Asymmetric Magnetoresistance and Ultrafast Carrier Transport in Ni-Doped MoS2 Nanosheets

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Kamble, Shilpa D. Kamble, Umesh P. Gawai, Padmakar G. Chavan, and 2 more This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-7595921/v1 This work is licensed under a CC BY 4.0 License Status: Published Journal Publication published 26 Nov, 2025 Read the published version in Journal of Materials Science: Materials in Electronics → Version 1 posted You are reading this latest preprint version Abstract Pure and Ni doped MoS 2 (Mo 1 − x Ni x S 2 at x = 0, 2, 4, 6, and 8%) nanosheets were synthesized via hydrothermal method to study the effect of Ni on their structural, optical, morphological, and transport properties. XRD confirmed the samples having hexagonal phase, with peak shifts and disappearance of the (002) reflection at higher doping levels, indicating lattice strain and reduced crystallinity supported by Raman spectra. HR-TEM micrographs confirm the formation of nanosheets decorated with Ni quantum dots. PL spectra exhibited A and B exciton peaks at ~ 797 nm and ~ 689 nm, with Ni doping affecting exciton dynamics and non-radiative recombination. Hall measurements shows n-type conduction in all samples, with carrier concentration and mobility strongly dependent on Ni content. Low doping (2%) reduces mobility and increases resistivity, while higher doping (8%) mobility (~ 2.13×10⁵ cm²/V·s) and conductivity (0.608 S/cm) increases, induces metallic-like behavior with very high mobility. The R-T behavior of 4% Ni-doped MoS 2 a semiconductor-to-metal-like transition near 220–250 K, with resistivity decreasing exponentially with temperature in the semiconducting regime and shifting to higher resistivity under applied magnetic field, confirming field-induced suppression of carrier mobility. It demonstrates a distinctive asymmetric MR(H) hysteresis with significant positive and negative MR contributions, confirming the coexistence of orbital and spin-dependent scattering mechanisms. The asymmetry (-10.22% Vs 23.36%) strongly evidences the role of localized Ni moments and defect-induced magnetic states in modulating carrier transport. Mobility transport property Hall Effect Resistivity Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 1 Introduction Nanosheets of transition-metal dichalcogenides (TMDs) have been emerged as important two dimensional materials for manufacturing future generation nanoscale devices to obtained fascinating electrical, optical, magnetic and transport phenomenon. These materials are widely explored in nanoelectronics, optoelectronics, batteries, sensors, memory, and biomedicine, owing to features like inversion symmetry, strong catalytic activity, and low interlayer friction [ 1 – 4 ]. Among TMDs, molybdenum disulfide (MoS 2 ) is particularly notable for its layered structure and it exhibits tuneable indirect and direct energy band gap of ~ 1.2 eV for bulk to ~ 1.9 eV for the monolayer respectively [ 5 – 7 ]. Atomic layer of MoS 2 contain a plane of molybdenum atoms mingle in between two planes of sulfur atoms, resulting a stable hexagonal lattice via Mo-S covalent bonds [ 8 ]. Depending on the atomic stacking and coordination environment, MoS 2 can crystallize in three main polymorphic phases: hexagonal (2H), octahedral (1T), and rhombohedral (3R) [ 9 ], each offering unique electronic and structural characteristics. Intrinsic MoS 2 is a n-type semiconductor material with high hole concentration. In large-scale MoS 2 nanostructures, the formation of a type-II heterojunction with p-type silicon (p-Si) facilitates efficient photovoltaic behavior by enabling effective charge carrier separation and transport. The incorporation of magnetic dopants such as Co, Ni, Mn, and Fe introduces internal magnetic moments into MoS 2 monolayers, providing a pathway to control valley Zeeman splitting (VZS) phenomena [ 8 ]. It is one of the notable candidate of the group-VI metal dichalcogenides, MoS 2 demonstrates superior performance in visible light photodetection due to its strong light absorption, tunable bandgap, and fast photo response characteristics. Its nanostructured forms have been widely investigated for applications in catalysis, sensing, photodetectors, solar energy harvesting, nonlinear optics, and optoelectronic devices, benefiting from excellent photostability under visible illumination [ 10 – 11 ]. Beyond optoelectronics, MoS 2 has also shown promise in cleaned energy related applications, like hydrogen evolution and wastewater purification, where it assists in degrading organic contaminants [ 12 ]. Previous studies have reported the hydrothermal synthesis of cobalt-doped MoS 2 nanosheets. For instance, Netravati et al. investigated their catalytic efficacy for nitroarene reduction [ 13 ], while Ma et al. demonstrated sustained hydrogen evolution reaction (HER) activity in alkaline environments [ 14 ]. Furthermore, Xu et al. reported that Co doping in MoS 2 /reduced graphene oxide composites enhanced lithium storage, achieving a capacity of 1236 mAh g⁻¹, attributed to changes in microstructure and morphology [ 15 ]. Overall, metal doping of MoS 2 has been shown to significantly enhance its performance across a variety of domains including hydrogen production [ 16 ], photovoltaic devices, supercapacitors [ 17 ], lithium-ion batteries [ 18 ], optoelectronics [ 19 ], and fluorescence-based sensing technologies [ 20 ].In electrocatalysis, fabricating MoS 2 nanosheets directly on conductive MoO 2 supports-such as 3D MoO 2 scaffolds-enhances charge transfer and active site availability [ 10 ]. These MoS 2 /MoO 2 hybrids boast low onset overpotentials (~ 142 mV), high current densities, low Tafel slopes (~ 35.6 mV dec⁻¹), and remarkable durability in hydrogen evolution reactions (HER).Hybrids combining MoS 2 and MoO 2 are also achievable-for instance, through one-step hydrothermal methods for composites used in hydrogen evolution, or CVD-based methods that yield finely crystalline hybrid morphologies for electrochemical catalysts [ 8 – 11 ]. In this study, we synthesized pure and Ni-doped MoS 2 nanostructures via a hydrothermal method to examine the influence of Ni incorporation on their structure, optical and transport properties by varying Ni content (0–8%), we systematically analyzed changes in structure, vibrational modes, excitonic and electronic features using XRD, Raman, PL, FTIR, TEM and Hall effect, R-T, MR-H respectively. The results revealed peak shifts, disappearance of the (002) plane at higher doping, modified exciton intensities, and Ni-decorated nanosheets with altered stoichiometry. Using Hall effect, we calculated carrier concentration (N b ), mobility (µ), and resistivity (ρ), which vary with Ni doping percentage. Heavy doping (8% Ni) dramatically increases mobility (~ 2.13×10⁵ cm²/V·s) and conductivity (0.608 S/cm), indicating the formation of extended electron pathways, possibly via impurity-band formation or Ni-induced metallic conduction channels. The results of magnetoresistance reveal that an asymmetric hysteresis in the R–H field is observed. These findings highlight how controlled Ni doping tunes the properties of MoS 2 composites, making them promising application in thermoelectrics. 2 EXPERIMENTAL DETAILS Pure and Ni doped MoS 2 nanosheets with varying compositions (0, 2, 4, 6, and 8%) were prepared via hydrothermal synthesis. Analytical-grade reagents, including ammonium molybdate tetrahydrate ((NH 4 ) 6 Mo 7 O 24 4H 2 O), Nickel nitrate hexahydrate (Ni(NO 3 ) 2 ·6H 2 O), and thiourea, were used as received without additional purification. For the synthesis, appropriate quantities of ammonium molybdate tetrahydrate (1 mM), Nickel nitrate ((1-x) mM), and thiourea (2 mM) were individually dissolved in 25 ml of deionized (DI) water in separate beakers. The thiourea solution was then added dropwise to the precursor mixture, followed by stirring at room temperature for 1 hour. The resulting solution was transferred to a 100 ml Teflon-lined stainless steel autoclave, which was sealed and heated on a hot plate at 185°C for 8 hours before being allowed to cool naturally. The obtained products were purified by repeated washing with ethanol and DI water, followed by filtration. The final material was dried under vacuum at 120°C for 5 hours. The synthesized products were characterized using various techniques. X-ray diffraction (XRD) analysis was conducted with a Bruker D8 Advance diffractometer employing Cu Kα radiation (wavelength = 1.5406 Å). Fourier-transform infrared (FTIR) spectroscopy was performed using a Bruker Vertex 70 spectrometer to obtain absorption spectra. UV-Vis absorption spectra were recorded on a PerkinElmer Lambda 950 spectrophotometer. Field Emission Gun-Transmission Electron Microscope with selected-area electron diffraction (SAED) (FEG-TEM 300kV) patterns were captured at an accelerating voltage of 300 kV using a FEI Tecnai G2 F30 TEM (IIT-B). Energy-dispersive spectra (EDS) were acquired with a JEOL JSM-6360 scanning electron microscope (SEM). Local structural properties of the samples were examined using micro-Raman spectroscopy (Horiba, LASER wavelength 532 nm). Hall Effect data was obtained using Ecopia HMS 3000 Hall Effect Measurement System with 0.57 T magnetic field. The temperature dependence of electrical resistivity (R-T) and magnetoresistance (MR-H) was measured on 9T-PPMS Quantum Design physical properties measurement system. 3 Results and Discussion 3.1 X-ray Diffraction study: Figure 1 (a) depicted of MoS 2 and 2% Ni-MoS 2 , the prominent peaks were observed at 13.94°, 34.57° and 58.45° are characteristic of the hexagonal crystal structure (2H phase) of MoS 2 , which is in line with the (002), (101) and (110) planes, respectively matches to JCPDS No.37-1492 a = b ≈ 3.181 Å and c ≈ 12.287 Å. In contrast, for higher Ni-doped MoS 2 samples the peak at 14° is absent or disappears. The slight shifts in the peak positions, particularly at 34.57°, 58.45° to 33.46°, 56.79° suggest that the incorporation of Ni atoms into the MoS 2 lattice has altered the local structure. This shift in the peaks is relative to their positions in pure MoS 2 , points towards structural strain and a slight contraction of the lattice. Such shifts in peak positions have been reported in other studies of Ni-doped MoS 2 , where Ni substitution causes a reduction in lattice parameters due to the smaller ionic radius of Ni²⁺ (69 pm) compared to Mo⁴⁺ (70 pm). The reduction of the (002) peak after 4%Ni doping is less pronounced in this case but indicates a minor contraction of the interlayer spacing. This is consistent with findings in similar transition metal-doped MoS 2 systems, where lattice strain or distortion is caused by the incorporation of Ni ions, leading to altered stacking and a reduction in crystallinity, showing amorphous nature of XRD patterns. In this analysis, the XRD peaks for MoS 2 indicate structural modifications that align with previously reported literature [ 12 – 18 ]. 3.2 Raman shift: Figure 2 (a-b) displayed the Raman spectrum of Pure and Ni-doped MoS 2 (x = 0,2, 4, 6, 8%) exhibits several characteristic peaks that provide insight into the material's structural and vibrational properties. Figure 2 (a) displayed the Raman spectra of Pure and 2% Ni doped MoS 2 reveals distinct peaks at approximately 241, 293, 343, 382 and 407cm − 1 , which are key to identifying the phases of MoS 2 .These peaks correspond to the \(\:{E}_{2g}^{1}\) , and A₁g vibrational modes at ~ 382 in-plane vibration of Mo-S and ~ 407cm − 1 out-planevibration of S atom correspond to 2H-MoS 2 phase. A peaks at ~ 241 cm⁻¹ can be associated with the J 2 mode of 1T-MoS 2 . It is derived from the oscillation of sulphur atoms perpendicular to the basal plane. Other peaks at ~ 343, are attributed to J 3 of 1T-MoS 2 m phasealong with 293 cm − 1 these peaks related to MoO 3 orthorhombic phase, it consistent with findings in prior studies [ 19 – 22 ]. Figure 2 (b) depicted the Raman shift of Ni (0.04, 0.06, 0.08, 0.10) doped MoS 2 reveals distinct peaks at approximately 142, 189, 279, 347 and 401 cm − 1 , which are key to identifying the 1T and 2H phases of MoS 2 . These peaks correspond to the J₁, J₂, J₃ and A₁g vibrational modes of 1T and 2H-MoS 2 respectively [ 23 – 26 ]. Notably, the prominent peaks at 142, 189, 347 cm⁻¹ are attributed to phonon modes and Mo-Mo stretching vibrations, providing evidence for the presence of the 1T phase of MoS 2 , consistent with findings in prior studies [ 27 – 28 ]. Whereas, the E₁g peak at 279 cm − 1 is linked to the octahedral arrangement of Mo atoms in 1T- MoS 2 . A significant observation is the absence of the characteristic E₂g¹ peak of 2H-MoS 2 at 383 cm − 1 , indicating that the 2H phase is not present. Meanwhile, the peak at 401 cm − 1 , typically associated with 2H- MoS 2 , is observed in pure MoS 2 samples but vanishes in Co-doped MoS 2 samples, suggesting a structural transformation induced by doping [ 28 – 29 ]. Raman spectroscopy stands out as a unique tool capable of distinguishing between the 1T and 2H phases of MoS 2 . Existing literature highlights that the 1T phase is characterized by peaks at approximately 156, 226, and 333 cm − 1 , while the 2H phase exhibits peaks at 380 and 404 cm − 1 , corresponding to the E₁²g and A₁g modes, respectively [ 30 – 31 ]. Based on the Raman data, it can be inferred that Ni doped (4 to 8%) MoS 2 exhibits a mixed 1T/2H structure. 3.3 PL Spectra Figure 3 displayed the photoluminescence (PL) spectra of pure and Ni-doped MoS 2 samples recorded from 500 to 900 nm wavenumber. It exhibit two distinctive features that provide insight into the excitonic behaviour, a strong peak at approximately ~ 797 nm and accompanied by shoulder peak at around ~ 689 nm [ 28 – 29 ]. These peaks correspond to the characteristic A and B excitons of MoS 2 , arising from direct bandgap transitions at the K point of the Brillouin zone, which are crucial for understanding the optical properties of these nanocomposites [ 30 – 31 ].The strong peak at ~ 797 nm is primarily attributed to the A exciton, representing the transition between the valence band maximum and the conduction band minimum. This indicates a high degree of optical quality in the MoS 2 samples, with effective exciton formation and minimal non-radiative recombination. The shoulder peak at ~ 689 nm is related to the B exciton, originating from transitions involving higher energy states in the valence band. The weaker intensity of the B exciton is typical due to its higher energy state and can be influenced by interlayer coupling and crystallinity [ 31 ].Variations in peak intensity between pure and Ni-doped samples may reflect changes in exciton binding energy and defect states introduced by Ni. An increased intensity of the A exciton peak in Ni-doped samples suggests improved charge carrier dynamics, while a decrease may indicate enhanced non-radiative processes. The band gaps remain consistent around 1.55–1.56 eV for peak A and around 1.80 eV for peak B, which is typical for MoS 2 . The intensity of peaks A and B is notably higher for pure MoS 2 and 8% Ni- MoS 2 compared to other Ni doping levels. Obtained results are consistent with the reported literature [ 28 – 34 ]. 3.4 FTIR study: Figure 4 displayed FTIR spectra which is a valuable technique for analyzing the vibrational properties and functional groups present in any materials. MoS 2 exhibits characteristic peaks associated with the Mo-S linkage, typically in the 400–500 cm -1 range [ 35 – 36 ]. A vibrational mode at 447 cm -1 is specifically assigned to the Mo-S linkage in synthesized samples. The broad absorption band in the 850–1000 cm⁻¹ region and the bands in the 500–780 cm⁻¹ range attributed to the stretching vibrations of O-Mo units and the bridging oxygen atoms in O-Mo-O bonds. A peak around 532 cm⁻¹ for specific Mo compounds has been assigned to the O-Mo-O mode [ 35 – 36 ].Hence the distinct pair of peaks at 1014, 1051cm⁻¹ strongly indicates the presence of a MoO 2 moiety, which is important for understanding the coordination environment of molybdenum within the MoO 2 structure.In a study of another peaks at 532, 620 and 780cm -1 were assigned to Mo-S and S-S bonds, respectively, and additional peaks were observed for sulphate vibrations and N-H stretching/bending vibrations, indicating the presence of other functional groups or impurities [ 36 ]. The peaks around 3283, 2088, 1450 and 1570cm -1 are often observed in MoS 2 samples, attributed to hydroxyl functionalities of adsorbed moisture from the atmosphere [ 35 – 42 ]. 3.5 Transport Properties The electronic transport properties of pure and Ni (2%, 4%, 6%, and 8%) doped MoS 2 Hall effect measurements were carried out at 300 K using the Van der Pauw method. I-V characteristics of Hall voltage and Hall current of samples are shown in Fig. 5 . As seen in the figure, these characteristics have Ohmic behavior, and there are slight deviations in resistivity between a-b, b-c, c-d, and d-a contacts. Also, this observed Ohmicbehavior provides an indication that Hall Effect measurements were performed properly. All samples exhibit n-type behavior, indicating electrons as the dominant charge carriers and all parameters are given in Table 1 . Pure MoS 2 shows a carrier concentration of 5.12 × 10 15 cm − 3 with moderate resistivity (1.60 × 10 2 Ω·cm) and mobility of 7.61 cm 2 /V·s, consistent with lightly electron-doped semiconducting characteristics. For the 2% Ni-doped sample, the experimental results show a carrier concentration of 2.63 × 10 14 cm − 3 , resistivity of 1.13 × 10 3 Ω·cm, and mobility of 21.1 cm 2 /V·s. This indicates that Ni doping reduces the electron density compared to pristine MoS 2 while simultaneously enhancing mobility, suggesting partial delocalization of electrons and the formation of defect states that contribute to conduction. As the Ni content increases to 4%, the carrier concentration, mobility, and resistivity exhibit non-monotonic changes due to competing effects of defect scattering, lattice distortion, and impurity band formation. At 6% Ni, stronger localization and higher resistivity are observed, while 8% Ni doping leads to a significant increase in mobility and reduction of resistivity, indicative of metallic-like transport possibly due to percolative conduction paths. Overall, Ni acts as an effective n-type dopant in MoS 2 , and its concentration critically tunes the balance between carrier localization, scattering, and extended conduction, making Ni-doped MoS 2 a promising candidate for electronic and thermoelectric applications. Table 1 Hall parameters of pure and Ni doped MoS 2 samples. Sample RH (cm 3 /C) Carrier Concentration Nb (cm − 3 ) Mobility µ (cm 2 /V·s) Resistivity ρ (Ω·cm) Conductivity σ (S/cm) Carrier Type MoS 2 1.219×10 3 5.12×10 15 7.61 1.60×10 2 6.24×10 − 3 n-type 2% Ni- MoS 2 2.378×10 4 2.63×10 14 21.1 1.13×10 3 8.87×10 − 4 n-type 4% Ni- MoS 2 3.261×10 4 1.91×10 14 248 1.31×10 2 7.61×10 − 3 n-type 6% Ni- MoS 2 6.670×10 5 9.36×10 12 21.9 3.05×10 4 3.28×10 − 5 n-type 8% Ni- MoS 2 3.506×10 5 1.78×10 13 2.13×10 5 1.64 0.608 n-type The temperature-dependent longitudinal electrical resistance, represented as ρ xx ( T ), was evaluated at various applied magnetic fields ranging from 0 T to 6 T for nanosheets of 4% Ni-doped MoS 2 as illustrated in Fig. 6 (a) at the temperature range of 100–300 K. The resistivity measurement was conducted on strip-shaped pellets with dimensions 2.5 × 2.5 × 1.5 mm 3 (length × width × thickness). At 0T, resistivity decreases monotonically with increasing temperature, indicating semiconducting behavior at low T. The resistivity of 4% Ni-doped MoS 2 decreases exponentially with increasing temperature, reflecting thermally activated semiconducting behavior at low temperatures and a semiconductor-to-metal-like transition around 200–250 K as shown in inset Fig. 6 (a). With the application of magnetic field (1-6T), the overall resistivity values increase, and the transition shifts toward higher resistivity values, suggesting magnetic field-induced scattering of charge carriers. The R-T behavior of 4% Ni-doped MoS₂ reveals that Ni incorporation introduces impurity levels and localized states that significantly influence carrier transport [ 42 ]. At higher temperatures, thermally activated carriers dominate, leading to a steep decrease in resistivity. However, the resistivity upturn at lower temperatures may be attributed to carrier localization, strong Coulomb interactions, or Ni-related defect scattering. The R–T curve shows a resistivity upturn only under an applied magnetic field, indicating that low-temperature transport in Ni-doped MoS₂ is dominated by spin-dependent scattering [ 43 ]. This behavior is consistent with the Kondo effect, where magnetic impurities scatter conduction electrons. In zero field, this scattering is weak or masked by other conduction processes, but the magnetic field aligns the impurity spins, enhancing scattering and producing the observed resistivity peaks. The observed shift in resistivity under magnetic field reflects the suppression of carrier mobility due to enhanced Lorentz force-induced scattering. The positive magnetoresistance suggests weak localization or Kondo-like scattering, consistent with Ni introducing localized magnetic moments [ 44 – 45 ]. Thus, Ni doping not only tunes the semiconductor-metal transition in MoS 2 but also enhances its magneto transport response. Figure 6 (b) displayed the field-dependent magnetoresistance (MR) of 4% Ni-doped MoS₂ at 250 K exhibits an asymmetric hysteresis loop with respect to the ± 6T magnetic field. In this case the asymmetric features meaning different values of ρ(H) for opposite H polarities. We define MR(%) = 100 × ((ρ(H)-ρ(0))/ρ(0)) here [ 42 – 45 ]. Unlike the symmetric MR response expected for non-magnetic semiconductors, the present system demonstrates strong sweep-direction dependence, confirming the role of dopant-induced magnetic interactions in governing transport. At low fields, MR(%) varies nonlinearly, and the forward and reverse field sweeps do not coincide, giving rise to a distinct hysteresis window [ 46 – 49 ]. This behavior is attributed to the presence of localized Ni-induced magnetic moments, which interact with charge carriers and give rise to spin-dependent scattering [ 42 – 50 ]. The irreversibility between forward and reverse scans reflects the partial pinning and relaxation of these magnetic moments during field cycling. Quantitatively, the MR(%) reaches approximately − 10.22% under negative field and about + 23.36% under positive field at 60 kOe. The asymmetry between positive and negative MR(%) is a clear indication that both ordinary MR(orbital scattering due to Lorentz force) and extraordinary MR (from localized magnetic clusters and spin polarization) coexist in the system. This non-reciprocal MR response is a hallmark of systems with granular ferromagnetism, exchange-bias-like coupling, or spin-orbit scattering, which can introduce direction-dependent resistivity changes. The overall positive MR trend highlights that carrier mobility is suppressed by field-induced orbital scattering, while the negative MR contribution suggests field-assisted suppression of spin scattering in certain configurations. The competition and imbalance between these two mechanisms lead to the asymmetric hysteresis observed. Such asymmetric MR loops in 4%Ni-MoS 2 provide strong evidence for the emergence of magnetically active states coupled with transport in the 2D host lattice. H. Zhang et al. [ 51 ] theoretically predicted, using DFT calculations, a negative magnetoresistance of -13.79% at 300 K for 3-layer MoS 2 /Ni(fcc). Similarly, W. Jie et al. [ 52 ] experimentally demonstrated that monolayer MoS 2 exhibits magnetoresistance values up to -12.7%. In comparison, our experimental measurements reveal a negative magnetoresistance of -10.22% at 250 K, which is consistent with the theoretical trend, despite slight differences in magnitude and measurement temperature [ 43 – 52 ]. 3.6 Morphological study Figure 7 (a-c) presents HR-TEM micrographs of 2% Ni-doped MoS 2 nanosheets, while Fig. 7 (d) shows the corresponding SAED pattern. The low-magnification TEM image (Fig. 7 a) reveals sheet-like morphologies with lateral dimensions in the nanometer to sub-micrometer range. At higher magnification (Fig. 7 b), uniformly distributed Ni quantum dots can be observed decorating the MoS 2 nanosheets. The high-resolution TEM image (Fig. 7 c) shows well-resolved lattice fringes corresponding to MoS 2 crystalline planes, along with regions of reduced fringe contrast, suggesting partial amorphization. The SAED pattern (Fig. 7 d) exhibits distinct concentric diffraction rings, indicative of a polycrystalline structure. This observation aligns with XRD analysis of the HRTEM image, which revealed characteristic lattice spacings of MoS 2 , together with variations likely arising from Ni incorporation and associated lattice distortion [ 38 , 48 ]. The coexistence of ordered and disordered regions implies that Ni doping affects the crystallinity, potentially introducing strain and altering local stacking sequences [ 39 – 40 , 47 ].Elemental analysis using energy-dispersive spectroscopy (EDS), as presented in Fig. 8 (a-d), reveals that the pure MoS 2 sample contains 49.62 at% Mo and 50.38 at% S. Upon 2% Ni doping, the composition changes markedly to 61.55 at% Mo, 36.63 at% S and 1.82 at% Ni. These results, obtained from point EDS analysis (Fig. 8 a, c), indicate a significant reduction in sulphur content and a corresponding increase in molybdenum, suggesting that Ni incorporation alters the stoichiometry and possibly induces partial sulphur loss or oxygen incorporation [ 49 – 52 ]. 4 Conclusion This study demonstrates that Ni doping significantly modifies the structural, vibrational, optical, and electronic transport properties of MoS 2 nanostructures. XRD and Raman analyses reveal lattice distortions and interlayer coupling, while PL confirms tunable excitonic behavior with doping concentration. FTIR validates Mo-S bonding, and TEM/EDS confirm nanosheet morphology with Ni quantum dot decoration and stoichiometric changes. Hall measurements indicate n-type conduction, with carrier concentration, mobility, and resistivity strongly dependent on Ni content. The combined R-T and MR(%) measurements on 4% Ni-doped MoS₂ provide new insights into its magneto-transport behavior. The R-T data confirm a thermally activated semiconducting state with a transition to metallic-like conduction near 250 K, while the field-dependent shift highlights the role of magnetic scattering in transport. The MR-H curves display a clear asymmetric hysteresis, with magnetoresistance values of -10.22% and + 23.36% under negative and positive fields, respectively, indicating strong coupling between charge carriers and localized Ni moments. Declarations Conflicts of Interest: The authors declare that they have no conflicts of interest. Acknowledgments: The authors sincerely thank Dr.Vasant Sathe, and Devedra Kumar, UGC-DAE CSR, Indore, India, for his invaluable assistance with the Raman shift and magnetoresistance (R-T, MR-H) measurements respectively. Author contribution statement: All authors have contributed equally to the research and preparation of this work. Funding: This research was funded by BARTI through a fellowship awarded to CDK (Award Letter No: BARTI/Fellowship/BANRF-2021/2135). Data availability statement: The data supporting the findings of this study are available from the corresponding author upon reasonable request. References J. Lee, K.F. Mak, J. Shan, Nat. Nanotechnol. 11 (2016) 421. H.T. Yuan, M.S. Bahramy, K. Morimoto, S.F. Wu, K. Nomura, B.J. Yang, et al., Nat. Phys. 9 (2013) 563. Y. Ye, J. Xiao, H.L. Wang, Z.L. Ye, H.Y. Zhu, M. Zhao, et al., Nat. Nanotechnol. 11 (2016) 597. G.R. 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16:14:16","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":254204,"visible":true,"origin":"","legend":"\u003cp\u003e(a) displayed for the pure and 2% doped MoS\u003csub\u003e2\u003c/sub\u003e and (b) displayed for 4% to 8% Ni doped MoS\u003csub\u003e2 \u003c/sub\u003enanostructures.\u003c/p\u003e","description":"","filename":"floatimage2.png","url":"https://assets-eu.researchsquare.com/files/rs-7595921/v1/27f14a10129169a2388f892c.png"},{"id":92885474,"identity":"bf8f57ce-6adb-40ab-97b8-c2ae858043a7","added_by":"auto","created_at":"2025-10-06 16:22:09","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":105894,"visible":true,"origin":"","legend":"\u003cp\u003ePL spectra of pure and Ni doped MoS\u003csub\u003e2\u003c/sub\u003e nanostructure.\u003c/p\u003e","description":"","filename":"floatimage3.png","url":"https://assets-eu.researchsquare.com/files/rs-7595921/v1/15b06b16fa59f1ae884ed406.png"},{"id":92885032,"identity":"64bbfe74-b10b-483b-ae6d-0e8f2a837f8d","added_by":"auto","created_at":"2025-10-06 16:14:09","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":126976,"visible":true,"origin":"","legend":"\u003cp\u003eFTIR spectra of Pure and 2% Ni doped MoS\u003csub\u003e2\u003c/sub\u003e nanostructure.\u003c/p\u003e","description":"","filename":"floatimage4.png","url":"https://assets-eu.researchsquare.com/files/rs-7595921/v1/781295098913d2aabf41a992.png"},{"id":92885046,"identity":"2b254b4d-453c-40ca-8879-61c15e3332c1","added_by":"auto","created_at":"2025-10-06 16:14:11","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":363705,"visible":true,"origin":"","legend":"\u003cp\u003eI-V characteristics of pure and Ni doped MoS\u003csub\u003e2 \u003c/sub\u003enanostructures.\u003c/p\u003e","description":"","filename":"floatimage5.png","url":"https://assets-eu.researchsquare.com/files/rs-7595921/v1/d3c6ecd6cee1e3d860c800c8.png"},{"id":92885475,"identity":"22f5dcf1-1a3e-4ff7-88d5-f95f6632c5cb","added_by":"auto","created_at":"2025-10-06 16:22:09","extension":"png","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":305164,"visible":true,"origin":"","legend":"\u003cp\u003e(a) Magnetic field dependant resistivity (b) percentage of magnetoresistance at 250K for 4% Ni doped MoS\u003csub\u003e2\u003c/sub\u003e nanosheets.\u003c/p\u003e","description":"","filename":"floatimage6.png","url":"https://assets-eu.researchsquare.com/files/rs-7595921/v1/f36ecfec80cde549e214381d.png"},{"id":92885101,"identity":"aed0dfc6-7d0b-4f1c-bd7a-798c2928645d","added_by":"auto","created_at":"2025-10-06 16:14:16","extension":"png","order_by":7,"title":"Figure 7","display":"","copyAsset":false,"role":"figure","size":151466,"visible":true,"origin":"","legend":"\u003cp\u003e(a-c) and (d) shows the HR-TEM micrograph and SAED patterns of 2% Ni doped MoS\u003csub\u003e2 \u003c/sub\u003enanosheets respectively.\u003c/p\u003e","description":"","filename":"floatimage7.png","url":"https://assets-eu.researchsquare.com/files/rs-7595921/v1/d84b08576009f5ed8028402f.png"},{"id":92885040,"identity":"0c761bed-ad11-4115-b3ba-f571b7650a3b","added_by":"auto","created_at":"2025-10-06 16:14:10","extension":"png","order_by":8,"title":"Figure 8","display":"","copyAsset":false,"role":"figure","size":169932,"visible":true,"origin":"","legend":"\u003cp\u003e(a, c) shows the spot for point analysis measures the elemental composition and its corresponding EDS spectra (b) pure MoS\u003csub\u003e2 \u003c/sub\u003e(b) 2% Ni doped MoS\u003csub\u003e2 \u003c/sub\u003erespectively.\u003c/p\u003e","description":"","filename":"floatimage8.png","url":"https://assets-eu.researchsquare.com/files/rs-7595921/v1/7b82ddb7b863e90f09bbfe25.png"},{"id":97178793,"identity":"9f9f2835-8c89-45a9-9452-2fe0edf5cd18","added_by":"auto","created_at":"2025-12-01 16:13:41","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":2423794,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-7595921/v1/152b2d84-3c55-4cbf-a22a-16f5c6ff7fbc.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"\u003cp\u003eAsymmetric Magnetoresistance and Ultrafast Carrier Transport in Ni-Doped MoS\u003csub\u003e2\u003c/sub\u003e Nanosheets\u003c/p\u003e","fulltext":[{"header":"1 Introduction","content":"\u003cp\u003eNanosheets of transition-metal dichalcogenides (TMDs) have been emerged as important two dimensional materials for manufacturing future generation nanoscale devices to obtained fascinating electrical, optical, magnetic and transport phenomenon. These materials are widely explored in nanoelectronics, optoelectronics, batteries, sensors, memory, and biomedicine, owing to features like inversion symmetry, strong catalytic activity, and low interlayer friction [\u003cspan additionalcitationids=\"CR2 CR3\" citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e4\u003c/span\u003e]. Among TMDs, molybdenum disulfide (MoS\u003csub\u003e2\u003c/sub\u003e) is particularly notable for its layered structure and it exhibits tuneable indirect and direct energy band gap of ~\u0026thinsp;1.2 eV for bulk to ~\u0026thinsp;1.9 eV for the monolayer respectively [\u003cspan additionalcitationids=\"CR6\" citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e]. Atomic layer of MoS\u003csub\u003e2\u003c/sub\u003e contain a plane of molybdenum atoms mingle in between two planes of sulfur atoms, resulting a stable hexagonal lattice via Mo-S covalent bonds [\u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e8\u003c/span\u003e]. Depending on the atomic stacking and coordination environment, MoS\u003csub\u003e2\u003c/sub\u003e can crystallize in three main polymorphic phases: hexagonal (2H), octahedral (1T), and rhombohedral (3R) [\u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e9\u003c/span\u003e], each offering unique electronic and structural characteristics.\u003c/p\u003e\u003cp\u003eIntrinsic MoS\u003csub\u003e2\u003c/sub\u003e is a n-type semiconductor material with high hole concentration. In large-scale MoS\u003csub\u003e2\u003c/sub\u003e nanostructures, the formation of a type-II heterojunction with p-type silicon (p-Si) facilitates efficient photovoltaic behavior by enabling effective charge carrier separation and transport. The incorporation of magnetic dopants such as Co, Ni, Mn, and Fe introduces internal magnetic moments into MoS\u003csub\u003e2\u003c/sub\u003e monolayers, providing a pathway to control valley Zeeman splitting (VZS) phenomena [\u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e8\u003c/span\u003e]. It is one of the notable candidate of the group-VI metal dichalcogenides, MoS\u003csub\u003e2\u003c/sub\u003e demonstrates superior performance in visible light photodetection due to its strong light absorption, tunable bandgap, and fast photo response characteristics. Its nanostructured forms have been widely investigated for applications in catalysis, sensing, photodetectors, solar energy harvesting, nonlinear optics, and optoelectronic devices, benefiting from excellent photostability under visible illumination [\u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e10\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e11\u003c/span\u003e]. Beyond optoelectronics, MoS\u003csub\u003e2\u003c/sub\u003e has also shown promise in cleaned energy related applications, like hydrogen evolution and wastewater purification, where it assists in degrading organic contaminants [\u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e12\u003c/span\u003e]. Previous studies have reported the hydrothermal synthesis of cobalt-doped MoS\u003csub\u003e2\u003c/sub\u003e nanosheets. For instance, Netravati et al. investigated their catalytic efficacy for nitroarene reduction [\u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e], while Ma et al. demonstrated sustained hydrogen evolution reaction (HER) activity in alkaline environments [\u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e14\u003c/span\u003e]. Furthermore, Xu et al. reported that Co doping in MoS\u003csub\u003e2\u003c/sub\u003e/reduced graphene oxide composites enhanced lithium storage, achieving a capacity of 1236 mAh g⁻\u0026sup1;, attributed to changes in microstructure and morphology [\u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e]. Overall, metal doping of MoS\u003csub\u003e2\u003c/sub\u003e has been shown to significantly enhance its performance across a variety of domains including hydrogen production [\u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e], photovoltaic devices, supercapacitors [\u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e17\u003c/span\u003e], lithium-ion batteries [\u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e18\u003c/span\u003e], optoelectronics [\u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e19\u003c/span\u003e], and fluorescence-based sensing technologies [\u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e].In electrocatalysis, fabricating MoS\u003csub\u003e2\u003c/sub\u003enanosheets directly on conductive MoO\u003csub\u003e2\u003c/sub\u003e supports-such as 3D MoO\u003csub\u003e2\u003c/sub\u003e scaffolds-enhances charge transfer and active site availability [\u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e10\u003c/span\u003e]. These MoS\u003csub\u003e2\u003c/sub\u003e/MoO\u003csub\u003e2\u003c/sub\u003e hybrids boast low onset overpotentials (~\u0026thinsp;142 mV), high current densities, low Tafel slopes (~\u0026thinsp;35.6 mV dec⁻\u0026sup1;), and remarkable durability in hydrogen evolution reactions (HER).Hybrids combining MoS\u003csub\u003e2\u003c/sub\u003e and MoO\u003csub\u003e2\u003c/sub\u003eare also achievable-for instance, through one-step hydrothermal methods for composites used in hydrogen evolution, or CVD-based methods that yield finely crystalline hybrid morphologies for electrochemical catalysts [\u003cspan additionalcitationids=\"CR9 CR10\" citationid=\"CR8\" class=\"CitationRef\"\u003e8\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e11\u003c/span\u003e].\u003c/p\u003e\u003cp\u003eIn this study, we synthesized pure and Ni-doped MoS\u003csub\u003e2\u003c/sub\u003e nanostructures via a hydrothermal method to examine the influence of Ni incorporation on their structure, optical and transport properties by varying Ni content (0\u0026ndash;8%), we systematically analyzed changes in structure, vibrational modes, excitonic and electronic features using XRD, Raman, PL, FTIR, TEM and Hall effect, R-T, MR-H respectively. The results revealed peak shifts, disappearance of the (002) plane at higher doping, modified exciton intensities, and Ni-decorated nanosheets with altered stoichiometry. Using Hall effect, we calculated carrier concentration (N\u003csub\u003eb\u003c/sub\u003e), mobility (\u0026micro;), and resistivity (ρ), which vary with Ni doping percentage. Heavy doping (8% Ni) dramatically increases mobility (~\u0026thinsp;2.13\u0026times;10⁵ cm\u0026sup2;/V\u0026middot;s) and conductivity (0.608 S/cm), indicating the formation of extended electron pathways, possibly via impurity-band formation or Ni-induced metallic conduction channels. The results of magnetoresistance reveal that an asymmetric hysteresis in the R\u0026ndash;H field is observed. These findings highlight how controlled Ni doping tunes the properties of MoS\u003csub\u003e2\u003c/sub\u003ecomposites, making them promising application in thermoelectrics.\u003c/p\u003e"},{"header":"2 EXPERIMENTAL DETAILS","content":"\u003cp\u003ePure and Ni doped MoS\u003csub\u003e2\u003c/sub\u003enanosheets with varying compositions (0, 2, 4, 6, and 8%) were prepared via hydrothermal synthesis. Analytical-grade reagents, including ammonium molybdate tetrahydrate ((NH\u003csub\u003e4\u003c/sub\u003e)\u003csub\u003e6\u003c/sub\u003eMo\u003csub\u003e7\u003c/sub\u003eO\u003csub\u003e24\u003c/sub\u003e4H\u003csub\u003e2\u003c/sub\u003eO), Nickel nitrate hexahydrate (Ni(NO\u003csub\u003e3\u003c/sub\u003e)\u003csub\u003e2\u003c/sub\u003e\u0026middot;6H\u003csub\u003e2\u003c/sub\u003eO), and thiourea, were used as received without additional purification. For the synthesis, appropriate quantities of ammonium molybdate tetrahydrate (1 mM), Nickel nitrate ((1-x) mM), and thiourea (2 mM) were individually dissolved in 25 ml of deionized (DI) water in separate beakers. The thiourea solution was then added dropwise to the precursor mixture, followed by stirring at room temperature for 1 hour. The resulting solution was transferred to a 100 ml Teflon-lined stainless steel autoclave, which was sealed and heated on a hot plate at 185\u0026deg;C for 8 hours before being allowed to cool naturally. The obtained products were purified by repeated washing with ethanol and DI water, followed by filtration. The final material was dried under vacuum at 120\u0026deg;C for 5 hours.\u003c/p\u003e\u003cp\u003eThe synthesized products were characterized using various techniques. X-ray diffraction (XRD) analysis was conducted with a Bruker D8 Advance diffractometer employing Cu Kα radiation (wavelength\u0026thinsp;=\u0026thinsp;1.5406 \u0026Aring;). Fourier-transform infrared (FTIR) spectroscopy was performed using a Bruker Vertex 70 spectrometer to obtain absorption spectra. UV-Vis absorption spectra were recorded on a PerkinElmer Lambda 950 spectrophotometer. Field Emission Gun-Transmission Electron Microscope with selected-area electron diffraction (SAED) (FEG-TEM 300kV) patterns were captured at an accelerating voltage of 300 kV using a FEI Tecnai G2 F30 TEM (IIT-B). Energy-dispersive spectra (EDS) were acquired with a JEOL JSM-6360 scanning electron microscope (SEM). Local structural properties of the samples were examined using micro-Raman spectroscopy (Horiba, LASER wavelength 532 nm). Hall Effect data was obtained using Ecopia HMS 3000 Hall Effect Measurement System with 0.57 T magnetic field. The temperature dependence of electrical resistivity (R-T) and magnetoresistance (MR-H) was measured on 9T-PPMS Quantum Design physical properties measurement system.\u003c/p\u003e"},{"header":"3 Results and Discussion","content":"\u003cdiv id=\"Sec4\" class=\"Section2\"\u003e\u003ch2\u003e3.1 X-ray Diffraction study:\u003c/h2\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003eFigure \u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e (a) depicted of MoS\u003csub\u003e2\u003c/sub\u003eand 2% Ni-MoS\u003csub\u003e2\u003c/sub\u003e, the prominent peaks were observed at 13.94\u0026deg;, 34.57\u0026deg; and 58.45\u0026deg; are characteristic of the hexagonal crystal structure (2H phase) of MoS\u003csub\u003e2\u003c/sub\u003e, which is in line with the (002), (101) and (110) planes, respectively matches to JCPDS No.37-1492 a\u0026thinsp;=\u0026thinsp;b\u0026thinsp;\u0026asymp;\u0026thinsp;3.181 \u0026Aring; and c\u0026thinsp;\u0026asymp;\u0026thinsp;12.287 \u0026Aring;. In contrast, for higher Ni-doped MoS\u003csub\u003e2\u003c/sub\u003esamples the peak at 14\u0026deg; is absent or disappears. The slight shifts in the peak positions, particularly at 34.57\u0026deg;, 58.45\u0026deg; to 33.46\u0026deg;, 56.79\u0026deg; suggest that the incorporation of Ni atoms into the MoS\u003csub\u003e2\u003c/sub\u003e lattice has altered the local structure. This shift in the peaks is relative to their positions in pure MoS\u003csub\u003e2\u003c/sub\u003e, points towards structural strain and a slight contraction of the lattice. Such shifts in peak positions have been reported in other studies of Ni-doped MoS\u003csub\u003e2\u003c/sub\u003e, where Ni substitution causes a reduction in lattice parameters due to the smaller ionic radius of Ni\u0026sup2;⁺ (69 pm) compared to Mo⁴⁺ (70 pm). The reduction of the (002) peak after 4%Ni doping is less pronounced in this case but indicates a minor contraction of the interlayer spacing. This is consistent with findings in similar transition metal-doped MoS\u003csub\u003e2\u003c/sub\u003e systems, where lattice strain or distortion is caused by the incorporation of Ni ions, leading to altered stacking and a reduction in crystallinity, showing amorphous nature of XRD patterns. In this analysis, the XRD peaks for MoS\u003csub\u003e2\u003c/sub\u003e indicate structural modifications that align with previously reported literature [\u003cspan additionalcitationids=\"CR13 CR14 CR15 CR16 CR17\" citationid=\"CR12\" class=\"CitationRef\"\u003e12\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e18\u003c/span\u003e].\u003c/p\u003e\u003c/div\u003e\u003cdiv id=\"Sec5\" class=\"Section2\"\u003e\u003ch2\u003e3.2 Raman shift:\u003c/h2\u003e\u003cp\u003eFigure \u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e (a-b) displayed the Raman spectrum of Pure and Ni-doped MoS\u003csub\u003e2\u003c/sub\u003e(x\u0026thinsp;=\u0026thinsp;0,2, 4, 6, 8%) exhibits several characteristic peaks that provide insight into the material's structural and vibrational properties. Figure\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e (a) displayed the Raman spectra of Pure and 2% Ni doped MoS\u003csub\u003e2\u003c/sub\u003ereveals distinct peaks at approximately 241, 293, 343, 382 and 407cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, which are key to identifying the phases of MoS\u003csub\u003e2\u003c/sub\u003e.These peaks correspond to the \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\:{E}_{2g}^{1}\\)\u003c/span\u003e\u003c/span\u003e, and A₁g vibrational modes at ~\u0026thinsp;382 in-plane vibration of Mo-S and ~\u0026thinsp;407cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e out-planevibration of S atom correspond to 2H-MoS\u003csub\u003e2\u003c/sub\u003ephase. A peaks at ~\u0026thinsp;241 cm⁻\u0026sup1; can be associated with the J\u003csub\u003e2\u003c/sub\u003e mode of 1T-MoS\u003csub\u003e2\u003c/sub\u003e. It is derived from the oscillation of sulphur atoms perpendicular to the basal plane. Other peaks at ~\u0026thinsp;343, are attributed to J\u003csub\u003e3\u003c/sub\u003e of 1T-MoS\u003csub\u003e2\u003c/sub\u003e m phasealong with 293 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e these peaks related to MoO\u003csub\u003e3\u003c/sub\u003e orthorhombic phase, it consistent with findings in prior studies [\u003cspan additionalcitationids=\"CR20 CR21\" citationid=\"CR19\" class=\"CitationRef\"\u003e19\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e]. Figure\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e (b) depicted the Raman shift of Ni (0.04, 0.06, 0.08, 0.10) doped MoS\u003csub\u003e2\u003c/sub\u003e reveals distinct peaks at approximately 142, 189, 279, 347 and 401 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, which are key to identifying the 1T and 2H phases of MoS\u003csub\u003e2\u003c/sub\u003e. These peaks correspond to the J₁, J₂, J₃ and A₁g vibrational modes of 1T and 2H-MoS\u003csub\u003e2\u003c/sub\u003e respectively [\u003cspan additionalcitationids=\"CR24 CR25\" citationid=\"CR23\" class=\"CitationRef\"\u003e23\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e]. Notably, the prominent peaks at 142, 189, 347 cm⁻\u0026sup1; are attributed to phonon modes and Mo-Mo stretching vibrations, providing evidence for the presence of the 1T phase of MoS\u003csub\u003e2\u003c/sub\u003e, consistent with findings in prior studies [\u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e]. Whereas, the E₁g peak at 279 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e is linked to the octahedral arrangement of Mo atoms in 1T- MoS\u003csub\u003e2\u003c/sub\u003e. A significant observation is the absence of the characteristic E₂g\u0026sup1; peak of 2H-MoS\u003csub\u003e2\u003c/sub\u003e at 383 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, indicating that the 2H phase is not present. Meanwhile, the peak at 401 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, typically associated with 2H- MoS\u003csub\u003e2\u003c/sub\u003e, is observed in pure MoS\u003csub\u003e2\u003c/sub\u003e samples but vanishes in Co-doped MoS\u003csub\u003e2\u003c/sub\u003e samples, suggesting a structural transformation induced by doping [\u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e29\u003c/span\u003e]. Raman spectroscopy stands out as a unique tool capable of distinguishing between the 1T and 2H phases of MoS\u003csub\u003e2\u003c/sub\u003e. Existing literature highlights that the 1T phase is characterized by peaks at approximately 156, 226, and 333 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, while the 2H phase exhibits peaks at 380 and 404 cm\u003csup\u003e\u0026minus;\u0026thinsp;1\u003c/sup\u003e, corresponding to the E₁\u0026sup2;g and A₁g modes, respectively [\u003cspan citationid=\"CR30\" class=\"CitationRef\"\u003e30\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e31\u003c/span\u003e]. Based on the Raman data, it can be inferred that Ni doped (4 to 8%) MoS\u003csub\u003e2\u003c/sub\u003e exhibits a mixed 1T/2H structure.\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003c/div\u003e\u003cdiv id=\"Sec6\" class=\"Section2\"\u003e\u003ch2\u003e3.3 PL Spectra\u003c/h2\u003e\u003cp\u003eFigure \u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e displayed the photoluminescence (PL) spectra of pure and Ni-doped MoS\u003csub\u003e2\u003c/sub\u003e samples recorded from 500 to 900 nm wavenumber. It exhibit two distinctive features that provide insight into the excitonic behaviour, a strong peak at approximately\u0026thinsp;~\u0026thinsp;797 nm and accompanied by shoulder peak at around ~\u0026thinsp;689 nm [\u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e29\u003c/span\u003e]. These peaks correspond to the characteristic A and B excitons of MoS\u003csub\u003e2\u003c/sub\u003e, arising from direct bandgap transitions at the K point of the Brillouin zone, which are crucial for understanding the optical properties of these nanocomposites [\u003cspan citationid=\"CR30\" class=\"CitationRef\"\u003e30\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e31\u003c/span\u003e].The strong peak at ~\u0026thinsp;797 nm is primarily attributed to the A exciton, representing the transition between the valence band maximum and the conduction band minimum. This indicates a high degree of optical quality in the MoS\u003csub\u003e2\u003c/sub\u003esamples, with effective exciton formation and minimal non-radiative recombination. The shoulder peak at ~\u0026thinsp;689 nm is related to the B exciton, originating from transitions involving higher energy states in the valence band. The weaker intensity of the B exciton is typical due to its higher energy state and can be influenced by interlayer coupling and crystallinity [\u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e31\u003c/span\u003e].Variations in peak intensity between pure and Ni-doped samples may reflect changes in exciton binding energy and defect states introduced by Ni. An increased intensity of the A exciton peak in Ni-doped samples suggests improved charge carrier dynamics, while a decrease may indicate enhanced non-radiative processes. The band gaps remain consistent around 1.55\u0026ndash;1.56 eV for peak A and around 1.80 eV for peak B, which is typical for MoS\u003csub\u003e2\u003c/sub\u003e. The intensity of peaks A and B is notably higher for pure MoS\u003csub\u003e2\u003c/sub\u003e and 8% Ni- MoS\u003csub\u003e2\u003c/sub\u003e compared to other Ni doping levels. Obtained results are consistent with the reported literature [\u003cspan additionalcitationids=\"CR29 CR30 CR31 CR32 CR33\" citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR34\" class=\"CitationRef\"\u003e34\u003c/span\u003e].\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003c/div\u003e\u003cdiv id=\"Sec7\" class=\"Section2\"\u003e\u003ch2\u003e3.4 FTIR study:\u003c/h2\u003e\u003cp\u003eFigure \u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e displayed FTIR spectra which is a valuable technique for analyzing the vibrational properties and functional groups present in any materials. MoS\u003csub\u003e2\u003c/sub\u003e exhibits characteristic peaks associated with the Mo-S linkage, typically in the 400\u0026ndash;500 cm\u003csup\u003e-1\u003c/sup\u003e range [\u003cspan citationid=\"CR35\" class=\"CitationRef\"\u003e35\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR36\" class=\"CitationRef\"\u003e36\u003c/span\u003e]. A vibrational mode at 447 cm\u003csup\u003e-1\u003c/sup\u003eis specifically assigned to the Mo-S linkage in synthesized samples. The broad absorption band in the 850\u0026ndash;1000 cm⁻\u0026sup1; region and the bands in the 500\u0026ndash;780 cm⁻\u0026sup1; range attributed to the stretching vibrations of O-Mo units and the bridging oxygen atoms in O-Mo-O bonds. A peak around 532 cm⁻\u0026sup1; for specific Mo compounds has been assigned to the O-Mo-O mode [\u003cspan citationid=\"CR35\" class=\"CitationRef\"\u003e35\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR36\" class=\"CitationRef\"\u003e36\u003c/span\u003e].Hence the distinct pair of peaks at 1014, 1051cm⁻\u0026sup1; strongly indicates the presence of a MoO\u003csub\u003e2\u003c/sub\u003e moiety, which is important for understanding the coordination environment of molybdenum within the MoO\u003csub\u003e2\u003c/sub\u003estructure.In a study of another peaks at 532, 620 and 780cm\u003csup\u003e-1\u003c/sup\u003ewere assigned to Mo-S and S-S bonds, respectively, and additional peaks were observed for sulphate vibrations and N-H stretching/bending vibrations, indicating the presence of other functional groups or impurities [\u003cspan citationid=\"CR36\" class=\"CitationRef\"\u003e36\u003c/span\u003e]. The peaks around 3283, 2088, 1450 and 1570cm\u003csup\u003e-1\u003c/sup\u003e are often observed in MoS\u003csub\u003e2\u003c/sub\u003esamples, attributed to hydroxyl functionalities of adsorbed moisture from the atmosphere [\u003cspan additionalcitationids=\"CR36 CR37 CR38 CR39 CR40 CR41\" citationid=\"CR35\" class=\"CitationRef\"\u003e35\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR42\" class=\"CitationRef\"\u003e42\u003c/span\u003e].\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003c/div\u003e\u003cdiv id=\"Sec8\" class=\"Section2\"\u003e\u003ch2\u003e3.5 Transport Properties\u003c/h2\u003e\u003cp\u003eThe electronic transport properties of pure and Ni (2%, 4%, 6%, and 8%) doped MoS\u003csub\u003e2\u003c/sub\u003e Hall effect measurements were carried out at 300 K using the Van der Pauw method. I-V characteristics of Hall voltage and Hall current of samples are shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e. As seen in the figure, these characteristics have Ohmic behavior, and there are slight deviations in resistivity between a-b, b-c, c-d, and d-a contacts. Also, this observed Ohmicbehavior provides an indication that Hall Effect measurements were performed properly. All samples exhibit n-type behavior, indicating electrons as the dominant charge carriers and all parameters are given in Table \u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e. Pure MoS\u003csub\u003e2\u003c/sub\u003e shows a carrier concentration of 5.12 \u0026times; 10\u003csup\u003e15\u003c/sup\u003e cm\u003csup\u003e\u0026minus;\u0026thinsp;3\u003c/sup\u003e with moderate resistivity (1.60 \u0026times; 10\u003csup\u003e2\u003c/sup\u003eΩ\u0026middot;cm) and mobility of 7.61 cm\u003csup\u003e2\u003c/sup\u003e/V\u0026middot;s, consistent with lightly electron-doped semiconducting characteristics. For the 2% Ni-doped sample, the experimental results show a carrier concentration of 2.63 \u0026times; 10\u003csup\u003e14\u003c/sup\u003e cm\u003csup\u003e\u0026minus;\u0026thinsp;3\u003c/sup\u003e, resistivity of 1.13 \u0026times; 10\u003csup\u003e3\u003c/sup\u003eΩ\u0026middot;cm, and mobility of 21.1 cm\u003csup\u003e2\u003c/sup\u003e/V\u0026middot;s. This indicates that Ni doping reduces the electron density compared to pristine MoS\u003csub\u003e2\u003c/sub\u003e while simultaneously enhancing mobility, suggesting partial delocalization of electrons and the formation of defect states that contribute to conduction. As the Ni content increases to 4%, the carrier concentration, mobility, and resistivity exhibit non-monotonic changes due to competing effects of defect scattering, lattice distortion, and impurity band formation. At 6% Ni, stronger localization and higher resistivity are observed, while 8% Ni doping leads to a significant increase in mobility and reduction of resistivity, indicative of metallic-like transport possibly due to percolative conduction paths. Overall, Ni acts as an effective n-type dopant in MoS\u003csub\u003e2\u003c/sub\u003e, and its concentration critically tunes the balance between carrier localization, scattering, and extended conduction, making Ni-doped MoS\u003csub\u003e2\u003c/sub\u003e a promising candidate for electronic and thermoelectric applications.\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003e\u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab1\" border=\"1\"\u003e\u003ccaption language=\"En\"\u003e\u003cdiv class=\"CaptionNumber\"\u003eTable 1\u003c/div\u003e\u003cdiv class=\"CaptionContent\"\u003e\u003cp\u003eHall parameters of pure and Ni doped MoS\u003csub\u003e2\u003c/sub\u003e samples.\u003c/p\u003e\u003c/div\u003e\u003c/caption\u003e\u003ccolgroup cols=\"7\"\u003e\u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e\u003cdiv align=\"char\" char=\"\u0026times;\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e\u003cdiv align=\"char\" char=\"\u0026times;\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e\u003cdiv align=\"left\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e\u003cdiv align=\"left\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\u003e\u003c/div\u003e\u003cdiv align=\"left\" class=\"colspec\" colname=\"c6\" colnum=\"6\"\u003e\u003c/div\u003e\u003cdiv align=\"left\" class=\"colspec\" colname=\"c7\" colnum=\"7\"\u003e\u003c/div\u003e\u003cthead\u003e\u003ctr\u003e\u003cth align=\"left\" colname=\"c1\"\u003e\u003cp\u003eSample\u003c/p\u003e\u003c/th\u003e\u003cth align=\"left\" colname=\"c2\"\u003e\u003cp\u003eRH (cm\u003csup\u003e3\u003c/sup\u003e/C)\u003c/p\u003e\u003c/th\u003e\u003cth align=\"left\" colname=\"c3\"\u003e\u003cp\u003eCarrier Concentration Nb (cm\u003csup\u003e\u0026minus;\u0026thinsp;3\u003c/sup\u003e)\u003c/p\u003e\u003c/th\u003e\u003cth align=\"left\" colname=\"c4\"\u003e\u003cp\u003eMobility \u0026micro; (cm\u003csup\u003e2\u003c/sup\u003e/V\u0026middot;s)\u003c/p\u003e\u003c/th\u003e\u003cth align=\"left\" colname=\"c5\"\u003e\u003cp\u003eResistivity ρ (Ω\u0026middot;cm)\u003c/p\u003e\u003c/th\u003e\u003cth align=\"left\" colname=\"c6\"\u003e\u003cp\u003eConductivity σ (S/cm)\u003c/p\u003e\u003c/th\u003e\u003cth align=\"left\" colname=\"c7\"\u003e\u003cp\u003eCarrier Type\u003c/p\u003e\u003c/th\u003e\u003c/tr\u003e\u003c/thead\u003e\u003ctbody\u003e\u003ctr\u003e\u003ctd align=\"left\" colname=\"c1\"\u003e\u003cp\u003eMoS\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"char\" char=\"\u0026times;\" colname=\"c2\"\u003e\u003cp\u003e1.219\u0026times;10\u003csup\u003e3\u003c/sup\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"char\" char=\"\u0026times;\" colname=\"c3\"\u003e\u003cp\u003e5.12\u0026times;10\u003csup\u003e15\u003c/sup\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c4\"\u003e\u003cp\u003e7.61\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c5\"\u003e\u003cp\u003e1.60\u0026times;10\u003csup\u003e2\u003c/sup\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c6\"\u003e\u003cp\u003e6.24\u0026times;10\u003csup\u003e\u0026minus;\u0026thinsp;3\u003c/sup\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c7\"\u003e\u003cp\u003en-type\u003c/p\u003e\u003c/td\u003e\u003c/tr\u003e\u003ctr\u003e\u003ctd align=\"left\" colname=\"c1\"\u003e\u003cp\u003e2% Ni- MoS\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"char\" char=\"\u0026times;\" colname=\"c2\"\u003e\u003cp\u003e2.378\u0026times;10\u003csup\u003e4\u003c/sup\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"char\" char=\"\u0026times;\" colname=\"c3\"\u003e\u003cp\u003e2.63\u0026times;10\u003csup\u003e14\u003c/sup\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c4\"\u003e\u003cp\u003e21.1\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c5\"\u003e\u003cp\u003e1.13\u0026times;10\u003csup\u003e3\u003c/sup\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c6\"\u003e\u003cp\u003e8.87\u0026times;10\u003csup\u003e\u0026minus;\u0026thinsp;4\u003c/sup\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c7\"\u003e\u003cp\u003en-type\u003c/p\u003e\u003c/td\u003e\u003c/tr\u003e\u003ctr\u003e\u003ctd align=\"left\" colname=\"c1\"\u003e\u003cp\u003e4% Ni- MoS\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"char\" char=\"\u0026times;\" colname=\"c2\"\u003e\u003cp\u003e3.261\u0026times;10\u003csup\u003e4\u003c/sup\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"char\" char=\"\u0026times;\" colname=\"c3\"\u003e\u003cp\u003e1.91\u0026times;10\u003csup\u003e14\u003c/sup\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c4\"\u003e\u003cp\u003e248\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c5\"\u003e\u003cp\u003e1.31\u0026times;10\u003csup\u003e2\u003c/sup\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c6\"\u003e\u003cp\u003e7.61\u0026times;10\u003csup\u003e\u0026minus;\u0026thinsp;3\u003c/sup\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c7\"\u003e\u003cp\u003en-type\u003c/p\u003e\u003c/td\u003e\u003c/tr\u003e\u003ctr\u003e\u003ctd align=\"left\" colname=\"c1\"\u003e\u003cp\u003e6% Ni- MoS\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"char\" char=\"\u0026times;\" colname=\"c2\"\u003e\u003cp\u003e6.670\u0026times;10\u003csup\u003e5\u003c/sup\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"char\" char=\"\u0026times;\" colname=\"c3\"\u003e\u003cp\u003e9.36\u0026times;10\u003csup\u003e12\u003c/sup\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c4\"\u003e\u003cp\u003e21.9\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c5\"\u003e\u003cp\u003e3.05\u0026times;10\u003csup\u003e4\u003c/sup\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c6\"\u003e\u003cp\u003e3.28\u0026times;10\u003csup\u003e\u0026minus;\u0026thinsp;5\u003c/sup\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c7\"\u003e\u003cp\u003en-type\u003c/p\u003e\u003c/td\u003e\u003c/tr\u003e\u003ctr\u003e\u003ctd align=\"left\" colname=\"c1\"\u003e\u003cp\u003e8% Ni- MoS\u003csub\u003e2\u003c/sub\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"char\" char=\"\u0026times;\" colname=\"c2\"\u003e\u003cp\u003e3.506\u0026times;10\u003csup\u003e5\u003c/sup\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"char\" char=\"\u0026times;\" colname=\"c3\"\u003e\u003cp\u003e1.78\u0026times;10\u003csup\u003e13\u003c/sup\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c4\"\u003e\u003cp\u003e2.13\u0026times;10\u003csup\u003e5\u003c/sup\u003e\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c5\"\u003e\u003cp\u003e1.64\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c6\"\u003e\u003cp\u003e0.608\u003c/p\u003e\u003c/td\u003e\u003ctd align=\"left\" colname=\"c7\"\u003e\u003cp\u003en-type\u003c/p\u003e\u003c/td\u003e\u003c/tr\u003e\u003c/tbody\u003e\u003c/colgroup\u003e\u003c/table\u003e\u003c/div\u003e\u003c/p\u003e\u003cp\u003eThe temperature-dependent longitudinal electrical resistance, represented as \u003cem\u003eρ\u003c/em\u003e\u003csub\u003e\u003cem\u003exx\u003c/em\u003e\u003c/sub\u003e(\u003cem\u003eT\u003c/em\u003e), was evaluated at various applied magnetic fields ranging from 0 T to 6 T for nanosheets of 4% Ni-doped MoS\u003csub\u003e2\u003c/sub\u003e as illustrated in Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e (a) at the temperature range of 100\u0026ndash;300 K. The resistivity measurement was conducted on strip-shaped pellets with dimensions 2.5 \u0026times; 2.5 \u0026times; 1.5 mm\u003csup\u003e3\u003c/sup\u003e (length \u0026times; width \u0026times; thickness). At 0T, resistivity decreases monotonically with increasing temperature, indicating semiconducting behavior at low T. The resistivity of 4% Ni-doped MoS\u003csub\u003e2\u003c/sub\u003e decreases exponentially with increasing temperature, reflecting thermally activated semiconducting behavior at low temperatures and a semiconductor-to-metal-like transition around 200\u0026ndash;250 K as shown in inset Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e (a). With the application of magnetic field (1-6T), the overall resistivity values increase, and the transition shifts toward higher resistivity values, suggesting magnetic field-induced scattering of charge carriers. The R-T behavior of 4% Ni-doped MoS₂ reveals that Ni incorporation introduces impurity levels and localized states that significantly influence carrier transport [\u003cspan citationid=\"CR42\" class=\"CitationRef\"\u003e42\u003c/span\u003e]. At higher temperatures, thermally activated carriers dominate, leading to a steep decrease in resistivity. However, the resistivity upturn at lower temperatures may be attributed to carrier localization, strong Coulomb interactions, or Ni-related defect scattering. The R\u0026ndash;T curve shows a resistivity upturn only under an applied magnetic field, indicating that low-temperature transport in Ni-doped MoS₂ is dominated by spin-dependent scattering [\u003cspan citationid=\"CR43\" class=\"CitationRef\"\u003e43\u003c/span\u003e]. This behavior is consistent with the Kondo effect, where magnetic impurities scatter conduction electrons. In zero field, this scattering is weak or masked by other conduction processes, but the magnetic field aligns the impurity spins, enhancing scattering and producing the observed resistivity peaks. The observed shift in resistivity under magnetic field reflects the suppression of carrier mobility due to enhanced Lorentz force-induced scattering. The positive magnetoresistance suggests weak localization or Kondo-like scattering, consistent with Ni introducing localized magnetic moments [\u003cspan citationid=\"CR44\" class=\"CitationRef\"\u003e44\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR45\" class=\"CitationRef\"\u003e45\u003c/span\u003e]. Thus, Ni doping not only tunes the semiconductor-metal transition in MoS\u003csub\u003e2\u003c/sub\u003e but also enhances its magneto transport response.\u003c/p\u003e\u003cp\u003eFigure \u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e (b) displayed the field-dependent magnetoresistance (MR) of 4% Ni-doped MoS₂ at 250 K exhibits an asymmetric hysteresis loop with respect to the \u0026plusmn;\u0026thinsp;6T magnetic field. In this case the asymmetric features meaning different values of ρ(H) for opposite H polarities. We define MR(%)\u0026thinsp;=\u0026thinsp;100 \u0026times; ((ρ(H)-ρ(0))/ρ(0)) here [\u003cspan additionalcitationids=\"CR43 CR44\" citationid=\"CR42\" class=\"CitationRef\"\u003e42\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR45\" class=\"CitationRef\"\u003e45\u003c/span\u003e]. Unlike the symmetric MR response expected for non-magnetic semiconductors, the present system demonstrates strong sweep-direction dependence, confirming the role of dopant-induced magnetic interactions in governing transport. At low fields, MR(%) varies nonlinearly, and the forward and reverse field sweeps do not coincide, giving rise to a distinct hysteresis window [\u003cspan additionalcitationids=\"CR47 CR48\" citationid=\"CR46\" class=\"CitationRef\"\u003e46\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR49\" class=\"CitationRef\"\u003e49\u003c/span\u003e]. This behavior is attributed to the presence of localized Ni-induced magnetic moments, which interact with charge carriers and give rise to spin-dependent scattering [\u003cspan additionalcitationids=\"CR43 CR44 CR45 CR46 CR47 CR48 CR49\" citationid=\"CR42\" class=\"CitationRef\"\u003e42\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR50\" class=\"CitationRef\"\u003e50\u003c/span\u003e]. The irreversibility between forward and reverse scans reflects the partial pinning and relaxation of these magnetic moments during field cycling. Quantitatively, the MR(%) reaches approximately \u0026minus;\u0026thinsp;10.22% under negative field and about\u0026thinsp;+\u0026thinsp;23.36% under positive field at 60 kOe. The asymmetry between positive and negative MR(%) is a clear indication that both ordinary MR(orbital scattering due to Lorentz force) and extraordinary MR (from localized magnetic clusters and spin polarization) coexist in the system. This non-reciprocal MR response is a hallmark of systems with granular ferromagnetism, exchange-bias-like coupling, or spin-orbit scattering, which can introduce direction-dependent resistivity changes. The overall positive MR trend highlights that carrier mobility is suppressed by field-induced orbital scattering, while the negative MR contribution suggests field-assisted suppression of spin scattering in certain configurations. The competition and imbalance between these two mechanisms lead to the asymmetric hysteresis observed. Such asymmetric MR loops in 4%Ni-MoS\u003csub\u003e2\u003c/sub\u003e provide strong evidence for the emergence of magnetically active states coupled with transport in the 2D host lattice. H. Zhang \u003cem\u003eet al.\u003c/em\u003e [\u003cspan citationid=\"CR51\" class=\"CitationRef\"\u003e51\u003c/span\u003e] theoretically predicted, using DFT calculations, a negative magnetoresistance of -13.79% at 300 K for 3-layer MoS\u003csub\u003e2\u003c/sub\u003e/Ni(fcc). Similarly, W. Jie \u003cem\u003eet al.\u003c/em\u003e [\u003cspan citationid=\"CR52\" class=\"CitationRef\"\u003e52\u003c/span\u003e] experimentally demonstrated that monolayer MoS\u003csub\u003e2\u003c/sub\u003e exhibits magnetoresistance values up to -12.7%. In comparison, our experimental measurements reveal a negative magnetoresistance of -10.22% at 250 K, which is consistent with the theoretical trend, despite slight differences in magnitude and measurement temperature [\u003cspan additionalcitationids=\"CR44 CR45 CR46 CR47 CR48 CR49 CR50 CR51\" citationid=\"CR43\" class=\"CitationRef\"\u003e43\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR52\" class=\"CitationRef\"\u003e52\u003c/span\u003e].\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003c/div\u003e\u003cdiv id=\"Sec9\" class=\"Section2\"\u003e\u003ch2\u003e3.6 Morphological study\u003c/h2\u003e\u003cp\u003eFigure \u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e (a-c) presents HR-TEM micrographs of 2% Ni-doped MoS\u003csub\u003e2\u003c/sub\u003enanosheets, while Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e(d) shows the corresponding SAED pattern. The low-magnification TEM image (Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003ea) reveals sheet-like morphologies with lateral dimensions in the nanometer to sub-micrometer range. At higher magnification (Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003eb), uniformly distributed Ni quantum dots can be observed decorating the MoS\u003csub\u003e2\u003c/sub\u003enanosheets. The high-resolution TEM image (Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003ec) shows well-resolved lattice fringes corresponding to MoS\u003csub\u003e2\u003c/sub\u003ecrystalline planes, along with regions of reduced fringe contrast, suggesting partial amorphization. The SAED pattern (Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003ed) exhibits distinct concentric diffraction rings, indicative of a polycrystalline structure. This observation aligns with XRD analysis of the HRTEM image, which revealed characteristic lattice spacings of MoS\u003csub\u003e2\u003c/sub\u003e, together with variations likely arising from Ni incorporation and associated lattice distortion [\u003cspan citationid=\"CR38\" class=\"CitationRef\"\u003e38\u003c/span\u003e, \u003cspan citationid=\"CR48\" class=\"CitationRef\"\u003e48\u003c/span\u003e]. The coexistence of ordered and disordered regions implies that Ni doping affects the crystallinity, potentially introducing strain and altering local stacking sequences [\u003cspan citationid=\"CR39\" class=\"CitationRef\"\u003e39\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR40\" class=\"CitationRef\"\u003e40\u003c/span\u003e, \u003cspan citationid=\"CR47\" class=\"CitationRef\"\u003e47\u003c/span\u003e].Elemental analysis using energy-dispersive spectroscopy (EDS), as presented in Fig.\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e8\u003c/span\u003e (a-d), reveals that the pure MoS\u003csub\u003e2\u003c/sub\u003e sample contains 49.62 at% Mo and 50.38 at% S. Upon 2% Ni doping, the composition changes markedly to 61.55 at% Mo, 36.63 at% S and 1.82 at% Ni. These results, obtained from point EDS analysis (Fig.\u0026nbsp;\u003cspan refid=\"Fig8\" class=\"InternalRef\"\u003e8\u003c/span\u003ea, c), indicate a significant reduction in sulphur content and a corresponding increase in molybdenum, suggesting that Ni incorporation alters the stoichiometry and possibly induces partial sulphur loss or oxygen incorporation [\u003cspan additionalcitationids=\"CR50 CR51\" citationid=\"CR49\" class=\"CitationRef\"\u003e49\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR52\" class=\"CitationRef\"\u003e52\u003c/span\u003e].\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003cp\u003e\u003c/p\u003e\u003c/div\u003e"},{"header":"4 Conclusion","content":"\u003cp\u003eThis study demonstrates that Ni doping significantly modifies the structural, vibrational, optical, and electronic transport properties of MoS\u003csub\u003e2\u003c/sub\u003e nanostructures. XRD and Raman analyses reveal lattice distortions and interlayer coupling, while PL confirms tunable excitonic behavior with doping concentration. FTIR validates Mo-S bonding, and TEM/EDS confirm nanosheet morphology with Ni quantum dot decoration and stoichiometric changes. Hall measurements indicate n-type conduction, with carrier concentration, mobility, and resistivity strongly dependent on Ni content. The combined R-T and MR(%) measurements on 4% Ni-doped MoS₂ provide new insights into its magneto-transport behavior. The R-T data confirm a thermally activated semiconducting state with a transition to metallic-like conduction near 250 K, while the field-dependent shift highlights the role of magnetic scattering in transport. The MR-H curves display a clear asymmetric hysteresis, with magnetoresistance values of -10.22% and +\u0026thinsp;23.36% under negative and positive fields, respectively, indicating strong coupling between charge carriers and localized Ni moments.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003cstrong\u003eConflicts of Interest:\u003c/strong\u003e The authors declare that they have no conflicts of interest.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eAcknowledgments:\u003c/strong\u003e The authors sincerely thank Dr.Vasant Sathe, and Devedra Kumar, UGC-DAE CSR, Indore, India, for his invaluable assistance with the Raman shift and magnetoresistance (R-T, MR-H) measurements respectively.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eAuthor contribution statement:\u0026nbsp;\u003c/strong\u003eAll authors have contributed equally to the research and preparation of this work.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eFunding:\u0026nbsp;\u003c/strong\u003eThis research was funded by BARTI through a fellowship awarded to CDK (Award Letter No: BARTI/Fellowship/BANRF-2021/2135).\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eData availability statement:\u003c/strong\u003e The data supporting the findings of this study are available from the corresponding author upon reasonable request.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\n\u003cli\u003eJ. 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Hao, ACS Nano 11 (2017) 6950.\u003c/li\u003e\n\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":true,"highlight":"","institution":"","isAcceptedByJournal":true,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true},"keywords":"Mobility, transport property, Hall Effect, Resistivity","lastPublishedDoi":"10.21203/rs.3.rs-7595921/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-7595921/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003ePure and Ni doped MoS\u003csub\u003e2\u003c/sub\u003e (Mo\u003csub\u003e1\u0026thinsp;\u0026minus;\u0026thinsp;x\u003c/sub\u003eNi\u003csub\u003ex\u003c/sub\u003eS\u003csub\u003e2\u003c/sub\u003e at x\u0026thinsp;=\u0026thinsp;0, 2, 4, 6, and 8%) nanosheets were synthesized via hydrothermal method to study the effect of Ni on their structural, optical, morphological, and transport properties. XRD confirmed the samples having hexagonal phase, with peak shifts and disappearance of the (002) reflection at higher doping levels, indicating lattice strain and reduced crystallinity supported by Raman spectra. HR-TEM micrographs confirm the formation of nanosheets decorated with Ni quantum dots. PL spectra exhibited A and B exciton peaks at ~\u0026thinsp;797 nm and ~\u0026thinsp;689 nm, with Ni doping affecting exciton dynamics and non-radiative recombination. Hall measurements shows n-type conduction in all samples, with carrier concentration and mobility strongly dependent on Ni content. Low doping (2%) reduces mobility and increases resistivity, while higher doping (8%) mobility (~\u0026thinsp;2.13\u0026times;10⁵ cm\u0026sup2;/V\u0026middot;s) and conductivity (0.608 S/cm) increases, induces metallic-like behavior with very high mobility. The R-T behavior of 4% Ni-doped MoS\u003csub\u003e2\u003c/sub\u003e a semiconductor-to-metal-like transition near 220\u0026ndash;250 K, with resistivity decreasing exponentially with temperature in the semiconducting regime and shifting to higher resistivity under applied magnetic field, confirming field-induced suppression of carrier mobility. It demonstrates a distinctive asymmetric MR(H) hysteresis with significant positive and negative MR contributions, confirming the coexistence of orbital and spin-dependent scattering mechanisms. The asymmetry (-10.22% Vs 23.36%) strongly evidences the role of localized Ni moments and defect-induced magnetic states in modulating carrier transport.\u003c/p\u003e","manuscriptTitle":"Asymmetric Magnetoresistance and Ultrafast Carrier Transport in Ni-Doped MoS2 Nanosheets","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2025-10-06 16:12:19","doi":"10.21203/rs.3.rs-7595921/v1","editorialEvents":[{"type":"communityComments","content":0}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true}}],"origin":"","ownerIdentity":"c2f19f01-996e-4fbd-86be-892b88ec75dc","owner":[],"postedDate":"October 6th, 2025","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"posted","subjectAreas":[],"tags":[],"updatedAt":"2025-12-01T16:07:06+00:00","versionOfRecord":{"articleIdentity":"rs-7595921","link":"https://doi.org/10.1007/s10854-025-16254-0","journal":{"identity":"journal-of-materials-science-materials-in-electronics","isVorOnly":false,"title":"Journal of Materials Science: Materials in Electronics"},"publishedOn":"2025-11-26 15:58:07","publishedOnDateReadable":"November 26th, 2025"},"versionCreatedAt":"2025-10-06 16:12:19","video":"","vorDoi":"10.1007/s10854-025-16254-0","vorDoiUrl":"https://doi.org/10.1007/s10854-025-16254-0","workflowStages":[]},"version":"v1","identity":"rs-7595921","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-7595921","identity":"rs-7595921","version":["v1"]},"buildId":"8U1c8b4HqxoKbykW_rLl7","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}