Ni0.05Ti1.95Nb10O29: an advanced anode material for high-performance lithium-ion storage

Ni0.05Ti1.95Nb10O29: an advanced anode material for high-performance lithium-ion storage | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Research Article Ni 0.05 Ti 1.95 Nb 10 O 29 : an advanced anode material for high-performance lithium-ion storage xiuli chen, Mingru Su, Xueli Chen, Pei Cui, Yu Zhou, Yunxuan Ji, and 2 more This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-3786761/v1 This work is licensed under a CC BY 4.0 License Status: Published Journal Publication published 24 Apr, 2024 Read the published version in Ionics → Version 1 posted 9 You are reading this latest preprint version Abstract Ti 2 Nb 10 O 29 (TNO) has garnered significant research attention due to its high specific capacity and excellent safety features, positioning it as a promising anode material for lithium-ion batteries (LIBs). Nevertheless, its rate capability is significantly hampered by poor electronic and ionic conductivity. In this paper, Ni 2+ doping has been first applied to address these issues. A series of Ni 2+ doped TNO (Ni x -TNO ( x = 0.03, 0.05, 0.07) electrode materials have been prepared to unveil the effects of Ni 2+ content. The experimental results unveil that Ni 2+ doping maintains the Wadsley-Roth shear structure of TNO while augmenting the single-cell volume and introducing additional oxygen vacancies in TNO. This generates a wider diffusion path and more active sites for lithium ions (Li + ). Besides, the introduction of Ni 2+ can alter the conductive field distribution of TNO, giving rise to a much higher electronic conductivity of Ni x -TNO. Among the synthesized Ni x -TNO, Ni 0.05 -TNO shows the best electrochemical performance, demonstrating a reversible capacity of 306 mAh g –1 with a Coulombic efficiency of 91.46% in the first cycle at 0.1 C and 146.19 mAh g –1 at 10 C after 500 cycles. Lithium-ion batteries Ti2Nb10O29 Ni2+ doping high-rate capability Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 1. Introduction To meet the urgent needs of human beings for higher energy density and safety performance of lithium-ion batteries, there are higher requirements for electrode materials[ 1 , 2 ]. The safety concern related to graphite, arising from the formation and growth of lithium dendrites at low working potentials, has yet to be adequately addressed[ 3 , 4 ]. Therefore, the research on high-voltage new anode materials is crucial to the development of lithium-ion batteries [ 5 , 6 ]. Previous studies showed that metal oxides are promising anode materials for LIBs since they can maintain structural stability during Li + intercalation/deintercalation [ 7 – 10 ]. Recently, Ti 2 Nb 10 O 29 (TNO) has gained significant attention as a high-voltage intercalation anode material [ 11 , 12 ]. Monoclinic TNO has a 3×4×∞ ReO 3 -type phase structure built by octahedrons of NbO 6 and TiO 6 , which can provide an open channel and stable structure for Li + intercalation[ 13 ]. Beyond that, TNO has three pairs of redox couples (Ti 4+ /Ti 3+ , Nb 5+ /Nb 4+ , and Nb 4+ /Nb 3+ ), which can contribute 22 electrons transfer per unit of chemistry, resulting in a theoretical specific capacity of 396 mAh g –1 [ 14 , 15 ]. However, the electrochemical performance of TNO is constrained by its intrinsic issues of poor electronic conductivity and a low Li-ion (Li + ) diffusion coefficient [ 16 ]. To address these issues, considerable research endeavors have been focused on designing and synthesizing nanostructures exhibiting various morphologies. The nanostructures with large specific surface areas and short distances of ion transport can facilitate the electrochemical reactions kinetics[ 17 – 21 ]. Besides, coating with other conductive materials was also applied to improve the electronic conductivity. Unfortunately, this method only enhances inter-particle conductivity and cannot alter the poor intrinsic electronic conductivity of TNO[ 22 ]. In addition, it lowers both the bulk and capacity densities of the material[ 23 ]. Moreover, the synthesis process of nanoparticles is intricate and requires significant time investment, making it hard to industrialization[ 24 ]. In contrast, micron particles are cheaper to synthesize and more feasible to produce. Up to now, some studies have been done on micron-sized TNO from the perspective of structural modification. Oxygen vacancies are common means to improve the crystal structure, Lin[ 25 ] synthesized a defective TNO (Ti 2 Nb 10 O 27.1 ) which shows high Li + diffusion coefficients far exceeding the original samples by a factor of six. In addition, ion doping is also an effective way to improve the electrochemical properties[ 23 ]. Wu[ 26 ] found that replacing a portion of Nb 5+ ions with Ti 4+ and W 6+ in TNO could lower the crystallinity and induce the generation of an amorphous phase. These can enhance ion transport and give rise to an isotropic Li + diffusion. Zheng[ 27 ] used Fe substitution to regulate the entropy, which could effectively lower the particle size and broaden the ion transport path. Nevertheless, the effect of other dopant ions on TNO has been rarely studied. Inspired by Fe substitution, Ni and Fe are in the same group of the periodic table. Following the pattern observed with Fe, the ionic radius of Ni 2+ (0.69 Å) is larger than that of Nb 5+ (0.64 Å) and Ti 4+ (0.61 Å) ions. Thus, the introduction of Ni 2+ might increase the cell volume which may offer an expanded pathway for Li + diffusion. Due to the empty 3d/4d orbitals of Ti/Nb, TNO demonstrates poor intrinsic electronic conductivity, Ni 2+ (t 6 2g e 2 g ) has two unpaired free electrons in the 3d orbitals which can introduce free electrons for the crystal, thus may contribute to the electronic conductivity. In addition, more oxygen vacancies may be generated to keep the structure electrically neutral, which can provide more lattice channels for ion transport, thus contributing to the Li + diffusion[ 3 , 20 ]. Here, we prepared Ni 2+ doped TNO (Ni x -TNO, x = 0, 0.03, 0.05, and 0.07) materials using a simple one-step solid-state reaction approach. Various in-depth analysis was carried out to systematically explore the beneficial impacts of Ni doping on the crystal structure and electrochemical properties. The results show that Ni 2+ can widen the ion transport channel and improve the diffusion coefficient of Li + in the matrix material. Among the various Ni x -TNO materials, Ni 0.05 -TNO displayed superior rate performance (181.76 mAh g –1 at 30 C) and outstanding durability, maintaining a substantial capacity of 146.19 mAh g –1 after 500 cycles, with an extremely low capacity decay of only 0.04% per cycle. 2. Experimental details 2.1 Materials Synthesis The Ni x -TNO samples were synthesized via a conventional one-step solid-state reaction with Nb 2 O 5 powder, anatase TiO 2 and NiO. To obtain Ni x -TNO, stoichiometric amounts of the raw materials were ball-milled in the planetary mill at a rotational speed of 400 rpm for 8 h. Ultimately, the obtained powder was subjected to heating at 1000 ℃ with a heating rate of 5 ℃/min, maintained for 10 hours in air, and then naturally cooled to room temperature. The Ti 2 Nb 10 O 29 material was prepared by using the same process. 2.2 Materials Characterization As-calcined powder crystal structures were characterized by powder X-ray diffraction (XRD) (Bruker D8 Advance, Germany, Cu K radiation source = 1.541 Å). Raman spectra were obtained from a Raman spectrometer (LabRAM HR, Horiba jobinyvon). Using transmission electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM, JEM-2100F), the morphologies (sizes and microstructures) were evaluated. The elemental distribution of the sample was detected using energy-dispersive X-ray spectroscopy (EDS) combined with high-resolution transmission electron microscopy. X-ray photoelectron spectroscopy (XPS, Thermo VG Scientific, VG MultiLab 2000) was utilized to analyze the surface chemical composition and valence state. 2.3 Electrochemical Measurement CR2025-type coin cells were assembled in a glove box filled with dry argon for the evaluation of electrochemical performances. A homogeneous slurry was prepared by thoroughly mixing 70wt% calcined powder, 10wt% polyvinylidene fluoride (PVDF), and 20wt% calcined powder in N-methyl-2-pyrrolidone (NMP). The slurry was uniformly cast onto copper foil and dried at 65°C for 10 hours, resulting in a loading density of approximately 1.0 mg cm − 2 for the electrode. Lithium foil served as the reference electrode for the battery. A microporous polypropylene film (Celgard 2500) was employed as the separator. The electrolyte comprised a 1 M LiPF 6 (DAN VEC) solution in a 1:1 weight ratio of ethylene carbonate (EC) to diethyl carbonate (DEC). Electrostatic discharge-charge tests were conducted using a multi-channel battery testing system (Neware CT-3008, China) at various current rates within the potential range of 3.0–1.0 V. Measurements of cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) were conducted using the electrochemical workstation (Chenhua, ChI660E, China). 3. Results and discussion Table 1 The detailed refined structural parameters for TNO and Ni 0.05 -TNO. Product a/Å b/Å c/Å α /° β /° γ /° Volume/Å 3 wRp Rp TNO 15.518 3.813 20.542 90 113.05 90 1117.59 0.062 0.045 Ni 0.05 -TNO 15.566 3.818 20.559 90 113.24 90 1123.63 0.061 0.042 Firstly, we investigate the crystal structure of Ni x -TNO ( x = 0.03, 0.05, and 0.07). As shown in Fig. 1 a, the diffraction peaks observed in Ni x -TNO index well to monoclinic phase TNO (space: A/2m, PDF#72–0159), without impurity phases of TiO 2 or Nb 2 O 5 . This indicates the successful synthesis of TNO and Ni doping does not change the space group. With Ni content increasing from 0 to 0.07, the position of the diffraction peak of the (020) crystal surface moves to smaller angles (Fig. 1 b), which suggests an increase of interplanar spacing at a higher Ni doping content. Besides, with the increase of Ni 2+ content, the diffraction peak intensity also decreases, indicating that Ni 2+ doping can effectively reduce the crystallinity of the material, which might reduce the Li + diffusion barrier[ 26 ]. However, excessive doping gives rise to the variation of crystal structure, as unveiled from the disappeared (11 \(\stackrel{\text{-}}{\text{1}}\) ) peak of Ni 0.07 -TNO in Fig. 1 c. More specifically, Fig. 1 d-e presents the refinement results of the XRD patterns for TNO and Ni 0.05 -TNO using the Rietveld method, accompanied by comprehensive structural parameters provided in Table 1 . It is seen that Ni 0.05 -TNO (1123.63 Å 3 ) has a larger volume of unit cells than TNO (1117.59 Å 3 ). This can be attributed to the fact that Ni 2+ has a larger ionic radius when compared to Ti 4+ and Nb 5+ . The larger volume of the unit cell can provide a wider diffusion channel for Li + diffusion (Fig. 1 h and 1 i). Further, Raman spectroscopy was applied to get insight into the bonding characteristics of the crystal structures. As shown in Fig. 1 f, the bands occurring at 896 and 1000 cm –1 correspond to the tensile vibration of NbO 6 [ 28 ]. The bands of 544 and 646 cm –1 refer to the vibration of the Ti − O bonds of TiO 6 [ 26 ]. As for the bands at 270 and 349 cm –1 , they are associated with symmetric and asymmetric bending motions of O-Ti-O and O-Nb-O bridge bonds, respectively[ 7 ]. However, the Ti–O vibrational peak of Ni 0.05 -TNO exhibits a slight blue shift, providing evidence for changes in the internal chemical environment, maybe attributed to increased cation-oxygen bonding and the development of oxygen vacancies[ 3 ]. The morphologies and particle sizes of each sample are examined through scanning electron microscopy (SEM). As depicted in Fig. 2 a-h, all samples present irregularly reunion particles, and the particle size ranges from 0.2 to 1 µm. Compared to the original sample, Ni x -TNO particles are more dispersed. To further reveal the morphological structures of Ni x -TNO, TEM characterizations were conducted (Fig. 3 a-i). The diffraction patterns in Fig. 3 b and 3 f unveil that TNO and Ni 0.05 -TNO are typical single-crystals. The different orientations of the crystal surfaces can be seen from Fig. 3 c and 3 g. After further amplification and analysis, the specific parameters of the crystal surface can be obtained (Fig. 3 d and 3 h). From the lattice fringes of (400) and (600) crystal planes of TNO and Ni 0.05 -TNO, their interlayer spacings are 0.354 and 0.237 nm respectively, which agrees well with the findings from XRD analyses. The homogeneous distribution of Ti, Nb, O, and Ni can be seen from the TEM-EDS elemental mapping (Fig. 3 i), suggesting the successful introduction of Ni 2+ into TNO. Then, XPS is utilized to investigate the surface composition and valence states of Ni 0.05 -TNO and TNO. As seen in Fig. 4 a, the full XPS spectrum of Ni 0.05 -TNO indicates the existence of Ti, Nb, O, and Ni, revealing that Ni has been successfully doped in Ni 0 . 05 -TNO. This can also be verified from the characteristic peaks of Ni 2+ in Ni 0 . 05 -TNO (Fig. 4 b). Similar results can be observed from TNO excluding the absence of the Ni element. As seen in Fig. 4 c-d, for the TNO, a couple of peaks located at 464.02 and 458.26 eV of the Ti spectrum originate from Ti 2p 1/2 and Ti 2p 3/2 , suggesting the existence of Ti 4+ . The Nb spectrum of TNO at 209.55 and 206.8 eV are indexed into Nb 3d 5/2 and Nb 3d 3/2 of Nb 5+ , separately. Specifically, the peaks of both Ti 2p and Nb 3d shift towards lower binding energy positions following Ni doping, which unveils more Ti 3+ and Nb 4+ in Ni 0.05 -TNO[ 5 ]. The presence of Ti 3+ and Nb 4+ can be attributed to the charge distribution caused by Ni 2+ doping[ 16 ]. From Fig. 4 e, Ni 0.05 -TNO shows a broader oxygen-deficient region in comparison with TNO, unveiling the more missing lattice O in Ni 0.05 -TNO[ 29 ]. This can also be reflected from the electron paramagnetic resonance (EPR). As illustrated in Fig. 4 f, both TNO and Ni 0.05 -TNO display an EPR signal at g = 2.0 (typical signal of oxygen vacancies) and Ni 0.05 -TNO demonstrates a stronger peak intensity than that of TNO, which indicates the existence of an increased number of oxygen vacancies in Ni 0.05 -TNO. The cyclic voltammetry (CV) was used to investigate the kinetic properties during the corresponding redox process in the voltage range of 1.0‒3.0 V for the first three cycles with the sweep of 0.2 mV s –1 . As shown in Fig. 5 a and 5 b, for each cell, the locations of cathodic peaks in the CV during the first cycle deviate from those observed in the subsequent two cycles, which is due to the change of electronic structure of TNO electrode induced by the distortion of TiO 6 or NbO 6 octahedra and the irreversible consumption of Li + during the process of Li + insertion[ 3 , 30 ]. The CV curves consistently display substantial sharp redox peaks at 1.55‒1.75 V, associated with the Nb 5+ /Nb 4+ redox couple, and small gentle peaks near 1.9 V, corresponding to the Ti 4+ /Ti 3+ redox couple. The broad peak at 1.0‒1.5 V refers to the Nb 4+ /Nb 3+ redox couple. Ni 0.05 -TNO exhibits reduced redox potential differences compared to pure TNO, demonstrating superior kinetic reversibility after Ni doping[ 39 ]. Figure 5 c illustrates the charge and discharge profiles of the initial cycle of all samples at a constant current density of 0.1 C. The charge and discharge curves can be divided into three regions according to the inflection point, which are consistent with the redox changes observed during the CV experiments. The regions of A and C correspond to the solid solution of Li + in TNO[ 32 ]. The plateau in region B involves a phase of two-phase transition corresponding to a redox reaction in 1.65v[ 27 , 33 ]. In this region, a longer reaction plateau in Ni 0.05 -TNO implies more capacity contribution, most likely originating from the more active sites brought about by oxygen vacancies. It is seen that the discharge capacity and Coulombic efficiency of the doped sample at small Ni content ( x = 0.03 and 0.05) are superior to those of the original sample. Ni 0.05 -TNO exhibits the most superior electrochemical performance, with the first discharge capacity and Coulombic efficiency of 306 mAh g –1 and 91.46%, respectively. This could be attributed to the fact that the doped samples exhibit smaller average particle sizes and higher (ionic and electronic) conductivities[ 31 ]. Thus, Ni 2+ doping has a positive effect on the surface reaction kinetics of Li + . Figure 5 d illustrates the rate capabilities of Ni x -TNO ( x = 0, 0.03, 0.05 and 0.07) at varied current densities. The capacities of Ni 0.05 -TNO at 0.5, 1, 2, 5, 10, 20, and 30 C are 265.68, 251.16, 239.78, 223.61, 204.89, 185.63, and 181.76 mAh g –1 , respectively, which significantly elevated in comparison to TNO (202.70, 189.90, 180.52, 170.09, 158.89, 147.43, and 138.62 mAh g –1 ). Moreover, the cyclic stability of Ni x -TNO at a large current rate of 10 C was evaluated (Fig. 5 e). It is seen that Ni 0.05 -TNO displays the highest cycling stability among the four samples. The reversible capacity of Ni 0.05 -TNO after 500 cycles is 146.19 mA h g –1 , with a capacity loss of only 0.04% per cycle, while the reversible capacities of other Ni x -TNO samples ( x = 0, 0.03 and 0.07) are 85.31, 125.95, and 81.96 mAh g –1 . The outstanding cyclic stability may be due to the wider Li + diffusion pathway after Ni 2+ doping, which helps stabilize the structure during repeated cycles[ 3 ]. The reason for the poor cycling performance of Ni 0.07 -TNO might be that excessive Ni 2+ doping results in excessive lattice distortion (see Fig. 1 c), which leads to a significant decrease in structural stability. Table 2 Impedance parameters and Li + diffusion coefficients of TNO and Ni x -TNO Product R ct (Ω) σ (Ω s –0.5 ) D ×10 –14 (cm 2 s –1 ) TNO 168.00 132.64 3.51 Ni 0.03 -TNO 55.35 96.32 32.3 Ni 0.05 -TNO 51.42 110.85 37.5 Ni 0.07 -TNO 69.15 37.99 20.7 In order to investigate the nature of ion transport during the charge and discharge processes, we further performed the impedance analysis test (A.C. impedance technique) on the battery. Figure 6 illustrates the Nyquist plots for both TNO and Ni x -TNO after cycling three times at 0.1 C with the fitted equivalent circuit inserted. In Fig. 6 a, a semicircular feature is present in the high-frequency region, which refers to the reactive process of electron transfer during Li + desolvation/adsorption ( R ct ). The low-frequency region is an inclined straight line, the slope of this line is related to the diffusion of Li + in the bulk crystals (Warburg resistance)[ 34 , 35 ]. The specific fitting parameters can be seen in Table 2 , the doped samples demonstrate much smaller R ct (55.35, 51.42 and 69.15 Ω for Ni 0.03 -TNO, Ni 0.05 -TNO and Ni 0.07 -TNO, respectively) than that (168.0 Ω) of the pristine samples. The reason might be that Ni 2+ could optimize the electronic structure of TNO, which facilitates the internal electron transfer, thus contributing to the electronic conductivity [ 36 ]. This can be verified from the obtained conductivity via the four-probe conductivity test. The electronic conductivity (2.2 × 10 –7 s cm –1 ) of Ni 0.05 -TNO is two orders of magnitude higher than that (1 × 10 –9 s cm –1 ) of TNO [ 25 ]. These results unveil that Ni doping is effective in tuning the electronic conductivity of TNO. Then, we explore the diffusion coefficient of Li + via the impedance analysis. The Li + diffusion coefficient is mainly related to the slope of the straight line in the low-frequency region, and the specific diffusion process can be obtained according to the following equation: $${D}_{{\text{L}\text{i}}^{+}}=\frac{{R}^{2}{T}^{2}}{2{A}^{2}{n}^{4}{F}^{4}{C}^{2}{\sigma }^{2}}$$ 1 , In the given expression, R represents the gas constant, T stands for the absolute temperature, A denotes the surface area of the active electrode, n is the number of electrons per molecule, F represents the Faraday constant, C is the molar concentration of Li + , and σ represents the Warburg factor. σ can be estimated based on the plot of the linear fit between Z and the inverse square root of the lower angular frequency (Fig. 6 b). It can be expressed by the following equation: $${\text{Z}}^{{\prime }}\text{ = }{\text{R}}_{\text{s}}\text{+}{\text{R}}_{\text{ct}}\text{+}{\text{σω}}^{\text{-}\text{1/2}}$$ 2 . The Li + diffusion coefficients of Ni x -TNO and TNO are tabulated in Table 2 . The Li + diffusion coefficients of Ni 0.03 -TNO, Ni 0.05 -TNO and Ni 0.07 -TNO are 3.23×10 –13 , 3.75×10 –13 , and 2.07×10 –13 cm 2 s –1 , respectively, which are markedly higher than that (3.51×10 –14 cm 2 s –1 ) of the pristine one. The Ni 0.05 -TNO displays the highest Li + diffusion coefficient. The reason for this phenomenon may be that the lattice distortion caused by Ni 2+ doping gives rise to an increase in the cell volume, which provides a wider channel for Li + diffusion. To further unveil the change of crystal structure during the (de)lithiation process of Ni 0.05 -TNO, the non-in situ XRD tests were conducted for the pole pieces by discharging or charging them to specific voltages at current densities of 0.2 C. Here, four points were respectively selected for the initial charging and discharging processes (Fig. 7 a). As shown in Fig. 7 b, all the samples match well with the monoclinic Ti 2 Nb 10 O 29 and the crystal diffraction peaks are relatively sharp, which suggest a good stability of the crystal structure during the charging and discharging process. Figure 7 c-d illustrates the enlarged (21 \(\stackrel{\text{-}}{\text{5}}\) ), (41 \(\stackrel{\text{-}}{\text{1}}\) ), and (020) crystal planes, and it is seen that the (020) crystal plane shifts to a low angle during discharging and returns to the initial position in the charging process. This unveils the good structural stability of Ni 0.05 -TNO during (de)lithiation. However, the lattice parameters of (21 \(\stackrel{\text{-}}{\text{5}}\) ) and (41 \(\stackrel{\text{-}}{\text{1}}\) ) crystal planes do not change significantly, which is due to that these crystal planes are not the preferential diffusion paths of Li + in Ni 0.05 -TNO[ 37 – 39 ]. 4. Conclusions In this paper, Ni x -TNO samples were synthesized using a simple solid-state method. The influence of Ni 2+ on the structure, morphology and valence distribution of the material was explored through a series of characterizations. According to the experimental results, Ni 0.05 -TNO is the most ideal electrode material. While the crystal structure remains unaffected by a moderate amount of Ni 2+ doping, an increase in cell parameters occurs, creating more extensive diffusion channels and active sites for Li + transport. In addition, the introduction of Ni alters the electronic environment of TNO, greatly improving the conductivity of the material and generating a certain amount of oxygen vacancies. Based on these advantages, Ni 0.05 -TNO exhibits the most favorable electrochemical performance among all samples. A large reversible capacity of 306 mAh g –1 and a high Coulombic efficiency of 91.46% can be reached at 0.1 C. Besides, there is still 146.19 mAh g –1 after 500 cycles at a discharge current of 10 C. The findings in our research offer a fresh perspective on enhancing niobium-based oxide materials for novel lithium-ion anodes. Declarations Conflict of Interest The authors declare no competing financial interest. Author Contribution Xiuli Chen: conceptualization, methodology, investigation, writing - original draft, and data curation. Mingru Su: formal analysis and resources. Xueli Chen: data curation and methodology. Pei Cui: methodology and formal analysis. Yu Zhou: formal analysis. Yunxuan Ji: data curation. Panpan Zhang: validation, supervision, writing - review & editing. Yunjian Liu: visualization, supervision, and funding acquisition. Acknowledgments This research was sponsored by the National Natural Science Foundation of China (52004103, 51974137 and 52304328), the Natural Science Foundation of Jiangsu Province (BK20220534), Jiangsu Double-Innovation PhD Program in 2022 (JSSCBS20221241) and China Postdoctoral Science Foundation (2023M733189). 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J Power Sources 328: 336–344 Gao J, Cheng X, Lou S, et al (2017) Self-doping Ti 1 -x Nb 2+ x O 7 anode material for lithium-ion battery and its electrochemical performance [J]. J Alloys Compd 728: 534–540 Griffith KJ, Seymour ID, Hope M A, et al (2019) Ionic and electronic conduction in TiNb 2 O 7 [J]. Journal of the American Chemical Society 141: 16706–16725 Griffith KJ, Harada Y, Egusa S, et al (2020) Titanium niobium oxide: from discovery to application in fast-charging lithium-ion batteries [J]. Chem Mater 33: 4–18 Cui P, Zhang P, Chen X, et al (2023) Oxygen defect and Cl-doped modulated TiNb 2 O 7 compound with high rate performance in lithium-ion batteries [J]. ACS Appl Mater Interfaces 15: 43745–43755 Additional Declarations No competing interests reported. Cite Share Download PDF Status: Published Journal Publication published 24 Apr, 2024 Read the published version in Ionics → Version 1 posted Editorial decision: Revision requested 03 Mar, 2024 Reviews received at journal 25 Feb, 2024 Reviews received at journal 12 Feb, 2024 Reviewers agreed at journal 17 Jan, 2024 Reviewers agreed at journal 16 Jan, 2024 Reviewers invited by journal 15 Jan, 2024 Editor assigned by journal 29 Dec, 2023 Submission checks completed at journal 29 Dec, 2023 First submitted to journal 21 Dec, 2023 You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. As a division of Research Square Company, we’re committed to making research communication faster, fairer, and more useful. We do this by developing innovative software and high quality services for the global research community. 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Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-3786761","acceptedTermsAndConditions":true,"allowDirectSubmit":false,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":264376089,"identity":"d6189d25-ca1a-46b6-8c54-05330c2b72fb","order_by":0,"name":"xiuli chen","email":"","orcid":"","institution":"Jiangsu University","correspondingAuthor":false,"prefix":"","firstName":"xiuli","middleName":"","lastName":"chen","suffix":""},{"id":264376090,"identity":"5aaac3d6-5900-4b2b-8edd-5898cc3cabbb","order_by":1,"name":"Mingru Su","email":"","orcid":"","institution":"Jiangsu University","correspondingAuthor":false,"prefix":"","firstName":"Mingru","middleName":"","lastName":"Su","suffix":""},{"id":264376091,"identity":"62c4b4d6-f4f6-40b7-8a54-cb1d7206b962","order_by":2,"name":"Xueli Chen","email":"","orcid":"","institution":"Jiangsu University","correspondingAuthor":false,"prefix":"","firstName":"Xueli","middleName":"","lastName":"Chen","suffix":""},{"id":264376092,"identity":"2b48178e-dbb8-4ab3-ab16-61f3cd2cbb26","order_by":3,"name":"Pei Cui","email":"","orcid":"","institution":"Jiangsu University","correspondingAuthor":false,"prefix":"","firstName":"Pei","middleName":"","lastName":"Cui","suffix":""},{"id":264376093,"identity":"c057ed0f-547e-4683-b75f-2fda6fb928d5","order_by":4,"name":"Yu Zhou","email":"","orcid":"","institution":"Jiangsu University","correspondingAuthor":false,"prefix":"","firstName":"Yu","middleName":"","lastName":"Zhou","suffix":""},{"id":264376094,"identity":"e566c34d-f362-455f-a20a-7f74b10b9d9f","order_by":5,"name":"Yunxuan Ji","email":"","orcid":"","institution":"Jiangsu University","correspondingAuthor":false,"prefix":"","firstName":"Yunxuan","middleName":"","lastName":"Ji","suffix":""},{"id":264376095,"identity":"38dde114-ca3f-4955-8ce5-3c7362d9a439","order_by":6,"name":"Panpan Zhang","email":"","orcid":"","institution":"Jiangsu University","correspondingAuthor":false,"prefix":"","firstName":"Panpan","middleName":"","lastName":"Zhang","suffix":""},{"id":264376096,"identity":"191dc84f-b1dc-4672-ab1d-28aeaf95e17e","order_by":7,"name":"yunjian Liu","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAA6ElEQVRIie3PsWvCUBDH8QuBZHk1Hc/B/g0PBHEI/i0ngUwZHDvZFCFZdPfPcHTz0kNdAq4dOtjFrRA3CxXUunXwZSz4vvN9+HEANts/rAFADIBPQZAzVzrsGYl3Jd12c1r2i+kgjuqQS8/9GVNbVPXmpEaC9Mnfc3RSZpJQswu+LGcGQsWkRNcZvbIk+qMBKo7fTYQfMvRcOK8keucCqo6RFMcMlQekpavFSesQOa+guhCoRdSWpJWhRiypGOs48ky/BH4S7b+y4ctik0t1+Al7gS+rmwQeE/qze/P8d2bNxhubzWa78079xFDp1vyD4wAAAABJRU5ErkJggg==","orcid":"","institution":"Jiangsu University","correspondingAuthor":true,"prefix":"","firstName":"yunjian","middleName":"","lastName":"Liu","suffix":""}],"badges":[],"createdAt":"2023-12-21 11:59:25","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-3786761/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-3786761/v1","draftVersion":[],"editorialEvents":[{"content":"https://doi.org/10.1007/s11581-024-05547-9","type":"published","date":"2024-04-24T23:27:18+00:00"}],"editorialNote":"","failedWorkflow":false,"files":[{"id":49075205,"identity":"d8e3c7f5-7d9c-4c12-bffa-3faa3ecf8d56","added_by":"auto","created_at":"2024-01-02 18:22:39","extension":"jpg","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":14625502,"visible":true,"origin":"","legend":"\u003cp\u003e(a) XRD patterns for TNO and Ni\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e-TNO (\u003cem\u003ex \u003c/em\u003e= 0.03, 0.05 and 0.07). Magnification of the (b) (002) and (c) (11\u003cimg width=\"8\" height=\"20\" src=\"file:///C:/Users/rpt0628/AppData/Local/Temp/msohtmlclip1/01/clip_image002.gif\"/\u003e) diffraction peaks. The Rietveld refinement of XRD patterns for (d) TNO and (e) Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO. (f) Raman spectra of TNO and Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO. (g) Crystal structure of monoclinic TNO phases along the b-axis and c-axis. (h) Crystallographic structure of TNO and (i) modified Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO.\u003c/p\u003e","description":"","filename":"floatimage1.jpg","url":"https://assets-eu.researchsquare.com/files/rs-3786761/v1/2f65ff8ba454e1e580713a5b.jpg"},{"id":49075618,"identity":"6f961578-da18-41be-a38c-d6d3cbde11db","added_by":"auto","created_at":"2024-01-02 18:30:39","extension":"jpg","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":321989,"visible":true,"origin":"","legend":"\u003cp\u003eSEM images of (a, e) TNO, (b, f) Ni\u003csub\u003e0.03\u003c/sub\u003e-TNO, (c, g) Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO and (d, h) Ni\u003csub\u003e0.07\u003c/sub\u003e-TNO.\u003c/p\u003e","description":"","filename":"floatimage2.jpg","url":"https://assets-eu.researchsquare.com/files/rs-3786761/v1/7f1607f47bb22647b37795f5.jpg"},{"id":49075206,"identity":"a91930f9-78d3-45b9-b76c-2e52745e39d6","added_by":"auto","created_at":"2024-01-02 18:22:39","extension":"jpg","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":16433385,"visible":true,"origin":"","legend":"\u003cp\u003eHR-TEM images of particle, SAED pattern and lattice view of (a-d) TNO and (e-h) Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO sample, respectively. (i) HRTEM EDS mappings of Ti, Nb, O, and Ni in Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO.\u003c/p\u003e","description":"","filename":"floatimage3.jpg","url":"https://assets-eu.researchsquare.com/files/rs-3786761/v1/dd5bf780395342fc87afb226.jpg"},{"id":49075620,"identity":"8535e6ea-270e-412c-abdd-3f3798a930b1","added_by":"auto","created_at":"2024-01-02 18:30:39","extension":"jpg","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":7529782,"visible":true,"origin":"","legend":"\u003cp\u003e(a) The full XPS spectra of TNO and Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO and high-resolution spectra of (b) Ni 2p and (c) Ti 2p, (d) Nb 3d, and (e) O1s. (f) The EPR spectra of TNO and Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO.\u003c/p\u003e","description":"","filename":"floatimage4.jpg","url":"https://assets-eu.researchsquare.com/files/rs-3786761/v1/3151ff2c4c817a14ab79fb43.jpg"},{"id":49075208,"identity":"a1616742-7070-4685-a791-510287beb7ee","added_by":"auto","created_at":"2024-01-02 18:22:39","extension":"jpg","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":8372722,"visible":true,"origin":"","legend":"\u003cp\u003eCV curves of (a) TNO and (b) Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO in the potential range of 1.0−3.0 V at 0.2 mV s\u003csup\u003e−1\u003c/sup\u003e. (c) The first cycle of charge-discharge curves at 0.1 C,(d) rate performance of all samples and (e) cycling performance at 10 C.\u003c/p\u003e","description":"","filename":"floatimage5.jpg","url":"https://assets-eu.researchsquare.com/files/rs-3786761/v1/a351ccd72336da2776c0b134.jpg"},{"id":49075619,"identity":"6a10930f-da29-489b-9945-da96de22b112","added_by":"auto","created_at":"2024-01-02 18:30:39","extension":"jpg","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":171422,"visible":true,"origin":"","legend":"\u003cp\u003e(a) Typical Nyquist plots and (b) the relationship between the real parts and ω\u003csup\u003e–0.5\u003c/sup\u003e of the as-prepared samples.\u003c/p\u003e","description":"","filename":"floatimage6.jpg","url":"https://assets-eu.researchsquare.com/files/rs-3786761/v1/3c2e6218f8e7ec4524342674.jpg"},{"id":49075203,"identity":"eee45259-6703-41fd-bf7d-6d1b4197175f","added_by":"auto","created_at":"2024-01-02 18:22:39","extension":"jpg","order_by":7,"title":"Figure 7","display":"","copyAsset":false,"role":"figure","size":230473,"visible":true,"origin":"","legend":"\u003cp\u003e(a-d) Ex-situ XRD patterns and corresponding potential curves during the initial charge and discharge process of the Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO electrode.\u003c/p\u003e","description":"","filename":"floatimage7.jpg","url":"https://assets-eu.researchsquare.com/files/rs-3786761/v1/c2e2c9fb735a6da6b54b6050.jpg"},{"id":55694934,"identity":"4a4eb67f-36ea-4c5d-b905-0c7d2bfaf0fd","added_by":"auto","created_at":"2024-05-02 00:54:26","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":1295959,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-3786761/v1/138df734-931c-4be8-83fc-b5c42200582a.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"\u003cp\u003e\u003cstrong\u003eNi\u003c/strong\u003e\u003csub\u003e\u003cstrong\u003e0.05\u003c/strong\u003e\u003c/sub\u003e\u003cstrong\u003eTi\u003c/strong\u003e\u003csub\u003e\u003cstrong\u003e1.95\u003c/strong\u003e\u003c/sub\u003e\u003cstrong\u003eNb\u003c/strong\u003e\u003csub\u003e\u003cstrong\u003e10\u003c/strong\u003e\u003c/sub\u003e\u003cstrong\u003eO\u003c/strong\u003e\u003csub\u003e\u003cstrong\u003e29\u003c/strong\u003e\u003c/sub\u003e\u003cstrong\u003e:\u003c/strong\u003e \u003cstrong\u003ean advanced anode material for high-performance lithium-ion storage\u003c/strong\u003e\u003c/p\u003e","fulltext":[{"header":"1. Introduction","content":"\u003cp\u003eTo meet the urgent needs of human beings for higher energy density and safety performance of lithium-ion batteries, there are higher requirements for electrode materials[\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e, \u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e]. The safety concern related to graphite, arising from the formation and growth of lithium dendrites at low working potentials, has yet to be adequately addressed[\u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e, \u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e4\u003c/span\u003e]. Therefore, the research on high-voltage new anode materials is crucial to the development of lithium-ion batteries [\u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e, \u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e]. Previous studies showed that metal oxides are promising anode materials for LIBs since they can maintain structural stability during Li\u003csup\u003e+\u003c/sup\u003e intercalation/deintercalation [\u003cspan additionalcitationids=\"CR8 CR9\" citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e10\u003c/span\u003e]. Recently, Ti\u003csub\u003e2\u003c/sub\u003eNb\u003csub\u003e10\u003c/sub\u003eO\u003csub\u003e29\u003c/sub\u003e (TNO) has gained significant attention as a high-voltage intercalation anode material [\u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e11\u003c/span\u003e, \u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e12\u003c/span\u003e]. Monoclinic TNO has a 3\u0026times;4\u0026times;\u0026infin; ReO\u003csub\u003e3\u003c/sub\u003e-type phase structure built by octahedrons of NbO\u003csub\u003e6\u003c/sub\u003e and TiO\u003csub\u003e6\u003c/sub\u003e, which can provide an open channel and stable structure for Li\u003csup\u003e+\u003c/sup\u003e intercalation[\u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e]. Beyond that, TNO has three pairs of redox couples (Ti\u003csup\u003e4+\u003c/sup\u003e/Ti\u003csup\u003e3+\u003c/sup\u003e, Nb\u003csup\u003e5+\u003c/sup\u003e/Nb\u003csup\u003e4+\u003c/sup\u003e, and Nb\u003csup\u003e4+\u003c/sup\u003e/Nb\u003csup\u003e3+\u003c/sup\u003e), which can contribute 22 electrons transfer per unit of chemistry, resulting in a theoretical specific capacity of 396 mAh g\u003csup\u003e\u0026ndash;1\u003c/sup\u003e[\u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e14\u003c/span\u003e, \u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e]. However, the electrochemical performance of TNO is constrained by its intrinsic issues of poor electronic conductivity and a low Li-ion (Li\u003csup\u003e+\u003c/sup\u003e) diffusion coefficient [\u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e]. To address these issues, considerable research endeavors have been focused on designing and synthesizing nanostructures exhibiting various morphologies. The nanostructures with large specific surface areas and short distances of ion transport can facilitate the electrochemical reactions kinetics[\u003cspan additionalcitationids=\"CR18 CR19 CR20\" citationid=\"CR17\" class=\"CitationRef\"\u003e17\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e21\u003c/span\u003e]. Besides, coating with other conductive materials was also applied to improve the electronic conductivity. Unfortunately, this method only enhances inter-particle conductivity and cannot alter the poor intrinsic electronic conductivity of TNO[\u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e]. In addition, it lowers both the bulk and capacity densities of the material[\u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e23\u003c/span\u003e]. Moreover, the synthesis process of nanoparticles is intricate and requires significant time investment, making it hard to industrialization[\u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e24\u003c/span\u003e]. In contrast, micron particles are cheaper to synthesize and more feasible to produce.\u003c/p\u003e \u003cp\u003eUp to now, some studies have been done on micron-sized TNO from the perspective of structural modification. Oxygen vacancies are common means to improve the crystal structure, Lin[\u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e] synthesized a defective TNO (Ti\u003csub\u003e2\u003c/sub\u003eNb\u003csub\u003e10\u003c/sub\u003eO\u003csub\u003e27.1\u003c/sub\u003e) which shows high Li\u003csup\u003e+\u003c/sup\u003e diffusion coefficients far exceeding the original samples by a factor of six. In addition, ion doping is also an effective way to improve the electrochemical properties[\u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e23\u003c/span\u003e]. Wu[\u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e] found that replacing a portion of Nb\u003csup\u003e5+\u003c/sup\u003e ions with Ti\u003csup\u003e4+\u003c/sup\u003e and W\u003csup\u003e6+\u003c/sup\u003e in TNO could lower the crystallinity and induce the generation of an amorphous phase. These can enhance ion transport and give rise to an isotropic Li\u003csup\u003e+\u003c/sup\u003e diffusion. Zheng[\u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e] used Fe substitution to regulate the entropy, which could effectively lower the particle size and broaden the ion transport path. Nevertheless, the effect of other dopant ions on TNO has been rarely studied.\u003c/p\u003e \u003cp\u003eInspired by Fe substitution, Ni and Fe are in the same group of the periodic table. Following the pattern observed with Fe, the ionic radius of Ni\u003csup\u003e2+\u003c/sup\u003e (0.69 \u0026Aring;) is larger than that of Nb\u003csup\u003e5+\u003c/sup\u003e (0.64 \u0026Aring;) and Ti\u003csup\u003e4+\u003c/sup\u003e (0.61 \u0026Aring;) ions. Thus, the introduction of Ni\u003csup\u003e2+\u003c/sup\u003e might increase the cell volume which may offer an expanded pathway for Li\u003csup\u003e+\u003c/sup\u003e diffusion. Due to the empty 3d/4d orbitals of Ti/Nb, TNO demonstrates poor intrinsic electronic conductivity, Ni\u003csup\u003e2+\u003c/sup\u003e (t\u003csup\u003e6\u003c/sup\u003e\u003csub\u003e2g\u003c/sub\u003ee\u003csup\u003e2\u003c/sup\u003e\u003csub\u003eg\u003c/sub\u003e) has two unpaired free electrons in the 3d orbitals which can introduce free electrons for the crystal, thus may contribute to the electronic conductivity. In addition, more oxygen vacancies may be generated to keep the structure electrically neutral, which can provide more lattice channels for ion transport, thus contributing to the Li\u003csup\u003e+\u003c/sup\u003e diffusion[\u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e, \u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eHere, we prepared Ni\u003csup\u003e2+\u003c/sup\u003e doped TNO (Ni\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e-TNO, \u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0, 0.03, 0.05, and 0.07) materials using a simple one-step solid-state reaction approach. Various in-depth analysis was carried out to systematically explore the beneficial impacts of Ni doping on the crystal structure and electrochemical properties. The results show that Ni\u003csup\u003e2+\u003c/sup\u003e can widen the ion transport channel and improve the diffusion coefficient of Li\u003csup\u003e+\u003c/sup\u003e in the matrix material. Among the various Ni\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e-TNO materials, Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO displayed superior rate performance (181.76 mAh g\u003csup\u003e\u0026ndash;1\u003c/sup\u003e at 30 C) and outstanding durability, maintaining a substantial capacity of 146.19 mAh g\u003csup\u003e\u0026ndash;1\u003c/sup\u003e after 500 cycles, with an extremely low capacity decay of only 0.04% per cycle.\u003c/p\u003e"},{"header":"2. Experimental details","content":"\u003cdiv id=\"Sec3\" class=\"Section2\"\u003e \u003ch2\u003e2.1 Materials Synthesis\u003c/h2\u003e \u003cp\u003eThe Ni\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e-TNO samples were synthesized via a conventional one-step solid-state reaction with Nb\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e5\u003c/sub\u003e powder, anatase TiO\u003csub\u003e2\u003c/sub\u003e and NiO. To obtain Ni\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e-TNO, stoichiometric amounts of the raw materials were ball-milled in the planetary mill at a rotational speed of 400 rpm for 8 h. Ultimately, the obtained powder was subjected to heating at 1000 ℃ with a heating rate of 5 ℃/min, maintained for 10 hours in air, and then naturally cooled to room temperature. The Ti\u003csub\u003e2\u003c/sub\u003eNb\u003csub\u003e10\u003c/sub\u003eO\u003csub\u003e29\u003c/sub\u003e material was prepared by using the same process.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec4\" class=\"Section2\"\u003e \u003ch2\u003e2.2 Materials Characterization\u003c/h2\u003e \u003cp\u003eAs-calcined powder crystal structures were characterized by powder X-ray diffraction (XRD) (Bruker D8 Advance, Germany, Cu K radiation source\u0026thinsp;=\u0026thinsp;1.541 \u0026Aring;). Raman spectra were obtained from a Raman spectrometer (LabRAM HR, Horiba jobinyvon). Using transmission electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM, JEM-2100F), the morphologies (sizes and microstructures) were evaluated. The elemental distribution of the sample was detected using energy-dispersive X-ray spectroscopy (EDS) combined with high-resolution transmission electron microscopy. X-ray photoelectron spectroscopy (XPS, Thermo VG Scientific, VG MultiLab 2000) was utilized to analyze the surface chemical composition and valence state.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec5\" class=\"Section2\"\u003e \u003ch2\u003e2.3 Electrochemical Measurement\u003c/h2\u003e \u003cp\u003eCR2025-type coin cells were assembled in a glove box filled with dry argon for the evaluation of electrochemical performances. A homogeneous slurry was prepared by thoroughly mixing 70wt% calcined powder, 10wt% polyvinylidene fluoride (PVDF), and 20wt% calcined powder in N-methyl-2-pyrrolidone (NMP). The slurry was uniformly cast onto copper foil and dried at 65\u0026deg;C for 10 hours, resulting in a loading density of approximately 1.0 mg cm\u003csup\u003e\u0026minus;\u0026thinsp;2\u003c/sup\u003e for the electrode. Lithium foil served as the reference electrode for the battery. A microporous polypropylene film (Celgard 2500) was employed as the separator. The electrolyte comprised a 1 M LiPF\u003csub\u003e6\u003c/sub\u003e (DAN VEC) solution in a 1:1 weight ratio of ethylene carbonate (EC) to diethyl carbonate (DEC). Electrostatic discharge-charge tests were conducted using a multi-channel battery testing system (Neware CT-3008, China) at various current rates within the potential range of 3.0\u0026ndash;1.0 V. Measurements of cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) were conducted using the electrochemical workstation (Chenhua, ChI660E, China).\u003c/p\u003e \u003c/div\u003e"},{"header":"3. Results and discussion","content":"\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\u003eThe detailed refined structural parameters for TNO and Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO.\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"13\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" 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 \u003cdiv align=\"left\" class=\"colspec\" colname=\"c8\" colnum=\"8\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c9\" colnum=\"9\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c10\" colnum=\"10\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c11\" colnum=\"11\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c12\" colnum=\"12\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c13\" colnum=\"13\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eProduct\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003ea/\u0026Aring;\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eb/\u0026Aring;\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003ec/\u0026Aring;\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colspan=\"2\" nameend=\"c6\" namest=\"c5\"\u003e \u003cp\u003e\u003cem\u003eα\u003c/em\u003e/\u0026deg;\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c7\"\u003e \u003cp\u003e\u003cem\u003eβ\u003c/em\u003e/\u0026deg;\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c8\"\u003e \u003cp\u003e\u003cem\u003eγ\u003c/em\u003e/\u0026deg;\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colspan=\"3\" nameend=\"c11\" namest=\"c9\"\u003e \u003cp\u003eVolume/\u0026Aring;\u003csup\u003e3\u003c/sup\u003e\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c12\"\u003e \u003cp\u003ewRp\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c13\"\u003e \u003cp\u003eRp\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eTNO\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e15.518\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e3.813\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colspan=\"2\" nameend=\"c5\" namest=\"c4\"\u003e \u003cp\u003e20.542\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e90\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e113.05\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colspan=\"2\" nameend=\"c9\" namest=\"c8\"\u003e \u003cp\u003e90\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c10\"\u003e \u003cp\u003e1117.59\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colspan=\"2\" nameend=\"c12\" namest=\"c11\"\u003e \u003cp\u003e0.062\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c13\"\u003e \u003cp\u003e0.045\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eNi\u003csub\u003e0.05\u003c/sub\u003e-TNO\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e15.566\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e3.818\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colspan=\"2\" nameend=\"c5\" namest=\"c4\"\u003e \u003cp\u003e20.559\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e90\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e113.24\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colspan=\"2\" nameend=\"c9\" namest=\"c8\"\u003e \u003cp\u003e90\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c10\"\u003e \u003cp\u003e1123.63\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colspan=\"2\" nameend=\"c12\" namest=\"c11\"\u003e \u003cp\u003e0.061\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c13\"\u003e \u003cp\u003e0.042\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\u003eFirstly, we investigate the crystal structure of Ni\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e-TNO (\u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.03, 0.05, and 0.07). As shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003ea, the diffraction peaks observed in Ni\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e-TNO index well to monoclinic phase TNO (space: A/2m, PDF#72\u0026ndash;0159), without impurity phases of TiO\u003csub\u003e2\u003c/sub\u003e or Nb\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e5\u003c/sub\u003e. This indicates the successful synthesis of TNO and Ni doping does not change the space group. With Ni content increasing from 0 to 0.07, the position of the diffraction peak of the (020) crystal surface moves to smaller angles (Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003eb), which suggests an increase of interplanar spacing at a higher Ni doping content. Besides, with the increase of Ni\u003csup\u003e2+\u003c/sup\u003e content, the diffraction peak intensity also decreases, indicating that Ni\u003csup\u003e2+\u003c/sup\u003e doping can effectively reduce the crystallinity of the material, which might reduce the Li\u003csup\u003e+\u003c/sup\u003e diffusion barrier[\u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e]. However, excessive doping gives rise to the variation of crystal structure, as unveiled from the disappeared (11\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\stackrel{\\text{-}}{\\text{1}}\\)\u003c/span\u003e\u003c/span\u003e) peak of Ni\u003csub\u003e0.07\u003c/sub\u003e-TNO in Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003ec. More specifically, Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003ed-e presents the refinement results of the XRD patterns for TNO and Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO using the Rietveld method, accompanied by comprehensive structural parameters provided in Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e. It is seen that Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO (1123.63 \u0026Aring;\u003csup\u003e3\u003c/sup\u003e) has a larger volume of unit cells than TNO (1117.59 \u0026Aring;\u003csup\u003e3\u003c/sup\u003e). This can be attributed to the fact that Ni\u003csup\u003e2+\u003c/sup\u003e has a larger ionic radius when compared to Ti\u003csup\u003e4+\u003c/sup\u003e and Nb\u003csup\u003e5+\u003c/sup\u003e. The larger volume of the unit cell can provide a wider diffusion channel for Li\u003csup\u003e+\u003c/sup\u003e diffusion (Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003eh and \u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003ei).\u003c/p\u003e \u003cp\u003eFurther, Raman spectroscopy was applied to get insight into the bonding characteristics of the crystal structures. As shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003ef, the bands occurring at 896 and 1000 cm\u003csup\u003e\u0026ndash;1\u003c/sup\u003e correspond to the tensile vibration of NbO\u003csub\u003e6\u003c/sub\u003e[\u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e]. The bands of 544 and 646 cm\u003csup\u003e\u0026ndash;1\u003c/sup\u003e refer to the vibration of the Ti\u0026thinsp;\u0026minus;\u0026thinsp;O bonds of TiO\u003csub\u003e6\u003c/sub\u003e[\u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e]. As for the bands at 270 and 349 cm\u003csup\u003e\u0026ndash;1\u003c/sup\u003e, they are associated with symmetric and asymmetric bending motions of O-Ti-O and O-Nb-O bridge bonds, respectively[\u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e]. However, the Ti\u0026ndash;O vibrational peak of Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO exhibits a slight blue shift, providing evidence for changes in the internal chemical environment, maybe attributed to increased cation-oxygen bonding and the development of oxygen vacancies[\u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e].\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe morphologies and particle sizes of each sample are examined through scanning electron microscopy (SEM). As depicted in Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003ea-h, all samples present irregularly reunion particles, and the particle size ranges from 0.2 to 1 \u0026micro;m. Compared to the original sample, Ni\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e-TNO particles are more dispersed. To further reveal the morphological structures of Ni\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e-TNO, TEM characterizations were conducted (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003ea-i). The diffraction patterns in Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003eb and \u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003ef unveil that TNO and Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO are typical single-crystals. The different orientations of the crystal surfaces can be seen from Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003ec and \u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003eg. After further amplification and analysis, the specific parameters of the crystal surface can be obtained (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003ed and \u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003eh). From the lattice fringes of (400) and (600) crystal planes of TNO and Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO, their interlayer spacings are 0.354 and 0.237 nm respectively, which agrees well with the findings from XRD analyses. The homogeneous distribution of Ti, Nb, O, and Ni can be seen from the TEM-EDS elemental mapping (Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003ei), suggesting the successful introduction of Ni\u003csup\u003e2+\u003c/sup\u003e into TNO.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThen, XPS is utilized to investigate the surface composition and valence states of Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO and TNO. As seen in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ea, the full XPS spectrum of Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO indicates the existence of Ti, Nb, O, and Ni, revealing that Ni has been successfully doped in Ni\u003csub\u003e0\u003c/sub\u003e.\u003csub\u003e05\u003c/sub\u003e-TNO. This can also be verified from the characteristic peaks of Ni\u003csup\u003e2+\u003c/sup\u003e in Ni\u003csub\u003e0\u003c/sub\u003e.\u003csub\u003e05\u003c/sub\u003e-TNO (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003eb). Similar results can be observed from TNO excluding the absence of the Ni element. As seen in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ec-d, for the TNO, a couple of peaks located at 464.02 and 458.26 eV of the Ti spectrum originate from Ti 2p\u003csub\u003e1/2\u003c/sub\u003e and Ti 2p\u003csub\u003e3/2\u003c/sub\u003e, suggesting the existence of Ti\u003csup\u003e4+\u003c/sup\u003e. The Nb spectrum of TNO at 209.55 and 206.8 eV are indexed into Nb 3d\u003csub\u003e5/2\u003c/sub\u003e and Nb 3d\u003csub\u003e3/2\u003c/sub\u003e of Nb\u003csup\u003e5+\u003c/sup\u003e, separately. Specifically, the peaks of both Ti 2p and Nb 3d shift towards lower binding energy positions following Ni doping, which unveils more Ti\u003csup\u003e3+\u003c/sup\u003e and Nb\u003csup\u003e4+\u003c/sup\u003e in Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO[\u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e5\u003c/span\u003e]. The presence of Ti\u003csup\u003e3+\u003c/sup\u003e and Nb\u003csup\u003e4+\u003c/sup\u003e can be attributed to the charge distribution caused by Ni\u003csup\u003e2+\u003c/sup\u003e doping[\u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e]. From Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ee, Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO shows a broader oxygen-deficient region in comparison with TNO, unveiling the more missing lattice O in Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO[\u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e29\u003c/span\u003e]. This can also be reflected from the electron paramagnetic resonance (EPR). As illustrated in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ef, both TNO and Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO display an EPR signal at \u003cem\u003eg\u003c/em\u003e\u0026thinsp;=\u0026thinsp;2.0 (typical signal of oxygen vacancies) and Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO demonstrates a stronger peak intensity than that of TNO, which indicates the existence of an increased number of oxygen vacancies in Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe cyclic voltammetry (CV) was used to investigate the kinetic properties during the corresponding redox process in the voltage range of 1.0‒3.0 V for the first three cycles with the sweep of 0.2 mV s\u003csup\u003e\u0026ndash;1\u003c/sup\u003e. As shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003ea and \u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003eb, for each cell, the locations of cathodic peaks in the CV during the first cycle deviate from those observed in the subsequent two cycles, which is due to the change of electronic structure of TNO electrode induced by the distortion of TiO\u003csub\u003e6\u003c/sub\u003e or NbO\u003csub\u003e6\u003c/sub\u003e octahedra and the irreversible consumption of Li\u003csup\u003e+\u003c/sup\u003e during the process of Li\u003csup\u003e+\u003c/sup\u003e insertion[\u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e, \u003cspan citationid=\"CR30\" class=\"CitationRef\"\u003e30\u003c/span\u003e]. The CV curves consistently display substantial sharp redox peaks at 1.55‒1.75 V, associated with the Nb\u003csup\u003e5+\u003c/sup\u003e/Nb\u003csup\u003e4+\u003c/sup\u003e redox couple, and small gentle peaks near 1.9 V, corresponding to the Ti\u003csup\u003e4+\u003c/sup\u003e/Ti\u003csup\u003e3+\u003c/sup\u003e redox couple. The broad peak at 1.0‒1.5 V refers to the Nb\u003csup\u003e4+\u003c/sup\u003e/Nb\u003csup\u003e3+\u003c/sup\u003e redox couple. Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO exhibits reduced redox potential differences compared to pure TNO, demonstrating superior kinetic reversibility after Ni doping[\u003cspan citationid=\"CR39\" class=\"CitationRef\"\u003e39\u003c/span\u003e]. Figure\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003ec illustrates the charge and discharge profiles of the initial cycle of all samples at a constant current density of 0.1 C. The charge and discharge curves can be divided into three regions according to the inflection point, which are consistent with the redox changes observed during the CV experiments. The regions of A and C correspond to the solid solution of Li\u003csup\u003e+\u003c/sup\u003e in TNO[\u003cspan citationid=\"CR32\" class=\"CitationRef\"\u003e32\u003c/span\u003e]. The plateau in region B involves a phase of two-phase transition corresponding to a redox reaction in 1.65v[\u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e, \u003cspan citationid=\"CR33\" class=\"CitationRef\"\u003e33\u003c/span\u003e]. In this region, a longer reaction plateau in Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO implies more capacity contribution, most likely originating from the more active sites brought about by oxygen vacancies. It is seen that the discharge capacity and Coulombic efficiency of the doped sample at small Ni content (\u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.03 and 0.05) are superior to those of the original sample. Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO exhibits the most superior electrochemical performance, with the first discharge capacity and Coulombic efficiency of 306 mAh g\u003csup\u003e\u0026ndash;1\u003c/sup\u003e and 91.46%, respectively. This could be attributed to the fact that the doped samples exhibit smaller average particle sizes and higher (ionic and electronic) conductivities[\u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e31\u003c/span\u003e]. Thus, Ni\u003csup\u003e2+\u003c/sup\u003e doping has a positive effect on the surface reaction kinetics of Li\u003csup\u003e+\u003c/sup\u003e.\u003c/p\u003e \u003cp\u003eFigure\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003ed illustrates the rate capabilities of Ni\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e-TNO (\u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0, 0.03, 0.05 and 0.07) at varied current densities. The capacities of Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO at 0.5, 1, 2, 5, 10, 20, and 30 C are 265.68, 251.16, 239.78, 223.61, 204.89, 185.63, and 181.76 mAh g\u003csup\u003e\u0026ndash;1\u003c/sup\u003e, respectively, which significantly elevated in comparison to TNO (202.70, 189.90, 180.52, 170.09, 158.89, 147.43, and 138.62 mAh g\u003csup\u003e\u0026ndash;1\u003c/sup\u003e). Moreover, the cyclic stability of Ni\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e-TNO at a large current rate of 10 C was evaluated (Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003ee). It is seen that Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO displays the highest cycling stability among the four samples. The reversible capacity of Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO after 500 cycles is 146.19 mA h g\u003csup\u003e\u0026ndash;1\u003c/sup\u003e, with a capacity loss of only 0.04% per cycle, while the reversible capacities of other Ni\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e-TNO samples (\u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0, 0.03 and 0.07) are 85.31, 125.95, and 81.96 mAh g\u003csup\u003e\u0026ndash;1\u003c/sup\u003e. The outstanding cyclic stability may be due to the wider Li\u003csup\u003e+\u003c/sup\u003e diffusion pathway after Ni\u003csup\u003e2+\u003c/sup\u003e doping, which helps stabilize the structure during repeated cycles[\u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e]. The reason for the poor cycling performance of Ni\u003csub\u003e0.07\u003c/sub\u003e-TNO might be that excessive Ni\u003csup\u003e2+\u003c/sup\u003e doping results in excessive lattice distortion (see Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003ec), which leads to a significant decrease in structural stability.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab2\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 2\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eImpedance parameters and Li\u003csup\u003e+\u003c/sup\u003e diffusion coefficients of TNO and Ni\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e-TNO\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"4\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eProduct\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eR\u003csub\u003ect\u003c/sub\u003e (Ω)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003eσ (Ω s\u003csup\u003e\u0026ndash;0.5\u003c/sup\u003e)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003e\u003cem\u003eD\u003c/em\u003e\u0026times;10\u003csup\u003e\u0026ndash;14\u003c/sup\u003e (cm\u003csup\u003e2\u003c/sup\u003e s\u003csup\u003e\u0026ndash;1\u003c/sup\u003e)\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eTNO\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e168.00\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e132.64\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e3.51\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eNi\u003csub\u003e0.03\u003c/sub\u003e-TNO\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e55.35\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e96.32\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e32.3\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eNi\u003csub\u003e0.05\u003c/sub\u003e-TNO\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e51.42\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e110.85\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e37.5\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eNi\u003csub\u003e0.07\u003c/sub\u003e-TNO\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e69.15\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e37.99\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e20.7\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\u003eIn order to investigate the nature of ion transport during the charge and discharge processes, we further performed the impedance analysis test (A.C. impedance technique) on the battery. Figure\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e illustrates the Nyquist plots for both TNO and Ni\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e-TNO after cycling three times at 0.1 C with the fitted equivalent circuit inserted. In Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003ea, a semicircular feature is present in the high-frequency region, which refers to the reactive process of electron transfer during Li\u003csup\u003e+\u003c/sup\u003e desolvation/adsorption (\u003cem\u003eR\u003c/em\u003e\u003csub\u003e\u003cem\u003ect\u003c/em\u003e\u003c/sub\u003e). The low-frequency region is an inclined straight line, the slope of this line is related to the diffusion of Li\u003csup\u003e+\u003c/sup\u003e in the bulk crystals (Warburg resistance)[\u003cspan citationid=\"CR34\" class=\"CitationRef\"\u003e34\u003c/span\u003e, \u003cspan citationid=\"CR35\" class=\"CitationRef\"\u003e35\u003c/span\u003e]. The specific fitting parameters can be seen in Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e, the doped samples demonstrate much smaller \u003cem\u003eR\u003c/em\u003e\u003csub\u003e\u003cem\u003ect\u003c/em\u003e\u003c/sub\u003e (55.35, 51.42 and 69.15 Ω for Ni\u003csub\u003e0.03\u003c/sub\u003e-TNO, Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO and Ni\u003csub\u003e0.07\u003c/sub\u003e-TNO, respectively) than that (168.0 Ω) of the pristine samples. The reason might be that Ni\u003csup\u003e2+\u003c/sup\u003e could optimize the electronic structure of TNO, which facilitates the internal electron transfer, thus contributing to the electronic conductivity [\u003cspan citationid=\"CR36\" class=\"CitationRef\"\u003e36\u003c/span\u003e]. This can be verified from the obtained conductivity via the four-probe conductivity test. The electronic conductivity (2.2 \u0026times; 10\u003csup\u003e\u0026ndash;7\u003c/sup\u003e s cm\u003csup\u003e\u0026ndash;1\u003c/sup\u003e) of Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO is two orders of magnitude higher than that (1 \u0026times; 10\u003csup\u003e\u0026ndash;9\u003c/sup\u003e s cm\u003csup\u003e\u0026ndash;1\u003c/sup\u003e) of TNO [\u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e]. These results unveil that Ni doping is effective in tuning the electronic conductivity of TNO.\u003c/p\u003e \u003cp\u003eThen, we explore the diffusion coefficient of Li\u003csup\u003e+\u003c/sup\u003e via the impedance analysis. The Li\u003csup\u003e+\u003c/sup\u003e diffusion coefficient is mainly related to the slope of the straight line in the low-frequency region, and the specific diffusion process can be obtained according to the following equation:\u003cdiv id=\"Equ1\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ1\" name=\"EquationSource\"\u003e\n$${D}_{{\\text{L}\\text{i}}^{+}}=\\frac{{R}^{2}{T}^{2}}{2{A}^{2}{n}^{4}{F}^{4}{C}^{2}{\\sigma }^{2}}$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e1\u003c/div\u003e\u003c/div\u003e,\u003c/p\u003e \u003cp\u003eIn the given expression, R represents the gas constant, T stands for the absolute temperature, A denotes the surface area of the active electrode, n is the number of electrons per molecule, F represents the Faraday constant, C is the molar concentration of Li\u003csup\u003e+\u003c/sup\u003e, and σ represents the Warburg factor. \u003cem\u003eσ\u003c/em\u003e can be estimated based on the plot of the linear fit between Z and the inverse square root of the lower angular frequency (Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003eb). It can be expressed by the following equation:\u003cdiv id=\"Equ2\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ2\" name=\"EquationSource\"\u003e\n$${\\text{Z}}^{{\\prime }}\\text{ = }{\\text{R}}_{\\text{s}}\\text{+}{\\text{R}}_{\\text{ct}}\\text{+}{\\text{\u0026sigma;\u0026omega;}}^{\\text{-}\\text{1/2}}$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e2\u003c/div\u003e\u003c/div\u003e.\u003c/p\u003e \u003cp\u003eThe Li\u003csup\u003e+\u003c/sup\u003e diffusion coefficients of Ni\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e-TNO and TNO are tabulated in Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e. The Li\u003csup\u003e+\u003c/sup\u003e diffusion coefficients of Ni\u003csub\u003e0.03\u003c/sub\u003e-TNO, Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO and Ni\u003csub\u003e0.07\u003c/sub\u003e-TNO are 3.23\u0026times;10\u003csup\u003e\u0026ndash;13\u003c/sup\u003e, 3.75\u0026times;10\u003csup\u003e\u0026ndash;13\u003c/sup\u003e, and 2.07\u0026times;10\u003csup\u003e\u0026ndash;13\u003c/sup\u003e cm\u003csup\u003e2\u003c/sup\u003e s\u003csup\u003e\u0026ndash;1\u003c/sup\u003e, respectively, which are markedly higher than that (3.51\u0026times;10\u003csup\u003e\u0026ndash;14\u003c/sup\u003e cm\u003csup\u003e2\u003c/sup\u003e s\u003csup\u003e\u0026ndash;1\u003c/sup\u003e) of the pristine one. The Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO displays the highest Li\u003csup\u003e+\u003c/sup\u003e diffusion coefficient. The reason for this phenomenon may be that the lattice distortion caused by Ni\u003csup\u003e2+\u003c/sup\u003e doping gives rise to an increase in the cell volume, which provides a wider channel for Li\u003csup\u003e+\u003c/sup\u003e diffusion.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eTo further unveil the change of crystal structure during the (de)lithiation process of Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO, the non-in situ XRD tests were conducted for the pole pieces by discharging or charging them to specific voltages at current densities of 0.2 C. Here, four points were respectively selected for the initial charging and discharging processes (Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003ea). As shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003eb, all the samples match well with the monoclinic Ti\u003csub\u003e2\u003c/sub\u003eNb\u003csub\u003e10\u003c/sub\u003eO\u003csub\u003e29\u003c/sub\u003e and the crystal diffraction peaks are relatively sharp, which suggest a good stability of the crystal structure during the charging and discharging process. Figure\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003ec-d illustrates the enlarged (21\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\stackrel{\\text{-}}{\\text{5}}\\)\u003c/span\u003e\u003c/span\u003e), (41\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\stackrel{\\text{-}}{\\text{1}}\\)\u003c/span\u003e\u003c/span\u003e), and (020) crystal planes, and it is seen that the (020) crystal plane shifts to a low angle during discharging and returns to the initial position in the charging process. This unveils the good structural stability of Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO during (de)lithiation. However, the lattice parameters of (21\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\stackrel{\\text{-}}{\\text{5}}\\)\u003c/span\u003e\u003c/span\u003e) and (41\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\(\\stackrel{\\text{-}}{\\text{1}}\\)\u003c/span\u003e\u003c/span\u003e) crystal planes do not change significantly, which is due to that these crystal planes are not the preferential diffusion paths of Li\u003csup\u003e+\u003c/sup\u003e in Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO[\u003cspan additionalcitationids=\"CR38\" citationid=\"CR37\" class=\"CitationRef\"\u003e37\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR39\" class=\"CitationRef\"\u003e39\u003c/span\u003e].\u003c/p\u003e"},{"header":"4. Conclusions","content":"\u003cp\u003eIn this paper, Ni\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e-TNO samples were synthesized using a simple solid-state method. The influence of Ni\u003csup\u003e2+\u003c/sup\u003e on the structure, morphology and valence distribution of the material was explored through a series of characterizations. According to the experimental results, Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO is the most ideal electrode material. While the crystal structure remains unaffected by a moderate amount of Ni\u003csup\u003e2+\u003c/sup\u003e doping, an increase in cell parameters occurs, creating more extensive diffusion channels and active sites for Li\u003csup\u003e+\u003c/sup\u003e transport. In addition, the introduction of Ni alters the electronic environment of TNO, greatly improving the conductivity of the material and generating a certain amount of oxygen vacancies. Based on these advantages, Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO exhibits the most favorable electrochemical performance among all samples. A large reversible capacity of 306 mAh g\u003csup\u003e\u0026ndash;1\u003c/sup\u003e and a high Coulombic efficiency of 91.46% can be reached at 0.1 C. Besides, there is still 146.19 mAh g\u003csup\u003e\u0026ndash;1\u003c/sup\u003e after 500 cycles at a discharge current of 10 C. The findings in our research offer a fresh perspective on enhancing niobium-based oxide materials for novel lithium-ion anodes.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e \u003ch2\u003eConflict of Interest\u003c/h2\u003e \u003cp\u003eThe authors declare no competing financial interest.\u003c/p\u003e \u003c/p\u003e\u003ch2\u003eAuthor Contribution\u003c/h2\u003e\u003cp\u003eXiuli Chen: conceptualization, methodology, investigation, writing - original draft, and data curation. Mingru Su: formal analysis and resources. Xueli Chen: data curation and methodology. Pei Cui: methodology and formal analysis. Yu Zhou: formal analysis. Yunxuan Ji: data curation. Panpan Zhang: validation, supervision, writing - review \u0026amp; editing. Yunjian Liu: visualization, supervision, and funding acquisition.\u003c/p\u003e\u003ch2\u003eAcknowledgments\u003c/h2\u003e \u003cp\u003eThis research was sponsored by the National Natural Science Foundation of China (52004103, 51974137 and 52304328), the Natural Science Foundation of Jiangsu Province (BK20220534), Jiangsu Double-Innovation PhD Program in 2022 (JSSCBS20221241) and China Postdoctoral Science Foundation (2023M733189).\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\u003cli\u003e\u003cspan\u003eXie F, Xu J, Liao Q, et al (2023) Progress in niobium-based oxides as anode for fast-charging Li-ion batteries [J]. Energy Reviews 2: 100027\u003c/span\u003e\u003c/li\u003e \u003cli\u003e\u003cspan\u003eJiang T, Ma S, Deng J, et al (2022) Partially reduced titanium niobium oxide: a high-performance lithium-storage material in a broad temperature range [J]. 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ACS Appl Mater Interfaces 15: 43745\u0026ndash;43755\u003c/span\u003e\u003c/li\u003e\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":false,"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":"ionics","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"","sideBox":" Learn more about [Ionics](https://www.springer.com/journal/11581) ","snPcode":"11581","submissionUrl":"https://mc.manuscriptcentral.com/ionics","title":"Ionics","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"stoa","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false},"keywords":"Lithium-ion batteries, Ti2Nb10O29, Ni2+ doping, high-rate capability","lastPublishedDoi":"10.21203/rs.3.rs-3786761/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-3786761/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eTi\u003csub\u003e2\u003c/sub\u003eNb\u003csub\u003e10\u003c/sub\u003eO\u003csub\u003e29\u003c/sub\u003e (TNO) has garnered significant research attention due to its high specific capacity and excellent safety features, positioning it as a promising anode material for lithium-ion batteries (LIBs). Nevertheless, its rate capability is significantly hampered by poor electronic and ionic conductivity. In this paper, Ni\u003csup\u003e2+\u003c/sup\u003e doping has been first applied to address these issues. A series of Ni\u003csup\u003e2+\u003c/sup\u003e doped TNO (Ni\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e-TNO (\u003cem\u003ex\u003c/em\u003e = 0.03, 0.05, 0.07) electrode materials have been prepared to unveil the effects of Ni\u003csup\u003e2+\u003c/sup\u003e content. The experimental results unveil that Ni\u003csup\u003e2+\u003c/sup\u003e doping maintains the Wadsley-Roth shear structure of TNO while augmenting the single-cell volume and introducing additional oxygen vacancies in TNO. This generates a wider diffusion path and more active sites for lithium ions (Li\u003csup\u003e+\u003c/sup\u003e). Besides, the introduction of Ni\u003csup\u003e2+\u003c/sup\u003e can alter the conductive field distribution of TNO, giving rise to a much higher electronic conductivity of Ni\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e-TNO. Among the synthesized Ni\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e-TNO, Ni\u003csub\u003e0.05\u003c/sub\u003e-TNO shows the best electrochemical performance, demonstrating a reversible capacity of 306 mAh g\u003csup\u003e–1\u003c/sup\u003e with a Coulombic efficiency of 91.46% in the first cycle at 0.1 C and 146.19 mAh g\u003csup\u003e–1\u003c/sup\u003e at 10 C after 500 cycles.\u003c/p\u003e","manuscriptTitle":"Ni0.05Ti1.95Nb10O29: an advanced anode material for high-performance lithium-ion storage","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2024-01-02 18:22:34","doi":"10.21203/rs.3.rs-3786761/v1","editorialEvents":[{"type":"communityComments","content":0},{"type":"decision","content":"Revision requested","date":"2024-03-04T03:50:31+00:00","index":"","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2024-02-25T08:30:56+00:00","index":"hide","fulltext":""},{"type":"editorInvitedReview","content":"","date":"2024-02-12T17:09:07+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"dd443893-fad9-41b1-a659-e1d33481ca23","date":"2024-01-17T18:36:10+00:00","index":"hide","fulltext":""},{"type":"reviewerAgreed","content":"e6a3e0a5-baf1-4046-a881-0c9efd07fed7","date":"2024-01-16T11:35:18+00:00","index":"hide","fulltext":""},{"type":"reviewersInvited","content":"","date":"2024-01-15T17:45:06+00:00","index":"","fulltext":""},{"type":"editorAssigned","content":"","date":"2023-12-29T12:50:36+00:00","index":"","fulltext":""},{"type":"checksComplete","content":"","date":"2023-12-29T12:50:36+00:00","index":"","fulltext":""},{"type":"submitted","content":"Ionics","date":"2023-12-21T11:53:57+00:00","index":"","fulltext":""}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"ionics","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"","sideBox":" Learn more about [Ionics](https://www.springer.com/journal/11581) ","snPcode":"11581","submissionUrl":"https://mc.manuscriptcentral.com/ionics","title":"Ionics","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"stoa","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false}}],"origin":"","ownerIdentity":"21589fb6-ddc6-4e87-b6e8-0d040e8a2156","owner":[],"postedDate":"January 2nd, 2024","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"published-in-journal","subjectAreas":[],"tags":[],"updatedAt":"2024-05-01T23:27:18+00:00","versionOfRecord":{"articleIdentity":"rs-3786761","link":"https://doi.org/10.1007/s11581-024-05547-9","journal":{"identity":"ionics","isVorOnly":false,"title":"Ionics"},"publishedOn":"2024-04-24 23:27:18","publishedOnDateReadable":"April 24th, 2024"},"versionCreatedAt":"2024-01-02 18:22:34","video":"","vorDoi":"10.1007/s11581-024-05547-9","vorDoiUrl":"https://doi.org/10.1007/s11581-024-05547-9","workflowStages":[]},"version":"v1","identity":"rs-3786761","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-3786761","identity":"rs-3786761","version":["v1"]},"buildId":"qtupq5eGEP_6zYnWcrvyt","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}