for dispersion studies. Furthermore, mixed solvent systems (e.g., IPA–THF) provide additional flexibility, as their miscibility allows precise control of polarity and viscosity to improve dispersion stability [2, 9, 10].

Conventionally, N-methyl-2-pyrrolidone (NMP) has been widely used for MoS₂ dispersion due to its strong solvating ability. However, its significant toxicity and environmental hazards have increasingly limited large-scale applicability. In addition, sonochemical degradation of NMP during ultrasonication has been reported, raising further concerns for reliable data interpretation. These limitations have motivated the search for safer alternatives such as isopropyl alcohol (IPA), tetrahydrofuran (THF), and their mixtures, which offer relatively low toxicity while maintaining tunable physicochemical properties [4, 5, 11]. Nevertheless, the volatility and flammability of THF also necessitate careful handling and raise important considerations for practical applications.

Despite these developments, most prior studies have relied on qualitative or short-term methods such as UV–vis spectroscopy or dynamic light scattering (DLS), focusing primarily on exfoliation efficiency [2, 5]. Systematic and quantitative investigations into long-term dispersion behavior—particularly sedimentation kinetics over extended periods—remain scarce, despite their critical importance in identifying solvents suitable for intercalation-based structural engineering and electrochemical applications [7].

Previous studies have highlighted that homogeneous dispersion plays a decisive role in Na^⁺ intercalation efficiency and electrochemical reproducibility. Li et al. experimentally demonstrated that non-uniform dispersion during Na^⁺ insertion induces localized structural stress, which in turn promotes the formation of undesirable intermediate phases [12]. Furthermore, Massaro et al. revealed through DFT calculations that the Na^⁺ diffusion pathway and energy barrier differ significantly between the 1T and 3R phases of MoS₂, suggesting that the dispersion state can directly influence the energetic landscape of ion intercalation and the structural stability of the host lattice [6]. Collectively, these findings indicate that homogeneous dispersion enhances interlayer accessibility, prevents localized ion accumulation, and mitigates structural stress and uneven expansion, thereby enabling reversible insertion/extraction. As a result, the formation of intermediate phases is suppressed, and the reproducibility and stability of electrochemical reactions are substantially improved.

In this study, the dispersion stability of exfoliated MoS₂ nanoflakes was quantitatively evaluated in a series of single organic solvents and IPA–THF mixtures using Turbiscan analysis. Although this work does not directly include Na^⁺ intercalation experiments, such solvent-dependent stability assessments are crucial preparatory steps toward achieving uniform and reproducible Na^⁺ intercalation. These insights provide a fundamental foundation for structural optimization and reliable performance in electrochemical applications, including HER electrocatalysis.

2. Experimental Section

2.1 Preparation of Exfoliated MoS₂ Materials

Exfoliated MoS₂ powders were prepared using the quenching-assisted exfoliation method recently developed by our group (Sung et al., accepted for publication in Archives of Metallurgy and Materials). In the referenced study, bulk MoS₂ was thermally treated and rapidly quenched in liquified nitrogen, resulting in few-layer nanoflakes with a thickness of approximately 4–6 nm (Sung et al.). For the present work, the exfoliated MoS₂ sample obtained at the optimized temperature condition of 150 °C was selected for dispersion stability analysis.

2.2 Materials and Characterizations

To evaluate dispersion stability, 10 mg of exfoliated MoS₂ powder was added to 50 mL of each selected organic solvent and dispersed using a bath-type ultrasonic cleaner (40 kHz, 100 W) for 30 minutes at room temperature. The tested solvents included methanol, 1-butanol, 1-hexanol, 1-octanol, 1-decanol, 1-undecanol, isopropyl alcohol (IPA), tetrahydrofuran (THF), and IPA–THF binary mixtures with varying volume ratios (2.5:7.5, 5:5, and 7.5:2.5). All dispersions were left undisturbed at 25 °C for 72 hours. Stability measurements were performed using a Turbiscan LAB analyzer (Formulaction, France), which monitors temporal changes in light transmittance and backscattering along the sample height using a near-infrared laser (λ = 880 nm). The transmittance variation (ΔT), backscattering variation (ΔBS), and Turbiscan Stability Index (TSI) were obtained to quantitatively assess the sedimentation behavior. Lower values of these parameters indicate improved dispersion stability. All measurements were continuously monitored over a period of three days to ensure time-resolved stability analysis.

3. Results and Discussion

3.1 Dispersion Stability Analysis Based on Turbiscan

In this study, exfoliated MoS₂ powders were dispersed in various non-aqueous organic solvents and mixed solvent systems, and their sedimentation behavior and dispersion stability over time were quantitatively analyzed using a Turbiscan instrument [13-16]. This equipment employs a non-invasive optical scanning method based on static multiple light scattering (SMLS) to monitor real-time changes in particle migration and optical density between the upper and lower layers of the sample [13]. From this, key indicators such as transmittance (T), the average variation in transmittance (ΔT), backscattering variation (ΔBS), and the Turbiscan Stability Index (TSI) can be derived.

The transmittance T represents light transmittance as a function of both time and sample height (h), and is expressed by the following equation:

(1)

T(h,t)=T0·e−d·∅·Qs·γiλ

where T₀ is the transmittance of the continuous phase, d is the average particle diameter, ∅ is the volume fraction of the dispersed phase, Q_s is the scattering coefficient based on Mie theory, γ_i is the radial position in the vial, and λ is the mean free path of the photons. This equation allows for quantitative analysis of the influence of particle size, concentration, and scattering characteristics on the transmittance.

The average transmittance variation (ΔT) quantifies the change in transmittance at a specific time point relative to the initial state and serves as an indicator of dispersion stability, with lower ΔT values signifying better stability. It is calculated as follows:

(2)

ΔT=T¯l-T¯0=1Hu-Hl∑h=HlHu (Ti (h)-T0 (h))

where T_i (h) and T₀ (h) represent the transmittance at height h at time i and the initial time, respectively. H_u and H_l define the upper and lower bounds of the analysis height range. In this context, T¯l and T¯0 denote the mean transmittance values averaged across the defined height interval at time i and time 0, respectively. These values reflect overall light transmission within the dispersion column the measured region of the sample and indicate the temporal evolution of particle uniformity. ΔT is particularly valuable for detecting local sedimentation or aggregation phenomena.

The backscattering variation (ΔBS) reflects changes in the backscattered light intensity due to differences in particle distribution and agglomeration within the sample. It is defined as:

(3)

ΔBS=BSi (h)-BS0 (h)

where BS_i (h) and BS₀ (h) denote the backscattering intensity at height h at time i and at the initial time, respectively. ΔBS is highly sensitive to vertical migration of particles caused by sedimentation or creaming and is especially effective in systems exhibiting multiple scattering, allowing for accurate assessment of dispersion stability [16].

Lastly, the Turbiscan Stability Index (TSI) is a cumulative indicator that quantifies the overall variation in light scattering across the entire sample height over time. It is expressed as:

(4)

TSIi=∑h=0H Ti (h)-Ti-1 (h)

TSI is widely used to evaluate the overall stability of a dispersion system; larger values indicate more pronounced particle migration or aggregation, implying lower dispersion stability [15].

In this work, all four Turbiscan-derived quantitative indicators were comprehensively analyzed to assess the time-dependent dispersion stability of MoS₂ powders in various solvent environments. Based on these evaluations, solvent systems suitable for pre-treatment processes involving sodium ion intercalation were systematically identified, providing a rational basis for optimizing structural engineering approaches for HER electrocatalyst applications.

3.2. Dispersion Stability of MoS₂ Assessed by TSI

In this study, the dispersion stability of exfoliated MoS₂ nanoflakes in alcohol-based solvents was quantitatively evaluated using the Turbiscan Stability Index (TSI), and its correlation with the physicochemical properties of the solvents was systematically analyzed. MoS₂, as a typical two-dimensional nanomaterial with hydrophobic basal planes and hydrophilic edges, requires a solvent environment that is compatible with both types of surfaces [3]. Therefore, in addition to general polarity indices, parameters such as dipole moment, hydrophilic-lipophilic balance (HLB), viscosity, and hydrogen-bonding ability were taken into account to better understand the dispersion behavior [17].

The alcohol solvents were categorized into short-chain and long-chain types according to their HLB values. Solvents with HLB values greater than 6 were designated as short-chain, while those with values of 6 or less were considered long-chain alcohols. This classification served as a practical guideline for evaluating the balance between hydrophilic and lipophilic interactions with the MoS₂ surface.

Fig. 1 shows the TSI values of MoS₂ dispersed in linear alcohols with different alkyl chain lengths. A clear inverse relationship was observed between chain length and TSI value. Short-chain alcohols, such as methanol, 1-butanol, and 1-hexanol, exhibited relatively high TSI values, indicating rapid sedimentation and limited dispersion stability. On the other hand, long-chain alcohols, including 1-octanol, 1-decanol, and 1-undecanol, demonstrated significantly lower TSI values, reflecting greater resistance to sedimentation and improved long-term dispersion behavior. This behavior cannot be solely attributed to differences in molecular weight or volatility but is rather explained by the combination of lower polarity, higher viscosity, and greater interfacial affinity of long-chain alcohols with the hydrophobic basal planes of MoS₂ [17, 18]. While short-chain alcohols tend to form hydrogen bonds with the hydrophilic edge sites, they are less compatible with the basal planes and lack sufficient viscosity to suppress sedimentation. In contrast, long-chain alcohols reduce the interfacial energy mismatch and gravitational settling through their hydrophobicity and increased viscosity, leading to more stable colloidal dispersions. This enhanced colloidal stability is not only important from a physical dispersion standpoint but also highly relevant for subsequent Na^⁺ intercalation. Uniformly dispersed nanoflakes provide consistent interlayer accessibility, minimizing localized aggregation that could otherwise generate heterogeneous ion-diffusion pathways. In doing so, stable dispersions facilitate homogeneous Na^⁺ intercalation across both basal planes and edge sites, while reducing local strain and suppressing undesirable intermediate phase formation. Similar conclusions were drawn in previous studies, where homogeneous dispersions were shown to facilitate reversible Na^⁺ intercalation and improve electrochemical reproducibility by suppressing localized stress and phase heterogeneity [12, 14].

Fig. 2 presents a comparison of TSI values for MoS₂ dispersed in single solvents (isopropanol and tetrahydrofuran) and their binary mixtures at volume ratios of 2.5 to 7.5, 5 to 5, and 7.5 to 2.5. When used alone, isopropanol showed a TSI value of 46, while tetrahydrofuran showed a significantly higher TSI value of 74, indicating poor stability in both cases. Isopropanol, a polar protic solvent with a dipole moment of 1.66 D and an HLB of 11.5, forms hydrogen bonds with the edge sites of MoS₂ but does not interact well with the basal planes. Tetrahydrofuran, an aprotic solvent with low viscosity and limited hydrogen bonding ability, also failed to provide sufficient stabilization.

However, the binary mixtures of the two solvents exhibited notable improvements in dispersion behavior. In particular, the 5 to 5 volume ratio mixture showed the lowest TSI value of 41, indicating the most favorable dispersion condition. This enhanced stability is attributed to the complementary interactions between the two solvents: isopropanol contributes hydrogen bonding to the edge sites, while tetrahydrofuran provides improved compatibility with the basal planes [19]. Although the HLB value of the 5 to 5 mixture (approximately 10.6) slightly exceeds the ideal range of 4 to 8 reported for the dispersion of layered nanomaterials, its dipole moment of about 1.71 D falls within the favorable range of 1.4 to 2.5 D [19]. The resulting physicochemical environment balances polarity and interfacial interactions, effectively suppressing aggregation and sedimentation.

Table 1 summarizes the solvent properties and corresponding TSI values. The most stable dispersions, including those prepared using 1-decanol, 1-undecanol, and the 5 to 5 THF–IPA mixture, share a common characteristic in terms of having dipole moment values within the optimal range. However, it should be noted that the HLB value of the 5 to 5 mixture exceeds the previously suggested ideal range. This result suggests that even when the HLB condition is not fully met, appropriate tuning of solvent combinations and their interactions can compensate and still yield highly stable dispersions.

In summary, the dispersion behavior of MoS₂ in organic solvents is governed not by a single parameter but by a complex interplay of dipole moment, interfacial compatibility, viscosity, hydrogen-bonding capability, and HLB balance. Long-chain alcohols and mixed solvents with carefully tuned compositions were found to be effective in stabilizing MoS₂ nanoflakes. These findings offer a rational guideline for solvent design and optimization for two-dimensional materials in colloidal systems.

Compared with NMP, which possesses a relatively high dipole moment (~4.1 D) and an HLB value of ~8–9, the IPA–THF (5:5) mixture exhibits a dipole moment of ~1.7–1.8 D and an HLB value of ~10.6. Although these values differ slightly from the conventional solvent, they fall within or near the favorable ranges reported for the dispersion of layered nanomaterials. Importantly, the IPA–THF (5:5) mixture yielded the lowest TSI value (41) among all tested systems, demonstrating dispersion stability comparable to that of NMP. This finding suggests that IPA–THF binary solvents can provide a practical balance between physicochemical compatibility and colloidal stability, while offering significantly lower toxicity and safer handling than NMP.

3.3. Time- and Height-Resolved Turbiscan Analysis of MoS₂ Dispersion Stability

Fig. 3 presents the time-resolved optical profiles of MoS₂ dispersions in linear alcohol solvents, represented by transmittance variation (ΔT) and backscattering variation (ΔBS). The profiles are color-coded, with the curves gradually shifting from red (initial) to purple (final) as the measurement time progresses. A clear dependence on alkyl chain length was observed: as the chain length increased, the amplitudes of both ΔT and ΔBS decreased, indicating that longer-chain alcohols more effectively suppressed particle migration and aggregation. Methanol and 1-butanol exhibited a steep increase in transmittance in the upper region and pronounced changes in backscattering at the bottom, signifying early sedimentation and rapid particle rearrangement. In particular, the transmittance increase in the upper layer of methanol does not indicate enhanced stability but rather reflects the rapid settling of MoS₂ particles out of suspension. In contrast, dispersions in 1-octanol and 1-decanol showed only minor changes, limited to slight increases in ΔT at the top and weak variations in ΔBS at the bottom. Most notably, 1-undecanol maintained nearly constant ΔT across the entire sample height and negligible ΔBS variation throughout the measurement, demonstrating minimal structural rearrangement and excellent long-term stability. Hexanol, which has an intermediate chain length, exhibited more pronounced changes in both ΔT and ΔBS compared with octanol and decanol. Specifically, ΔT increased in the upper region and ΔBS fluctuated at the bottom, suggesting that its moderate viscosity and limited interfacial affinity were insufficient to fully suppress particle settling. These results indicate that in mono-alcohol systems, dispersion stability is primarily governed by viscosity and hydrophobic affinity with the MoS₂ basal planes rather than solvent polarity alone.

Fig. 4 compares the dispersion behavior of MoS₂ in single solvents (IPA, THF) and in mixed IPA/THF systems with different volume ratios. As in Fig. 3, the optical profiles are color-coded from red (initial) to purple (final) to represent the time evolution. In IPA, a polar protic solvent, moderate increases in ΔT were observed in the upper region along with minor variations in ΔBS at the bottom. This reflects partial stabilization through hydrogen bonding at the MoS₂ edge sites; however, the relatively low viscosity of IPA could not completely prevent sedimentation. THF, by contrast, produced the most unstable dispersion, characterized by sharp ΔT fluctuations across the entire sample height and large ΔBS variations near the bottom. This instability is consistent with its low viscosity, lack of hydrogen-bonding capability, and weak interfacial affinity with MoS₂ surfaces, all of which promote rapid re-agglomeration and sedimentation. Beyond its poor dispersion stability, THF also poses volatility and flammability concerns that further limit its applicability as a large-scale solvent. In this study, therefore, THF was used only as a comparative reference to highlight the synergistic stabilization achieved when combined with IPA.

Among the mixed solvent systems, the IPA:THF = 5:5 composition exhibited the most favorable dispersion stability, characterized by nearly flat ΔT profiles throughout the sample height and minimal ΔBS changes, indicative of a well-balanced stabilization effect. In this system, IPA provides strong hydrogen bonding to the MoS₂ edge sites, while THF interacts with the basal planes, producing a synergistic effect that optimizes polarity, interfacial tension, and solvation capacity. The 7.5:2.5 mixture also displayed relatively stable behavior but showed slightly larger ΔT variations in the upper region compared with the 5:5 mixture, suggesting that the stabilizing role of IPA remained dominant but was not fully optimized. In contrast, the 2.5:7.5 mixture exhibited THF-dominated instability, with rapid sedimentation, pronounced ΔBS changes, and strong optical fluctuations, underscoring that excessive THF content compromises both stability and reproducibility.

Overall, these findings highlight that IPA-dominant mixtures are the most favorable choice for practical applications. Such systems not only ensure superior dispersion stability through complementary edge–basal plane interactions but also mitigate handling risks and provide a safer environmental profile compared with conventional solvents such as NMP. Thus, the combination of high colloidal stability and reduced toxicity underscores the practical relevance of IPA-dominant mixtures as more sustainable and application-oriented solvent systems.

4. Conclusion

In this study, the dispersion stability of exfoliated MoS₂ nanoflakes was quantitatively assessed in various alcohol-based and mixed organic solvent systems using the Turbiscan Stability Index (TSI). The results revealed that solvent parameters such as dipole moment, viscosity, hydrogen-bonding ability, and hydrophilic-lipophilic balance (HLB) collectively influence colloidal stability. Among the tested solvents, long-chain alcohols such as 1-decanol and 1-undecanol exhibited superior stability due to their high viscosity and strong interfacial affinity with the hydrophobic basal planes of MoS₂. Additionally, binary mixtures of isopropanol (IPA) and tetrahydrofuran (THF) showed markedly improved dispersion behavior compared to either solvent alone, with the 5:5 volume ratio yielding the lowest TSI value. This enhancement was attributed to the synergistic effects of hydrogen bonding at edge sites and increased compatibility with basal planes. Notably, even though the HLB value of the 5:5 mixture exceeded the traditionally suggested range, its dipole moment remained within the optimal window, demonstrating that solvent systems can be effectively tailored to overcome individual limitations. These findings provide a practical framework for solvent selection and optimization in the processing of two-dimensional materials.

Article information

Funding

This work was supported by the project (PJE25160, ‘Development of TiN hard surface treatment technology on powder for application of tungsten cemented carbide material in cooperation with NUST, Pakistan’) funded by the Ministry of Economy and Finance (MOEF, Korea) as part of an international cooperation initiative.

Conflict of Interest

The authors declare no conflict of interest.

Data Availability Statement

The datasets generated during and/or analyzed during the current study are available from the corresponding author on reasonable request.

Author Information and Contribution

Jae Min Sung (Master’s student) contributed to conceptualization, investigation, data curation, and writing – original draft.

Dong-Won Kyung (Master’s student) participated in investigation and writing – review & editing.

Ammad Ali (PhD candidate) supported the formal analysis and contributed to writing – original draft.

Mi Hye Lee (Research technician) assisted with resources and materials preparation.

Kee-Ryung Park (Postdoctoral researcher) contributed to methodology and technical support.

Da-Woon Jeong (Principal researcher) participated in sample preparation and instrumentation.

Bum Sung Kim (Principal researcher) contributed to review & editing and validation.

Haejin Hwang (Professor) provided supervision and assisted in writing – review & editing.

Yoseb Song (Senior researcher; corresponding author) was responsible for funding acquisition, project administration, supervision, and writing – review & editing.

Acknowledgments

None.

Fig. 1.

Turbiscan stability index values of MoS₂ dispersions in alcohol-based solvents with varying carbon chain lengths.

Fig. 2.

Turbiscan stability index values of MoS₂ dispersions in polar organic solvents (IPA, THF) and their binary mixtures with different volume ratios. IPA, isopropanol; THF, tetrahydrofuran.

Fig. 3.

ΔT and ΔBS profiles of MoS₂ dispersions in alcohol-based solvents over 3 days (color scale from red to purple indicates time evolution).

Fig. 4.

ΔT and ΔBS profiles of MoS₂ dispersions in IPA, THF, and their binary solvent mixtures over 3 days (color scale from red to purple indicates time evolution). IPA, isopropanol; THF, tetrahydrofuran.

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